Compositions formed from calcium carbonate or magnesium carbonate-containing materials and surface treatment compositions comprising at least one cross-linking compound

A composition of calcium or magnesium carbonate-treated materials with a crosslinking compound enhances the mechanical properties and processability of elastomers, addressing the limitations of conventional fillers.

JP7812831B2Active Publication Date: 2026-02-10OMYA INT AG
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Patent Information

Application Number
JP2023501878
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2020-07-16
Filing Date
2021-07-15
Publication Date
2026-02-10
Estimated Expiration
2041-07-15

AI Technical Summary

Technical Problem

Elastomers often lack sufficient mechanical properties, such as tear resistance, tensile modulus, and tensile strength, and are difficult to process due to the limitations of conventional fillers like carbon black and silica, which pose health, safety, and environmental concerns.

Method used

A composition comprising calcium or magnesium carbonate-containing materials, treated with a surface treatment composition containing a crosslinking compound with specific functional groups, is used to enhance the mechanical properties of elastomers.

Benefits of technology

The composition improves tear resistance, tensile modulus, and tensile strength of elastomers while ensuring better processability, overcoming the limitations of traditional fillers.

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Abstract

The present invention relates to compositions formed from a calcium carbonate or magnesium carbonate containing material and a surface treatment composition comprising at least one crosslinking compound; a dry process for making such compositions; a curable elastomeric mixture comprising an elastomeric resin and the composition; a cured elastomeric product formed from the curable elastomeric mixture; a process for making the cured elastomeric product; the use of at least one crosslinking compound comprising at least two functional groups, at least one functional group suitable for crosslinking the elastomeric resin and at least one functional group suitable for reacting with the calcium carbonate or magnesium carbonate containing material, in compounding an elastomer formed from an elastomeric resin and at least one calcium carbonate or magnesium carbonate containing material; and articles formed from the cured elastomeric product.
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Description

[Technical Field]

[0001] The present invention relates to compositions formed from a calcium carbonate or magnesium carbonate containing material and a surface treatment composition comprising at least one crosslinking compound; a dry process for making such compositions; a curable elastomeric mixture comprising an elastomeric resin and the composition; a cured elastomeric product formed from the curable elastomeric mixture; a process for making the cured elastomeric product; the use of at least one crosslinking compound comprising at least two functional groups, at least one functional group suitable for crosslinking the elastomeric resin and at least one functional group suitable for reacting with the calcium carbonate or magnesium carbonate containing material, in compounding an elastomer formed from an elastomeric resin and at least one calcium carbonate or magnesium carbonate containing material; and articles formed from the cured elastomeric product. [Background technology]

[0002] Elastomers, commonly referred to as rubber, are crosslinked polymeric materials that have rubber-like elasticity, i.e., the ability to reversibly deform upon application of an external deforming force. Elastomers are widely used in, for example, tubeless articles, membranes, seals, gloves, pipes, cables, electrical connectors, oil hoses, shoe soles, O-ring seals, shaft seals, gaskets, tubing, valve stem seals, fuel hoses, tank seals, diaphragms, flexible pump liners, mechanical seals, pipe joints, valve lines, military flare blenders, electrical connectors, fuel joints, roll covers, firewall seals, and jet engine clips.

[0003] It is common in the art to add certain fillers to elastomer compositions, for example, to improve their mechanical properties. Commonly used reinforcing fillers include carbon black, (modified) silica particles, kaolin, and other clays. However, these fillers have certain drawbacks. For example, carbon black is highly conductive and therefore cannot be used as a filler in insulated cables. The color of carbon black also imposes limitations on its application, and filler materials such as carbon black or modified silica are difficult to handle due to health, safety, and environmental concerns. Furthermore, elastomers containing these fillers may still lack sufficient tear resistance. They can easily break during processing, for example, if a nick is already present. This can occur especially when the elastomer is still hot, e.g., unmolded.

[0004] The use of ground calcium carbonate and precipitated calcium carbonate in elastomer compositions has been reported. For example, U.S. Patent No. 3,374,198 A discloses a composition containing ethylene-propylene rubber and calcium carbonate as a reinforcing filler. Sobhy et al. (Egyptian Journal of Solids 2003, 26, 241-257) report on the curing and mechanical properties of natural and nitrile rubbers filled with calcium carbonate.

[0005] EP 3 192 837 A1 refers to surface-modified calcium carbonates that have been surface-treated with anhydrides or acids or salts thereof and suggests their use in, inter alia, polymer compositions, papermaking, paints, adhesives, sealants, pharmaceutical applications, crosslinking of rubber, polyolefins, polyvinyl chloride, in unsaturated polyester and alkyd resins.

[0006] In view of the above, there is a continuing need for elastomers that have excellent mechanical properties. Summary of the Invention [Problem to be solved by the invention]

[0007] It is therefore an object of the present invention to provide elastomers having excellent mechanical properties, in particular improved tear resistance, improved tensile modulus, tensile strength and / or elongation at break. Furthermore, it is desirable to provide elastomers having good processability.

[0008] These and other objects are solved by the subject matter defined in the independent claims. Advantageous embodiments of the invention are defined in the corresponding dependent claims. [Means for solving the problem]

[0009] According to one aspect of the present invention, a calcium carbonate or magnesium carbonate containing material selected from the group consisting of ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), surface-reacted calcium carbonate (SRCC), precipitated hydromagnesite, and mixtures thereof; a surface treatment composition in an amount of 0.5 to 10% by weight based on the total weight of the calcium carbonate or magnesium carbonate-containing material; A composition formed from the surface treatment composition comprises at least one crosslinking compound containing at least two functional groups, wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with the calcium carbonate or magnesium carbonate-containing material; A composition is provided.

[0010] According to one embodiment, the calcium carbonate-containing material is selected from the group consisting of: marble, limestone, dolomite, chalk, and mixtures thereof; or the precipitated calcium carbonate (PCC) is selected from the group consisting of mineralogical crystal forms of aragonite, vaterite, and calcite, colloidal PCC, and mixtures thereof; preferably, the calcium carbonate-containing material is a sedimentary ground calcium carbonate (GCC).

[0011] According to another embodiment, the calcium carbonate-comprising material is a heaped ground calcium carbonate (GCC) and / or a precipitated calcium carbonate (PCC) and has: (i) a weight median particle size d measured by a precipitation method in the range of 0.1 μm to 10 μm, preferably in the range of 0.15 μm to 5 μm, more preferably in the range of 0.2 μm to 3 μm, and most preferably in the range of 0.25 μm to 3 μm, for example, 0.3 μm to 2 μm or 0.3 μm to 1.5 μm; 50 and / or (ii) a top cut (d) measured by sedimentation method of ≦45 μm, preferably ≦30 μm, more preferably ≦20 μm, and most preferably ≦15 μm 98 ); and / or (iii) Nitrogen and 0.5 to 150 m, measured using the BET method according to ISO 9277:2010 2 / g, preferably 1 to 80m 2 / g specific surface area (BET); and / or (iv) a total residual moisture content of ≦2 wt.-%, preferably ≦1.5 wt.-%, more preferably ≦1.2 wt.-%, and most preferably ≦0.8 wt.-%, based on the total dry weight of the at least one calcium carbonate-comprising material.

[0012] According to yet another embodiment, the calcium carbonate-comprising material is a mixture of (sedimentary) ground calcium carbonate or precipitated calcium carbonate and carbon dioxide and one or more HO + The reaction product with the ion donor is surface-reacted calcium carbonate (SRCC), and this carbon dioxide is + formed in situ by treatment with an ion donor and / or provided from an external source; or The magnesium carbonate-containing material is precipitated hydromagnesite and has: (i) a volume median particle size d of 0.1 to 75 μm, preferably 0.5 to 50 μm, more preferably 1 to 40 μm, even more preferably 1.2 to 30 μm, and most preferably 1.5 to 15 μm 50 and / or (ii) a volume top cut particle size d of 0.2 to 150 μm, preferably 1 to 100 μm, more preferably 2 to 80 μm, even more preferably 2.4 to 60 μm, and most preferably 3 to 30 μm 98 and / or (iii) 15m measured using nitrogen and BET methods 2 / g~200m 2 / g, preferably 20m 2 / g~180m 2 / g, more preferably 25m 2 / g~140m 2 / g, and even more preferably 27m 2 / g~120m 2 / g, most preferably 30m 2 / g~100m 2 / g specific surface area.

[0013] According to one embodiment, at least one functional group of the crosslinking compound suitable for reacting with the calcium or magnesium carbonate containing material comprises one or more terminal triethoxysilyl, trimethoxysilyl, and / or organic acid anhydride and / or salts thereof, and / or carboxylic acid groups and / or salts thereof.

[0014] According to another embodiment, the crosslinking compound is at least one graft polymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a homo- or copolymer containing butadiene units and optionally styrene units, or a compound containing two trialkoxysilylalkyl groups bonded to a sulfur-containing trialkoxysilane, preferably a polysulfide.

[0015] According to yet another embodiment, the at least one graft polymer is: (a) a grafted polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer and having: (i) a number average molecular weight M measured by gel permeation chromatography of 1,000 to 20,000 g / mol, preferably 1,400 to 15,000 g / mol, and more preferably 2,000 to 10,000 g / mol; n and / or (ii) the number of functional groups per chain is in the range of 2 to 12, preferably 2 to 9, more preferably 2 to 6, and / or (iii) an anhydride equivalent weight in the range of 400 to 2200, preferably 500 to 2000, more preferably 550 to 1800; or (b) A grafted polybutadiene-styrene copolymer containing at least one succinic anhydride group obtained by grafting a polybutadiene-styrene copolymer with maleic anhydride and having a 1,2-vinyl content of 20 to 80 mol %, preferably 20 to 40 mol %, based on the total weight of the grafted polybutadiene-styrene copolymer.

[0016] According to one embodiment, the composition is formed by providing at least one calcium or magnesium carbonate-containing material and at least one cross-linking compound as a physical mixture and / or by contacting at least one calcium or magnesium carbonate-containing material with at least one cross-linking compound, whereby a surface treatment layer comprising at least one cross-linking compound and / or a salt-containing reaction product thereof is formed on the surface of the at least one calcium or magnesium carbonate-containing material.

[0017] According to another embodiment, the surface treatment composition further comprises at least one additional surface treatment agent selected from the group consisting of: (I) a blend of phosphoric acid esters of one or more phosphoric acid monoesters and / or salts thereof, and / or one or more phosphoric acid diesters and / or salts thereof, and / or (II) at least one saturated or unsaturated aliphatic linear or branched carboxylic acid and / or salt thereof, preferably at least one aliphatic carboxylic acid and / or salt thereof having a total number of carbon atoms of C4 to C24, more preferably at least one aliphatic carboxylic acid and / or salt thereof having a total number of carbon atoms of C12 to C20, most preferably at least one aliphatic carboxylic acid and / or salt thereof having a total number of carbon atoms of C16 to C18, and / or (III) at least one mono-substituted succinic anhydride and / or a salt thereof, which is a succinic anhydride mono-substituted with a group selected from a linear group, a branched group, an aliphatic group, and a cyclic group having a total carbon atom number of at least C2 to C30 in the substituent, and / or (IV) at least one polydialkylsiloxane, and (V) A mixture of one or more materials according to (I) to (IV).

[0018] According to a further aspect of the present invention there is provided a dry manufacturing process for the preparation of a composition as defined herein, said process comprising at least the following steps: (a) providing a calcium carbonate or magnesium carbonate-containing material selected from the group consisting of ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), surface-reacted calcium carbonate (SRCC), precipitated hydromagnesite, and mixtures thereof; (b) adding at least one crosslinking compound containing at least two functional groups to the calcium carbonate- or magnesium carbonate-containing material in an amount of 0.1 to 10 mg / m based on the total weight of the calcium carbonate- or magnesium carbonate-containing material; 2 wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with the calcium carbonate or magnesium carbonate containing material; (c) optionally providing at least one further surface treatment agent as defined herein; (d) optionally, heating the at least one crosslinkable compound; and (e) contacting, in one or more steps, the calcium carbonate or magnesium carbonate-containing material with the at least one cross-linking compound while mixing; (f) heating the at least one further surface treatment agent, if present, to a temperature at or above its melting point, thereby obtaining a molten surface treatment agent, and in one or more steps contacting the molten surface treatment agent with the at least one crosslinking compound simultaneously or subsequently with the calcium carbonate or magnesium carbonate-containing material while mixing.

[0019] According to yet a further aspect of the present invention, there is provided a curable elastomeric mixture comprising: (a) an elastomeric resin, and (b) 5 to 300% by weight, preferably 10 to 150% by weight, more preferably 20 to 110% by weight, and most preferably 40 to 100% by weight of a composition as defined herein, based on the total weight of the elastomeric resin; Here, the composition is dispersed in the elastomeric resin.

[0020] According to one embodiment, the elastomeric resin is selected from natural or synthetic rubber, preferably from the group consisting of acrylic rubber, butadiene rubber, acrylonitrile-butadiene rubber, epichlorohydrin rubber, isoprene rubber, ethylene-propylene rubber, ethylene-propylene-diene rubber, nitrile-butadiene rubber, butyl rubber, styrene-butadiene rubber, polyisoprene, hydrogenated nitrile-butadiene rubber, carboxylated nitrile-butadiene rubber, chloroprene rubber, isoprene-isobutylene rubber, chloro-isobutene-isoprene rubber, brominated isobutene-isoprene rubber, silicone rubber, fluorocarbon rubber, polyurethane rubber, polysulfide rubber, thermoplastic rubber, and mixtures thereof.

[0021] According to another embodiment, the mixture further comprises additives such as color pigments, fibers, e.g., cellulose, glass or wood fibers, dyes, waxes, lubricants, oxidation- and / or UV-stabilizers, plasticizers, hardeners, crosslinking coagents, antioxidants, and other fillers, e.g., carbon black, TiO2, mica, clay, precipitated silica, talc, or calcined kaolin. According to yet a further aspect of the present invention there is provided a cured elastomeric product formed from the curable elastomeric mixture defined herein.

[0022] According to yet a further aspect of the present invention, there is provided a process for producing a cured elastomeric product as defined herein, the process comprising the steps of: (a) providing an elastomeric resin; (b) providing as a filler 5 to 300 wt. % of at least one calcium carbonate or magnesium carbonate-containing material based on the total weight of the elastomeric resin; (c) 0.1 to 10 mg / m based on the total weight of the calcium carbonate or magnesium carbonate-containing material 2 providing at least one crosslinkable compound comprising at least two functional groups, wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with the calcium carbonate or magnesium carbonate containing material; (d) optionally providing at least one further surface treatment agent as defined in claim 9; (e) optionally providing further additives such as color pigments, fibers, e.g., cellulose, glass or wood fibers, dyes, waxes, lubricants, oxidation- and / or UV-stabilizers, plasticizers, hardeners, crosslinking coagents, antioxidants, and other fillers, e.g., carbon black, TiO2, mica, clay, precipitated silica, talc, or calcined kaolin; (f) contacting, in any order, the components of steps (a), (b), (c) and optionally steps (d) and (e); and (g) curing the mixture resulting from step (f), thereby forming a cured elastomeric product.

[0023]

[0023] According to one embodiment, in contacting step (f), firstly, in one or more steps, the at least one calcium carbonate- or magnesium carbonate-comprising material of step (b) is contacted with at least one crosslinking compound of step (c) and, if present, subsequently or simultaneously with at least one further surface treatment agent of step (d), while mixing, so that a surface treatment layer comprising the at least one crosslinking compound and / or a salt-containing reaction product thereof, and optionally at least one further surface treatment agent and / or a salt-containing reaction product thereof, forms on the surface of the at least one calcium carbonate- or magnesium carbonate-comprising material of step (b), and secondly, in one or more steps, this surface-treated calcium carbonate- or magnesium carbonate-comprising material is contacted with the elastomeric resin of step (a) while mixing.

[0024] According to another embodiment, before or after, preferably after, the contacting, while mixing, of the surface-treated calcium or magnesium carbonate-comprising material with the elastomeric resin of step (a) in one or more steps, the further additives of step (e) are contacted, while mixing, with said calcium or magnesium carbonate-comprising material in one or more steps.

[0025] According to yet another embodiment, the contacting step (f) is carried out during the curing step (g), wherein the at least one crosslinking compound is contacted while mixing with the elastomeric resin of step (a) before or after, preferably after, adding the at least one calcium carbonate or magnesium carbonate containing material.

[0026] According to a still further aspect of the present invention there is provided the use of at least one crosslinkable compound comprising at least two functional groups, wherein in the elastomer formulation formed from an elastomer resin and at least one calcium carbonate- or magnesium carbonate-containing material as a filler, at least one functional group is suitable for crosslinking the elastomer resin and at least one functional group is suitable for reacting with the calcium carbonate- or magnesium carbonate-containing material; There is provided a use for improving the mechanical properties of an elastomer so formulated compared to the same elastomer formed from the same elastomeric resin and at least one calcium or magnesium carbonate containing material, but not comprising said at least one crosslinking compound comprising at least two functional groups, at least one functional group being suitable for crosslinking the elastomeric resin and at least one functional group being suitable for reacting with said calcium or magnesium carbonate containing material.

[0027] According to yet another aspect of the present invention there is provided an article formed from the cured elastomeric product as defined herein, said article being selected from the group comprising tubeless articles, membranes, sealings, gloves, pipes, cables, electrical connectors, oil hoses, shoe soles, O-ring seals, shaft seals, gaskets, tubing, valve stem seals, fuel hoses, tank seals, diaphragms, flexible liners for pumps, mechanical seals, pipe couplings, valve lines, military flare blenders, electrical connectors, fuel joints, roll covers, firewall seals, jet engine clips, and the like.

[0028] For purposes of the present invention, the following terms shall be understood to have the following meanings:

[0029] As used herein, the term "acid" means an acid as defined by Bronsted and Lowry (e.g., H2SO4, HSO4 - ), where "free acid" refers only to the acid in its fully protonated form (e.g., H2SO4).

[0030] As used herein, the term "polymer" generally includes homopolymers and copolymers, such as block, graft, random, and alternating copolymers, as well as blends and modifications thereof. A polymer may be an amorphous polymer, a crystalline polymer, or a semi-crystalline polymer, i.e., a polymer containing crystalline and amorphous portions. Crystallinity is specified as a percentage and can be determined by differential scanning calorimetry (DSC). An amorphous polymer can be characterized by its glass transition temperature, and a crystalline polymer can be characterized by its melting point. A semi-crystalline polymer can be characterized by its glass transition temperature and / or its melting point.

[0031] The term "copolymer" as used herein refers to a polymer derived from more than one type of monomer. A copolymer obtained by copolymerization of two types of monomers can also be called a bipolymer, a copolymer obtained from three monomers can also be called a terpolymer, a copolymer obtained from four monomers can also be called a quaterpolymer, etc. (See IUPAC Compendium of Chemical Terminology, 2014, "Copolymer"). Thus, the term "homopolymer" refers to a polymer derived from one type of monomer.

[0032] An "elastomer" is a polymer that exhibits rubber-like elasticity and contains crosslinks, preferably permanent crosslinks.

[0033] For purposes of this invention, a "crosslinkable polymer" is a polymer that contains crosslinkable sites, such as carbon-carbon multiple bonds, halogen functional groups, or hydrocarbon moieties, and that forms an elastomer upon crosslinking. This term is used interchangeably with the term "elastomer precursor."

[0034] For purposes of this invention, the term "rubber" refers to a crosslinkable polymer or elastomer precursor that can be converted into an elastomer by a curing reaction, for example by vulcanization.

[0035] The term "glass transition temperature" in the sense of the present invention refers to the temperature at which a glass transition occurs, which is a reversible transition in an amorphous material (or in amorphous regions within a semi-crystalline material) from a hard, relatively brittle state to a molten or rubbery state. The glass transition temperature is always lower than the melting point of the crystalline state of the material, if it exists. The term "melting point" in the sense of the present invention refers to the temperature at which a solid changes from a solid to a liquid state at atmospheric pressure. At the melting point, the solid and liquid phases exist in equilibrium. The glass transition temperature and melting point are determined according to ISO 11357 at a heating rate of 10°C / min.

[0036] For purposes of this application, a "water-insoluble" material is defined as a material that, when 100 g of the material is mixed with 100 g of deionized water and filtered at 20° C. on a filter having a 0.2 mm pore size to recover a liquid filtrate, followed by evaporation of 100 g of the liquid filtrate at 95-100° C. at ambient pressure, gives 1 g or less of recovered solid material. A "water-soluble" material is defined as a material that, when 100 g of the material is mixed with 100 g of deionized water and filtered at 20° C. on a filter having a 0.2 mm pore size to recover a liquid filtrate, followed by evaporation of 100 g of the liquid filtrate at 95-100° C. at ambient pressure, gives more than 1 g of recovered solid material.

[0037] The term "surface reaction" in the sense of the present application shall be used to indicate that a material has been subjected to a process involving partial dissolution of this material in an aqueous environment, followed by a crystallization process at and around the surface of this material, which may occur in the absence or presence of further crystallization additives.

[0038] The term "surface treatment" in the sense of the present invention refers to a material that has been brought into contact with a surface treatment agent in such a way that a coating layer is obtained on at least part of the surface of this material.

[0039] In this specification, the "particle size" of particulate matter other than surface-reacted calcium carbonate and precipitated hydromagnesite is defined as the particle size distribution by weight, d xwhere d x is the weight percent of particles that is d x This refers to a diameter that is less than d 20 A value of d means that 20% by weight of all particles have a particle size smaller than that particle size. 50 The value is the weight median particle size, i.e., 50% by weight of all particles are smaller than this particle size. For the purposes of this invention, unless otherwise specified, particle size is referred to as the weight median particle size d 50 Particle size is defined as (wt). Particle size was determined using a Sedigraph® 5120 instrument from Micromeritics Instrument Corporation. This method and instrument is known to those skilled in the art and is commonly used to determine particle size of fillers and pigments. Measurements were made in an aqueous solution of 0.1 wt% Na4P2O7.

[0040] As used herein, the "particle size" of surface-reacted calcium carbonate or precipitated hydromagnesite is described as a volumetric particle size distribution. The volumetric median particle size d 50 was assessed using a Malvern Mastersizer 3000 Laser Diffraction System. 50 or d 98 indicates the diameter value at which 50% or 98% by volume of the particles have a diameter smaller than this value, respectively. The raw data obtained by the measurement are analyzed using Mie theory, assuming a particle refractive index of 1.57 and an absorption coefficient of 0.005.

[0041] A "salt" in the sense of the present invention is a compound consisting of an assembly of cations and anions (see IUPAC, Compendium of Chemical Terminology, 2nd Ed. ("Gold Book"), 1997, "Salts").

[0042] The "specific surface area" (m 2The total surface area (m² / g) of the material can be determined by the Brunauer-Emmett-Teller (BET) method using nitrogen as the adsorbed gas, using an ASAP 2460 instrument from Micromeritics. This method is well known to those skilled in the art and is defined in ISO 9277:2010. The sample is conditioned at 100°C for 30 minutes under vacuum before the measurement. 2 ) can be obtained by multiplying the specific surface area of ​​the material by its mass (g).

[0043] For the purposes of the present invention, the "solids content" of a liquid composition is a measure of the amount of material remaining after all solvent or water has evaporated. If desired, the "solids content" of a suspension given in % by weight within the meaning of the present invention can be determined using a Mettler-Toledo Moisture Analyzer HR73 (T=120°C, automatic switch-off 3, standard drying) with a sample size of 5-20 g.

[0044] Unless otherwise specified, the term "drying" refers to a process in which at least a portion of the water is removed from the material being dried, such that the resulting "dry" material reaches a constant weight at 105°C. Furthermore, a "dry" or "dry" material can be defined by its total moisture content, which may depend on the calcium carbonate- or magnesium carbonate-containing material used in the composition. Generally, a "dry" or "dry" material can be defined by its total moisture content being 2% by weight or less, preferably 1.5% by weight or less, more preferably 1.2% by weight or less, and most preferably 0.005-0.8% by weight, based on the total weight of the dry material, unless otherwise specified. This is particularly applicable when the calcium carbonate-containing material is selected from among heaped ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), and mixtures thereof. When the calcium carbonate-comprising material is surface-reacted calcium carbonate or the magnesium carbonate-comprising material is precipitated hydromagnesite, the "dry" or "dry" material preferably has a residual total moisture content of 0.01 wt. % to 10 wt. %, preferably 0.01 wt. % to 8 wt. %, more preferably 0.02 wt. % to 6 wt. %, and most preferably 0.03 wt. % to 4 wt. %, based on the total dry weight of the at least one calcium carbonate- or magnesium carbonate-comprising material.

[0045] For purposes of the present invention, the term "viscosity" or "Brookfield viscosity" refers to Brookfield viscosity. Brookfield viscosity for this purpose can be measured with a Brookfield DV-II+Pro viscometer at 25°C ± 1°C and 100 rpm using the appropriate spindle of a Brookfield RV-spindle set, and is specified in mPa·s or cPs. A person skilled in the art will select a spindle from the Brookfield RV-spindle set appropriate for the viscosity range to be measured based on their technical knowledge. For example, for a Brookfield viscosity range of 200 to 800 mPa·s, spindle number 3 can be used; for a viscosity range of 400 to 1600 mPa·s, spindle number 4 can be used; for a viscosity range of 800 to 3200 mPa·s, spindle number 5 can be used; for a viscosity range of 1000 to 2,000,000 mPa·s, spindle number 6 can be used; and for a viscosity range of 4,000 to 8,000,000 mPa·s, spindle number 7 can be used.

[0046] A "suspension" or "slurry" in the sense of the present invention comprises undissolved solids and water, and optionally further additives, and typically contains a large amount of solids and may therefore be more viscous and denser than the liquid from which it is formed.

[0047] The term "aqueous" suspension refers to a system in which the liquid phase comprises, and preferably consists of, water. However, this term does not exclude that the liquid phase of the aqueous suspension may contain a small amount of at least one water-miscible organic solvent selected from the group consisting of methanol, ethanol, acetone, acetonitrile, tetrahydrofuran, and mixtures thereof. When the aqueous suspension contains at least one water-miscible organic solvent, the liquid phase of the aqueous suspension contains the at least one water-miscible organic solvent in an amount of 0.1 to 40.0 wt.%, preferably 0.1 to 30.0 wt.%, more preferably 0.1 to 20.0 wt.%, and most preferably 0.1 to 10.0 wt.%, based on the total weight of the liquid phase of the aqueous suspension. For example, the liquid phase of the aqueous suspension may consist of water.

[0048] Where an indefinite or definite article is used when referring to a singular noun e.g. "a", "an" or "the", this includes a plural of that noun unless otherwise stated.

[0049] Where the term "comprising" is used in the present specification and claims, it does not exclude other elements. For the purposes of the present invention, the term "consisting of" is considered to be a preferred embodiment of the term "comprising". Hereinafter, when a group is defined to include at least a certain number of embodiments, this is to be understood as also disclosing a group that preferably consists only of these embodiments.

[0050] Terms such as "obtainable" or "defined" and "obtained" or "defined" are used interchangeably. For example, this does not mean that the term "obtained" indicates that, for example, an embodiment must be obtained by the sequence of steps that follows the term "obtained," unless the context clearly dictates otherwise, but that such a limited understanding is always included in the terms "obtained" or "defined," as a preferred embodiment.

[0051] When the terms "including" or "having" are used, these terms are meant to be equivalent to "comprising" as defined above.

[0052] The composition of the present invention is formed from a calcium carbonate or magnesium carbonate-containing material selected from the group consisting of heaped ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), surface-reacted calcium carbonate (SRCC), precipitated hydromagnesite, and mixtures thereof, and a surface treatment composition comprising 0.5 to 10 wt %, based on the total weight of the calcium carbonate or magnesium carbonate-containing material, of at least one crosslinking compound containing at least two functional groups, wherein at least one functional group is suitable for crosslinking an elastomeric resin and at least one functional group is suitable for reacting with the calcium carbonate or magnesium carbonate-containing material.

[0053] Preferred embodiments of the products of the invention are described in more detail below, with the understanding that these embodiments and details also apply to the inventive methods for their preparation and their use described herein.

[0054] Calcium carbonate or magnesium carbonate containing materials The compositions of the present invention are formed from raw materials comprising calcium or magnesium carbonate selected from the group consisting of heaped ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), surface-reacted calcium carbonate (SRCC), precipitated hydromagnesite, and mixtures thereof.

[0055] In one embodiment, the composition is formed from a calcium carbonate-comprising material that is a deposited ground calcium carbonate (GCC) and / or a precipitated calcium carbonate (PCC) or a surface-reacted calcium carbonate (SRCC). Preferably, the composition is formed from a calcium carbonate-comprising material that is a deposited ground calcium carbonate (GCC) or a precipitated calcium carbonate (PCC) or a surface-reacted calcium carbonate (SRCC). More preferably, the composition is formed from a calcium carbonate-comprising material that is a deposited ground calcium carbonate (GCC) or a precipitated calcium carbonate (PCC). Most preferably, the composition is formed from a calcium carbonate-comprising material that is a deposited ground calcium carbonate (GCC).

[0056] Alternatively, the composition is formed from a magnesium carbonate-containing material that is precipitated hydromagnesite.

[0057] However, it is preferred that the composition be formed from a calcium carbonate-containing material.

[0058] The calcium carbonate or magnesium carbonate-containing material can be provided in any suitable dry form. For example, the calcium carbonate or magnesium carbonate-containing material may be in the form of a powder and / or in a pressed or granulated form. For example, when the calcium carbonate-containing material is a heaped ground calcium carbonate (GCC) and / or a precipitated calcium carbonate (PCC), the residual total moisture content is preferably ≦2 wt. %, more preferably ≦1.5 wt. %, even more preferably ≦1.2 wt. %, and most preferably ≦0.8 wt. %, based on the total dry weight of the at least one calcium carbonate-containing material. Additionally or alternatively, the residual total moisture content is preferably ≧0.001 wt. %, more preferably ≧0.002 wt. %, and most preferably ≧0.005 wt. %, based on the total dry weight of the at least one calcium carbonate-containing material.

[0059]

[0044] In one embodiment, the total residual moisture content is preferably 0.001 wt.-% to 2 wt.-%, preferably 0.001 wt.-% to 1.5 wt.-%, more preferably 0.002 wt.-% to 1.2 wt.-%, and most preferably 0.005 wt.-% to 0.8 wt.-%, based on the total dry weight of the at least one calcium carbonate-comprising material.

[0060] "Ground calcium carbonate (GCC)" in the sense of the present invention (also called "sediment ground calcium carbonate") is calcium carbonate obtained from sedimentary sources such as marble, limestone, dolomite, chalk and / or mixtures thereof and processed by wet and / or dry processes such as grinding, screening and / or fractionation, for example by means of a cyclone or classifier. The term "sediment" ground calcium carbonate refers to calcium carbonate formed by the accumulation or precipitation of calcium carbonate particles and their subsequent cementation on the bed of the ocean or other body of water at the earth's surface.

[0061] According to one embodiment, the sedimentary ground calcium carbonate (GCC) is selected from the group consisting of marble, limestone, dolomite, chalk, and mixtures thereof. The ground calcium carbonate may contain further components present in the sedimentary source, such as magnesium carbonate, aluminosilicates, etc. Therefore, it is understood that the term "ground" calcium carbonate does not refer to calcium carbonate obtained by milling, but rather to calcium carbonate of sedimentary origin.

[0062] "Dolomite" is a calcium carbonate-containing mineral, i.e., a calcium-magnesium carbonate-mineral, having the chemical composition CaMg(CO3)2 ("CaCO3·MgCO3"). Dolomite minerals can contain at least 30.0 wt. %, preferably greater than 35.0 wt. %, and more preferably greater than 40.0 wt. % MgCO3, based on the total weight of the dolomite.

[0063] Generally, the grinding of the sedimentary ground calcium carbonate can be a dry or wet grinding process and can be carried out in any conventional grinding equipment, for example, in one or more of a ball mill, rod mill, vibratory mill, roll crusher, centrifugal impact mill, vertical bead mill, attrition mill, pin mill, hammer mill, crusher, shredder, declamper, knife cutter, or other such equipment known to those skilled in the art, under conditions such that grinding occurs primarily as a result of impact with secondary objects. When the calcium carbonate-containing material comprises a wet-ground calcium carbonate-containing mineral material, the grinding process can be carried out under conditions such that autogenous grinding occurs and / or by horizontal and / or vertical ball mill grinding and / or by other such methods known to those skilled in the art. The wet-processed ground calcium carbonate-containing material thus obtained can be washed and dewatered by known methods, for example, by agglomeration, filtration, or forced evaporation, before drying. The subsequent drying step (if required) can be carried out in a one-stage process, such as spray drying, or in at least two stages. Such mineral materials also typically undergo a beneficiation process (flotation, bleaching, or magnetic separation) to remove impurities.

[0064] In the sense of the present invention, "precipitated calcium carbonate" (PCC) is a synthetic material generally obtained by precipitation after the reaction of carbon dioxide with calcium hydroxide in an aqueous, semi-arid, or humid environment, or by precipitation from a solution of calcium ions and carbonate ions, e.g., CaCl2 and Na2CO3. Further possible methods for PCC production are the lime-soda process or the Solvay process, in which PCC is a by-product of ammonia production. Precipitated calcium carbonate exists in three primary crystalline forms: calcite, aragonite, and vaterite, with many different polymorphs (crystal habits) for each of these crystalline forms. Calcite has a trigonal structure with typical crystal habits such as scalenohedral (S-PCC), rhombohedral (R-PCC), hexagonal prismatic, tabletop, colloidal (C-PCC), cubic, and prismatic (P-PCC). Aragonite has an orthorhombic structure with a typical crystal habit of twinned hexagonal prisms, as well as a variety of thin, elongated prisms, curved blades, steeply sloped pyramids, chisel-like crystals, branched tree forms, and coral- or worm-like morphologies. Vaterite belongs to the hexagonal crystal system. The resulting PCC slurry can be mechanically dewatered and dried. PCC is described, for example, in EP 2 447 213 A1, EP 2 524 898 A1, EP 2 371 766 A1, EP 1 712 597 A1, EP 1 712 523 A1, or WO 2013 / 142473 A1. According to one embodiment of the present invention, the precipitated calcium carbonate is preferably a precipitated calcium carbonate selected from the group consisting of the mineral crystal forms of aragonite, vaterite and calcite, colloidal PCC, and mixtures thereof.

[0065] According to one embodiment, the sedimentary ground calcium carbonate (GCC) is selected from the group consisting of marble, limestone, dolomite, chalk and mixtures thereof, or the precipitated calcium carbonate (PCC) is selected from the group consisting of mineral crystal forms of aragonite, vaterite and calcite, colloidal PCC, and mixtures thereof.

[0066] Preferably, the calcium carbonate-comprising material is a heapedial ground calcium carbonate (GCC) such as marble, limestone or chalk. More preferably, the calcium carbonate-comprising material is a heapedial ground calcium carbonate (GCC) such as marble or limestone. Most preferably, the calcium carbonate-comprising material is a heapedial ground calcium carbonate (GCC) that is marble.

[0067] When the calcium carbonate-comprising material is a deposited ground calcium carbonate (GCC) and / or precipitated calcium carbonate (PCC), the calcium carbonate-comprising material preferably has a weight median particle size d measured by the sedimentation method in the range of 0.1 μm to 10 μm, preferably in the range of 0.15 μm to 5 μm, more preferably in the range of 0.2 μm to 3 μm, most preferably in the range of 0.25 μm to 3 μm, e.g., 0.3 μm to 2 μm or 0.3 μm to 1.5 μm. 50 It has.

[0068] Additionally or alternatively, the calcium carbonate-comprising material, which is a deposited ground calcium carbonate (GCC) and / or precipitated calcium carbonate (PCC), has a top cut (d as measured by the sedimentation method) of ≦45 μm, preferably ≦30 μm, more preferably ≦20 μm, and most preferably ≦15 μm. 98 )

[0069] In a preferred embodiment, the calcium carbonate-containing material, which is heaped ground calcium carbonate (GCC) and / or precipitated calcium carbonate (PCC), has a weight median particle size d measured by the sedimentation method in the range of 0.1 μm to 10 μm, preferably in the range of 0.15 μm to 5 μm, more preferably in the range of 0.2 μm to 3 μm, and most preferably in the range of 0.25 μm to 3 μm, for example in the range of 0.3 μm to 2 μm or 0.3 μm to 1.5 μm. 50 and a top cut (d) measured by sedimentation method of ≦45 μm, preferably ≦30 μm, more preferably ≦20 μm, and most preferably ≦15 μm 98 )

[0070] Additionally or alternatively, the calcium carbonate-containing material, which is ground calcium carbonate (GCC) and / or precipitated calcium carbonate (PCC), has a pH of 0.5 to 150 m as measured using nitrogen and the BET method according to ISO 9277:2010. 2 / g, preferably 1 to 80m 2 / g, more preferably 2 to 50m 2 / g, and even more preferably 2 to 40 m 2 / g, most preferably 3 to 25m 2 / g, e.g., 6 to 25 m 2 / g specific surface area.

[0071] In a preferred embodiment, the calcium carbonate-comprising material, which is a deposited ground calcium carbonate (GCC) and / or a precipitated calcium carbonate (PCC), has a weight median particle size d measured by the precipitation method. 50 is in the range of 0.1 μm to 10 μm, preferably in the range of 0.15 μm to 5 μm, more preferably in the range of 0.2 μm to 3 μm, most preferably in the range of 0.25 μm to 3 μm, for example, 0.3 μm to 2 μm or 0.3 μm to 1.5 μm, and the top cut (d 98 ) is ≦45 μm, preferably ≦30 μm, more preferably ≦20 μm, most preferably ≦15 μm, and the specific surface area (BET), measured using nitrogen and the BET method according to ISO 9277:2010, is between 0.5 and 150 m 2 / g, preferably 1 to 80m 2 / g, more preferably 2 to 50m 2 / g, and even more preferably 2 to 40 m 2 / g, most preferably 3 to 25m 2 / g, e.g., 6 to 25 m 2 / g.

[0072] Additionally or alternatively, the calcium carbonate-comprising material being a deposited ground calcium carbonate (GCC) and / or a precipitated calcium carbonate (PCC) has a residual total moisture content of ≦2 wt.-%, more preferably ≦1.5 wt.-%, even more preferably ≦1.2 wt.-%, and most preferably ≦0.8 wt.-%, based on the total dry weight of the at least one calcium carbonate-comprising material.

[0073] For example, the calcium carbonate-containing material is a ground calcium carbonate (GCC) and / or a precipitated calcium carbonate (PCC) and has: (i) a weight median particle size d measured by a precipitation method in the range of 0.1 μm to 10 μm, preferably in the range of 0.15 μm to 5 μm, more preferably in the range of 0.2 μm to 3 μm, and most preferably in the range of 0.25 μm to 3 μm, for example, 0.3 μm to 2 μm or 0.3 μm to 1.5 μm; 50 , or (ii) a top cut (d) measured by sedimentation method of ≦45 μm, preferably ≦30 μm, more preferably ≦20 μm, and most preferably ≦15 μm 98 ), or (iii) Nitrogen and 0.5 to 150 m, measured using the BET method according to ISO 9277:2010 2 / g, preferably 1 to 80m 2 / g, more preferably 2 to 50m 2 / g, and even more preferably 2 to 40 m 2 / g, most preferably 3 to 25m 2 / g, e.g., 6 to 25 m 2 / g specific surface area (BET), or (iv) a total residual moisture content of ≦2 wt.-%, more preferably ≦1.5 wt.-%, even more preferably ≦1.2 wt.-%, and most preferably ≦0.8 wt.-%, based on the total dry weight of the at least one calcium carbonate-comprising material.

[0074] Alternatively, the calcium carbonate-containing material is a ground calcium carbonate (GCC) and / or a precipitated calcium carbonate (PCC) and has: (i) a weight median particle size d measured by a precipitation method in the range of 0.1 μm to 10 μm, preferably in the range of 0.15 μm to 5 μm, more preferably in the range of 0.2 μm to 3 μm, and most preferably in the range of 0.25 μm to 3 μm, for example, 0.3 μm to 2 μm or 0.3 μm to 1.5 μm; 50 , and (ii) a top cut (d) measured by sedimentation method of ≦45 μm, preferably ≦30 μm, more preferably ≦20 μm, and most preferably ≦15 μm 98 ), and (iii) Nitrogen and 0.5 to 150 m, measured using the BET method according to ISO 9277:2010 2 / g, preferably 1 to 80m 2 / g, more preferably 2 to 50m 2 / g, and even more preferably 2 to 40 m 2 / g, most preferably 3 to 25m 2 / g, e.g., 6 to 25 m 2 / g specific surface area (BET), and (iv) a total residual moisture content of ≦2 wt.-%, more preferably ≦1.5 wt.-%, even more preferably ≦1.2 wt.-%, and most preferably ≦0.8 wt.-%, based on the total dry weight of the at least one calcium carbonate-comprising material.

[0075] According to one embodiment, the calcium carbonate-containing material is surface-reacted calcium carbonate (SRCC), which is a mixture of (sedimentary) ground or precipitated calcium carbonate with carbon dioxide and one or more HO. + The carbon dioxide is a reaction product with the ion donor, and this carbon dioxide is converted into HO + Preferably, the surface-reacted calcium carbonate is formed in situ by treatment with an ion donor. Preferably, the surface-reacted calcium carbonate is formed by treating (sedimentary) ground or precipitated calcium carbonate with carbon dioxide and one or more ions of HO. + The carbon dioxide is a reaction product with the ion donor, and this carbon dioxide is converted into HO + It is formed in situ by treatment with an ion donor.

[0076] In the context of the present invention, HO + The ion donor is a Bronsted acid and / or an acid salt.

[0077] In a preferred embodiment of the present invention, the surface-reacted calcium carbonate is obtained by a process comprising the following steps: (a) providing a suspension of (sediment) ground calcium carbonate or precipitated calcium carbonate; (b) a pK of 0 or less at 20°C a or a pK value of 0 to 2.5 at 20°C a adding at least one acid having a value of (c) treating the suspension of step (a) with carbon dioxide before, during, or after step (b). According to another embodiment, the surface-reacted calcium carbonate is obtained by a process comprising the following steps: (A) providing (sediment) ground calcium carbonate or precipitated calcium carbonate; (B) providing at least one water-soluble acid; (C) providing CO2 gas; (D) contacting the (sediment) ground or precipitated calcium carbonate of step (A) with at least one acid of step (B) and CO of step (C); wherein the method is characterized by: (i) at least one acid of step (B) has a pK, relative to the ionization of its first available hydrogen, greater than 2.5 and less than 7 at 20°C; a and the corresponding anion is formed upon loss of this first available hydrogen capable of producing a water-soluble calcium salt; and (ii) after contact of at least one acid with the (sedimentary) ground calcium carbonate or precipitated calcium carbonate, the hydrogen-containing salt has a pK of greater than 7 at 20°C in relation to the ionization of its first available hydrogen; a and if the salt anion is capable of forming a water-insoluble calcium salt, additionally providing at least one water-soluble salt.

[0078] The precipitated calcium carbonate is ground by the same means as those used to grind the (sediment) ground calcium carbonate described above, with carbon dioxide and at least one HO. + It can be milled before treatment with the ion donor.

[0079] According to one embodiment of the present invention, the (sedimentary) ground calcium carbonate or precipitated calcium carbonate has a weight median particle size d of 0.05 to 10.0 μm, preferably 0.1 to 5.0 μm, more preferably 0.2 to 3.0 μm, even more preferably 0.3 to 1.2 μm, and most preferably 0.3 to 0.4 μm. 50 According to a further embodiment of the present invention, the (sedimentary) ground calcium carbonate or precipitated calcium carbonate has a top cut particle size d of 0.15 to 55 μm, preferably 1 to 40 μm, more preferably 2 to 25 μm, most preferably 3 to 15 μm, in particular 3 μm. 98 The particle is in the form of a particle having the formula:

[0080] The (sedimentary) ground calcium carbonate and / or precipitated calcium carbonate can be used in the dry state or suspended in water. Preferably, the corresponding slurry has a content of (sedimentary) ground calcium carbonate or precipitated calcium carbonate in the range of 1% to 90% by weight, more preferably 3% to 60% by weight, even more preferably 5% to 40% by weight, and most preferably 10% to 25% by weight, based on the weight of the slurry.

[0081] One or more H3Os used in the production of surface-reacted calcium carbonate + The ion donor is HO under manufacturing conditions. + The acid may be any strong, medium-strong, or weak acid that generates ions, or a mixture thereof. According to the present invention, at least one HO + The ion donor is HO under manufacturing conditions. + It may also be an acid salt that generates ions.

[0082] According to one embodiment, at least one HO + The ion donor has a pK of 0 or less at 20°C. a It is a strong acid having the formula:

[0083] According to another embodiment, at least one HO + The ion donor has a pK of 0 to 2.5 at 20°C.a It is a moderately strong acid with a pK at 20°C a When pK at 20°C is 0 or less, the acid is preferably selected from sulfuric acid, hydrochloric acid, or a mixture thereof. a If is between 0 and 2.5, H3O + The ion donor is preferably selected from H2SO3, H3PO4, oxalic acid, or a mixture thereof. + The ion donor is an acid salt, e.g., Li + , Na + Or K + HSO4 that is at least partially neutralized by the corresponding cation such as - or H2PO4 - , or Li + , Na + , K. + , Mg 2+ or Ca 2+ HPO4 that has been at least partially neutralized by the corresponding cation such as 2- At least one H3O + The ion donor may be a mixture of one or more acids and one or more acid salts.

[0084] According to yet another embodiment, at least one HO + The ion donor has a pK, relative to the ionization of its first available hydrogen, greater than 2.5 and less than or equal to 7, when measured at 20°C. a A weak acid having a pK value greater than 7, relative to the ionization of its first available hydrogen, when measured at 20°C, and a corresponding anion capable of forming a water-soluble calcium salt. a and the salt anion is capable of forming a water-insoluble calcium salt, and additionally provides at least one water-soluble salt. According to a preferred embodiment, the weak acid has a pK of greater than 2.5 to 5 at 20°C. aPreferably, the weak acid is selected from the group consisting of acetic acid, formic acid, propanoic acid, and mixtures thereof. Exemplary cations of the water-soluble salt are selected from the group consisting of potassium, sodium, lithium, and mixtures thereof. In a more preferred embodiment, the cation is sodium or potassium. Exemplary anions of the water-soluble salt are selected from the group consisting of phosphate, dihydrogen phosphate, monohydrogen phosphate, oxalate, silicate, mixtures thereof, and hydrates thereof. In a more preferred embodiment, the anion is selected from the group consisting of phosphate, dihydrogen phosphate, monohydrogen phosphate, mixtures thereof, and hydrates thereof. In a most preferred embodiment, the anion is selected from the group consisting of dihydrogen phosphate, monohydrogen phosphate, mixtures thereof, and hydrates thereof. The addition of the water-soluble salt can be carried out dropwise or in one step. In the case of dropwise addition, the addition is preferably carried out within a period of 10 minutes. It is more preferred to add the salt in one step.

[0085] According to one embodiment of the present invention, at least one HO + The ion donor is selected from the group consisting of hydrochloric acid, sulfuric acid, sulfurous acid, phosphoric acid, citric acid, oxalic acid, acid salts, acetic acid, formic acid, and mixtures thereof. Preferably, at least one HO + Ion donors are hydrochloric acid, sulfuric acid, sulfurous acid, phosphoric acid, and oxalic acid; Li + , Na + or K + H2PO4 that is at least partially neutralized by the corresponding cation, such as - ;Li + , Na + , K. + , Mg 2+ or Ca 2+ HPO4 that has been at least partially neutralized by the corresponding cation such as 2- and mixtures thereof, more preferably the at least one acid is selected from the group consisting of hydrochloric acid, sulfuric acid, sulfurous acid, phosphoric acid, oxalic acid, and mixtures thereof, and most preferably at least one HO+ The ion donor is phosphoric acid.

[0086] One or more H3O + The ion donor can be added to the suspension as a concentrated solution or as a more dilute solution. Preferably, HO for (sedimentary) ground calcium carbonate or precipitated calcium carbonate. + The molar ratio of the ion donor is 0.01 to 4, more preferably 0.02 to 2, even more preferably 0.05 to 1, and most preferably 0.1 to 0.58.

[0087] Alternatively, the ground or precipitated calcium carbonate may be added to the suspension in water prior to suspending it. + It is also possible to add an ion donor to the water.

[0088] In a preferred embodiment, the surface-reacted calcium carbonate is prepared by reacting ground calcium carbonate with carbon dioxide and one or more HO in an aqueous medium (sediment). + The carbon dioxide is a reaction product with the ion donor, and this carbon dioxide is converted into HO + Formed in situ by treatment with an ion donor and HO + In a more preferred embodiment, the surface-reacted calcium carbonate is prepared by reacting a calcium carbonate-containing mineral selected from the group consisting of marble, chalk, limestone, and mixtures thereof with carbon dioxide and one or more HO in an aqueous medium. + The carbon dioxide is a reaction product with the ion donor, and this carbon dioxide is converted into HO + Formed in situ by treatment with an ion donor and HO + The ion donor is phosphoric acid.

[0089] In the next step, the ground or precipitated calcium carbonate is treated with carbon dioxide. A strong acid, such as sulfuric acid or hydrochloric acid, is added to the ground or precipitated calcium carbonate. + When used for treatment with an ion donor, carbon dioxide is generated automatically. Alternatively or additionally, carbon dioxide can be supplied from an external source.

[0090] H3O + Treatment with the ion donor and treatment with carbon dioxide can be carried out simultaneously when a strong or moderately strong acid is used. For example, when a strong acid has a pK in the range of 0 to 2.5 at 20°C, a First, using a medium-strong acid with + Treatment with an ion donor is also possible, where carbon dioxide is formed in situ, and thus treatment with carbon dioxide can be used to convert HO + This is done automatically in conjunction with treatment with the ion donor, followed by an additional treatment with carbon dioxide supplied from an external source.

[0091] In a preferred embodiment, HO + The ion donor treatment step and / or the carbon dioxide treatment step are repeated at least once, more preferably multiple times. According to one embodiment, at least one HO + The ion donor is added over a period of at least about 5 minutes, preferably at least about 10 minutes, typically from about 10 minutes to about 20 minutes, more preferably about 30 minutes, even more preferably about 45 minutes, and sometimes about 1 hour or more.

[0092] H3O + After treatment with the ion donor and treatment with carbon dioxide, the pH of the aqueous suspension, measured at 20°C, spontaneously reaches a value greater than 6.0, preferably greater than 6.5, more preferably greater than 7.0, even more preferably greater than 7.5, thereby producing surface-reacted (sedimented) ground calcium carbonate or surface-reacted precipitated calcium carbonate as an aqueous suspension having a pH greater than 6.0, preferably greater than 6.5, more preferably greater than 7.0, even more preferably greater than 7.5.

[0093] Further details about the production of surface-reacted (sedimented) ground calcium carbonate are disclosed in WO 00 / 39222 A1, WO 2004 / 083316 A1, WO 2005 / 121257 A2, WO 2009 / 074492 A1, EP 2 264 108 A1, EP 2 264 109 A1, and U.S. 2004 / 0020410 A1, the contents of these references being incorporated herein by reference.

[0094] Similarly, surface-reacted precipitated calcium carbonate is obtained. As can be seen in detail from WO 2009 / 074492 A1, surface-reacted precipitated calcium carbonate is obtained by reacting precipitated calcium carbonate with HO. + The surface-reacted precipitated calcium carbonate is obtained by contacting, in an aqueous medium, an insoluble and at least partially crystalline calcium salt of said anion formed on the surface of at least a portion of the precipitated calcium carbonate, with an anion capable of being solubilized in the aqueous medium and producing a water-insoluble calcium salt thereof, to form a slurry of surface-reacted precipitated calcium carbonate, wherein the surface-reacted precipitated calcium carbonate comprises an insoluble and at least partially crystalline calcium salt of said anion formed on the surface of at least a portion of the precipitated calcium carbonate.

[0095] The solubilized calcium ions are dissolved in HO + corresponds to excess solubilized calcium ions compared to the solubilized calcium ions naturally produced by dissolution of precipitated calcium carbonate by HO. + The ions are provided exclusively in the form of counterions to the anions, i.e., via addition of the anions in the form of acids or non-calcium salts, and in the absence of any further calcium ions or calcium ion generating sources.

[0096] The excess solubilized calcium ions are preferably provided by the addition of a soluble neutral or acidic calcium salt, or by the addition of an acid or a neutral or acidic non-calcium salt that generates a soluble neutral or acidic calcium salt in situ.

[0097] Above H3O + The ions may be provided by the addition of an acid or acid salt of the anion, or by the addition of an acid or acid salt which simultaneously acts to provide all or a portion of the excess solubilized calcium ions.

[0098] In a further preferred embodiment of the production of surface-reacted (sedimented) ground or precipitated calcium carbonate, the (sedimented) ground or precipitated calcium carbonate is treated with one or more HO in the presence of at least one compound selected from the group consisting of silicates, silica, aluminum hydroxide, alkaline earth aluminates such as sodium or potassium aluminate, magnesium oxide, or mixtures thereof. + The at least one silicate is preferably selected from aluminum silicate, calcium silicate, or alkaline earth metal silicate. These components are reacted with one or more HO + Prior to the addition of the ion donor and / or carbon dioxide, (sediment) can be added to the aqueous suspension comprising ground or precipitated calcium carbonate.

[0099] Alternatively, (sedimentary) ground or precipitated calcium carbonate and one or more H₃O + One or more components of silicate and / or silica and / or aluminum hydroxide and / or alkaline earth aluminate and / or magnesium oxide can be added to the aqueous suspension of (sediment) ground or precipitated calcium carbonate while the reaction with the ion donor and carbon dioxide has already begun. Further details about the production of surface-reacted (sediment) ground or precipitated calcium carbonate in the presence of at least one component of silicate and / or silica and / or aluminum hydroxide and / or alkaline earth aluminate are disclosed in WO 2004 / 083316 A1, the content of which is incorporated herein by reference.

[0100] The aqueous suspension comprising the surface-reacted calcium carbonate is dried to obtain the solid surface-reacted calcium carbonate in the form of granules or powder. Suitable drying methods are known to those skilled in the art.

[0101] When the surface-reacted calcium carbonate is dried, the total residual moisture content of the dried surface-reacted calcium carbonate can be 0.01 to 10 wt. %, based on the total weight of the dried surface-reacted calcium carbonate. According to one embodiment, the total residual moisture content of the dried surface-reacted calcium carbonate is 10 wt. % or less, preferably 8 wt. % or less, more preferably 6 wt. % or less, and most preferably 4 wt. % or less, based on the total weight of the dried surface-reacted calcium carbonate. According to another embodiment, the total residual moisture content of the dried surface-reacted calcium carbonate is 0.01 to 10 wt. %, preferably 0.01 to 8 wt. %, more preferably 0.02 to 6 wt. %, and most preferably 0.03 to 4 wt. %, based on the total dry weight of the at least one calcium carbonate- or magnesium carbonate-containing material.

[0102] The surface-reacted calcium carbonate may have different particle shapes, such as, for example, the shape of a rose, a golf ball, and / or a brain.

[0103] In a preferred embodiment, the surface-reacted calcium carbonate has a surface-reacted pH of 15 m as measured using nitrogen and BET methods. 2 / g~200m 2 / g, preferably 20m 2 / g~180m 2 / g, more preferably 25m 2 / g~140m 2 / g, and even more preferably 27m 2 / g~120m 2 / g, most preferably 30m 2 / g~100m 2 For example, surface-reacted calcium carbonate has a specific surface area of ​​75 m / g, as measured using nitrogen and BET methods. 2 / g~100m 2 / g. BET specific surface area in the sense of the present invention is defined as the surface area of ​​a particle divided by the mass of the particle. As used herein, specific surface area is measured by adsorption using the BET isotherm (ISO 9277:2010) and is expressed as m 2 It is specified in units of / g.

[0104] The surface-reacted calcium carbonate particles have a volume median particle size d of 0.1 to 75 μm, preferably 0.5 to 50 μm, more preferably 1 to 40 μm, even more preferably 1.2 to 30 μm, and most preferably 1.5 to 15 μm. 50 It is more preferred that the carboxyl group has (vol).

[0105] According to one embodiment, the surface-reacted calcium carbonate particles have a volume top cut particle size d of 0.2 to 150 μm, preferably 1 to 100 μm, more preferably 2 to 80 μm, even more preferably 2.4 to 60 μm, and most preferably 3 to 30 μm. 98 It has.

[0106] d x is the diameter of x% of the particles x This means that the diameter is less than d 98 This means that 98% of all particles have a particle size smaller than this value. 98 The value is also called the "top cut." x can be given in volume or weight percent. Thus, d 50 The (wt) value is the weight median particle size, i.e., the particle size below which 50% by weight of all particles are smaller, and d 50 The (vol) value is the volume median particle size, i.e. 50% by volume of all particles are smaller than this particle size.

[0107] Volume median particle size d 50 was evaluated using a Malvern Mastersizer 3000 Laser Diffraction System.50 or d 98 The values ​​indicate the diameter values ​​at which 50% or 98% by volume of the particles have a diameter smaller than this value, respectively. The raw data obtained by the measurement are analyzed using Mie theory, assuming a particle refractive index of 1.57 and an absorption coefficient of 0.005.

[0108] The weight median particle size is determined by the sedimentation method, which is an analysis of sedimentation behavior in a gravimetric field. Measurements are performed using a Sedigraph® 5120 from Micromeritics Instrument Corporation. This method and instrument are known to those skilled in the art and are commonly used to determine particle size of fillers and pigments. Measurements are performed in an aqueous solution of 0.1 wt% Na4P2O7. The sample is dispersed using a high-speed stirrer and sonicated.

[0109] This method and equipment is known to those skilled in the art and is commonly used to determine particle size of fillers and pigments.

[0110] Specific pore volume is measured using mercury intrusion porosimetry using a Micromeritics Autopore V 9620 mercury porosimeter with a maximum applied pressure of 414 MPa (60,000 psi), equivalent to a Laplace throat diameter of 0.004 μm (~nm). An equilibration time of 20 seconds is used for each pressure step. Sample material is then loaded onto a 5 cm 3The powder is sealed in the chamber and the data are corrected for mercury compression, penetrometer expansion, and sample material compression using the software Pore-Comp (Gane, PAC, Kettle, JP, Matthews, GP, and Ridgway, CJ, "Void Space Structure of Compressible Polymer Spheres and Consolidated Calcium Carbonate Paper-Coating Formulations", Industrial and Engineering Chemistry Research, 35(5), 1996, pp. 1753-1764).

[0111] The total pore volume seen in the integrated intrusion data can be separated into two regions with intrusion data ranging from 214 μm down to approximately 1-4 μm, indicating a strong contribution from coarse packing of the sample between any aggregate structures. Below these diameters, there is fine interparticle packing of the particles themselves. If the particles also contain intraparticle pores, this region is bimodal, and the intraparticle specific pore volume is defined as the specific pore volume of mercury intruded into pores narrower than the inflection point of the bimodal transition. The sum of these three regions gives the total pore volume of the powder, but is heavily influenced by the precipitation of powder at the coarse pore end of the original sample compaction / distribution.

[0112] Taking the first derivative of the cumulative intrusion curve reveals a pore size distribution based on the equivalent Laplace diameter, which necessarily includes pore obscuration. The derivative curve clearly shows the coarse aggregate pore structure region, the interparticle pore region, and, if present, the intraparticle pore region. Once the intraparticle pore size range is known, it is possible to subtract the remaining interparticle and interaggregate pore volumes from the total pore volume to obtain only the desired pore volume of the internal pores as pore volume per unit mass (specific pore volume). Of course, the same subtraction principle applies to isolating any other pore size region of interest.

[0113] Preferably, the surface-reacted calcium carbonate has a thickness of 0.1 to 2.3 cm, as calculated from mercury porosimetry measurements. 3 / g, more preferably 0.2 to 2.0 cm 3 / g, particularly preferably 0.4 to 1.8 cm 3 / g, most preferably 0.6 to 1.6 cm 3 / g of indented specific pore volume.

[0114] The intraparticle pore diameter of the surface-reacted calcium carbonate, as determined by mercury porosimetry, is preferably 0.004 to 1.6 μm, more preferably 0.005 to 1.3 μm, particularly preferably 0.006 to 1.15 μm, most preferably 0.007 to 1.0 μm, for example, in the range of 0.02 to 0.6 μm.

[0115] According to one embodiment of the present invention, the calcium carbonate-comprising material comprises, preferably consists of, surface-reacted calcium carbonate (SRCC), wherein the (sedimentary) ground calcium carbonate is selected from the group consisting of marble, chalk, limestone, and mixtures thereof, or the precipitated calcium carbonate is selected from the group consisting of precipitated calcium carbonate having the aragonite, vaterite, or calcite crystalline form, and mixtures thereof.

[0116] According to a further embodiment, the calcium carbonate-comprising material comprises, preferably consists of, surface-reacted calcium carbonate (SRCC), and At least 1 H3O + the ion donor is selected from the group consisting of hydrochloric acid, sulfuric acid, sulfurous acid, phosphoric acid, citric acid, oxalic acid, acid salts, acetic acid, formic acid, and mixtures thereof; Preferably, at least one HO + Ion donors are hydrochloric acid, sulfuric acid, sulfurous acid, phosphoric acid, and oxalic acid; Li + , Na + and / or K + H2PO4 at least partially neutralized with a cation selected from - ;Li + , Na + , K. + , Mg2+ and / or Ca 2+ HPO4 at least partially neutralized with a cation selected from 2- and mixtures thereof; More preferably, at least one of said HO + the ion donor is selected from the group consisting of hydrochloric acid, sulfuric acid, sulfurous acid, phosphoric acid, oxalic acid, and mixtures thereof; Most preferably, at least one of said HO + The ion donor is phosphoric acid.

[0117] In one embodiment, the magnesium carbonate-containing material is precipitated hydromagnesite (Mg5(CO3)4(OH)2·4H2O). When the hydromagnesite is dried, the total residual moisture content of the dried precipitated hydromagnesite can be 0.01 to 10 wt. % based on the total weight of the dried precipitated hydromagnesite. According to one embodiment, the total residual moisture content of the dried precipitated hydromagnesite is 10 wt. % or less, preferably 8 wt. % or less, more preferably 6 wt. % or less, and most preferably 4 wt. % or less, based on the total dry weight of the dried precipitated hydromagnesite. According to another embodiment, the total residual moisture content of the dried precipitated hydromagnesite is 0.01 wt. % to 10 wt. %, preferably 0.01 wt. % to 8 wt. %, more preferably 0.02 wt. % to 6 wt. %, and most preferably 0.03 wt. % to 4 wt. % based on the total dry weight of the precipitated hydromagnesite. In a preferred embodiment, the precipitated hydromagnesite has a solubility of 15 m as measured using nitrogen and BET methods. 2 / g~200m 2 / g, preferably 20m 2 / g~180m 2 / g, more preferably 25m 2 / g~140m 2 / g, and even more preferably 27m 2 / g~120m 2 / g, most preferably 30m 2 / g~100m 2For example, precipitated hydromagnesite has a specific surface area of ​​75 m / g, as measured using nitrogen and BET methods. 2 / g~100m 2 / g specific surface area.

[0118] The precipitated hydromagnesite particles have a volume median particle size d of 0.1 to 75 μm, preferably 0.5 to 50 μm, more preferably 1 to 40 μm, even more preferably 1.2 to 30 μm, and most preferably 1.5 to 15 μm. 50 It is more preferred that the carboxyl group has (vol).

[0119] According to one embodiment, the precipitated hydromagnesite particles have a volume particle size d of 0.2 to 150 μm, preferably 1 to 100 μm, more preferably 2 to 80 μm, even more preferably 2.4 to 60 μm, and most preferably 3 to 30 μm. 95 , preferably volume top cut particle size d 98 It has.

[0120] Surface treatment composition The composition of the present invention is formed from a calcium carbonate- or magnesium carbonate-containing material and 0.5 to 10% by weight of a surface treatment composition based on the total weight of the calcium carbonate- or magnesium carbonate-containing material.

[0121] The surface treatment composition comprises at least one crosslinking compound comprising at least two functional groups, wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with said calcium carbonate or magnesium carbonate-containing material.

[0122] It is understood that a "surface treatment composition" comprises one or more surface treatment agents, and preferably consists of one or more surface treatment agents. For example, a "surface treatment composition" preferably comprises, and preferably consists of, one surface treatment agent. Alternatively, a "surface treatment composition" comprises, and preferably consists of, two or more, preferably two surface treatment agents, and preferably consists of two or more, preferably two surface treatment agents.

[0123] A "surface treatment agent" in the sense of the present invention is any substance capable of reacting with and / or forming an adduct with the surface of a calcium carbonate- or magnesium carbonate-containing material, thereby forming a surface treatment layer on at least a portion of the surface of the calcium carbonate- or magnesium carbonate-containing material. It should be understood that the present invention is not limited to any particular surface treatment agent. Those skilled in the art know how to select an appropriate material for use as a surface treatment agent. However, it should be noted that the surface treatment composition according to the present invention must contain at least one crosslinking compound containing at least two functional groups, where at least one functional group is suitable for crosslinking an elastomeric resin and at least one functional group is suitable for reacting with a calcium carbonate- or magnesium carbonate-containing material as a surface treatment agent. That is, when the surface treatment composition comprises or preferably consists of one surface treatment agent, this surface treatment agent is a crosslinking compound containing at least two functional groups, where at least one functional group is suitable for crosslinking an elastomeric resin and at least one functional group is suitable for reacting with a calcium carbonate- or magnesium carbonate-containing material. When the surface treatment composition comprises, and preferably consists of, two or more surface treatment agents, one surface treatment agent is a crosslinking compound containing at least two functional groups, at least one functional group being suitable for crosslinking the elastomeric resin and at least one functional group being suitable for reacting with a raw material containing calcium carbonate or magnesium carbonate, while the additional surface treatment agent(s) may be a surface treatment agent different from such crosslinking compound. Such additional surface treatment agent(s) are described in more detail below.

[0124] The term "at least one" crosslinkable compound comprising at least two functional groups in the sense of the present invention means that this crosslinkable compound comprises, preferably consists of, one or more crosslinkable compounds comprising at least two functional groups.

[0125] In one embodiment of the present invention, the at least one crosslinkable compound containing at least two functional groups comprises, and preferably consists of, one crosslinkable compound. Alternatively, the at least one crosslinkable compound containing at least two functional groups comprises, and preferably consists of, two or more crosslinkable compounds. For example, the at least one crosslinkable compound containing at least two functional groups comprises, and preferably consists of, two or three crosslinkable compounds.

[0126] Preferably, the at least one cross-linkable compound comprising at least two functional groups comprises, more preferably consists of, one cross-linkable compound comprising at least two functional groups.

[0127] It is understood that the at least one crosslinkable compound comprising at least two functional groups comprises at least one functional group suitable for crosslinking the elastomeric resin.

[0128] For the purposes of the present invention, a "crosslinking compound" is a compound that contains functional groups, such as carbon-carbon multiple bonds, halogen functional groups, sulfur functional groups, or hydrocarbon moieties, and is suitable for crosslinking elastomeric resins during crosslinking. The inventors have surprisingly found that such crosslinking compounds can react with elastomeric resins, i.e., elastomeric precursors, during a crosslinking process, e.g., a chemical crosslinking process. In this way, the elastomeric resin is distributed (uniformly) over the entire surface of the calcium carbonate- or magnesium carbonate-containing material, thereby improving the chemical compatibility of the elastomeric resin and the mechanical properties of the elastomeric product, even when used in small amounts.

[0129] Furthermore, the at least one crosslinking compound comprising at least two functional groups comprises at least one functional group suitable for reacting with calcium carbonate- or magnesium carbonate-containing materials. For example, the at least one functional group of the crosslinking compound suitable for reacting with calcium carbonate- or magnesium carbonate-containing materials comprises one or more terminal triethoxysilyl, trimethoxysilyl, and / or organic acid anhydride and / or salts thereof and / or carboxylic acid groups and / or salts thereof. Preferably, the at least one functional group of the crosslinking compound suitable for reacting with calcium carbonate- or magnesium carbonate-containing materials comprises one or more terminal triethoxysilyl, trimethoxysilyl, organic acid anhydride and / or salts thereof, or carboxylic acid groups and / or salts thereof.

[0130] In a preferred embodiment, at least one functional group of the crosslinking compound suitable for reacting with calcium carbonate- or magnesium carbonate-containing materials comprises one or more organic acid anhydride groups and / or salts thereof, or carboxylic acid groups and / or salts thereof. Most preferably, at least one functional group of the crosslinking compound suitable for reacting with calcium carbonate- or magnesium carbonate-containing materials comprises one or more organic acid anhydride groups and / or salts thereof. Alternatively, at least one functional group of the crosslinking compound suitable for reacting with calcium carbonate- or magnesium carbonate-containing materials comprises one or more triethoxysilyl or trimethoxysilyl functional groups and / or salts thereof.

[0131] Preferably, the organic acid anhydride group(s) is / are one or more succinic anhydride groups obtained by grafting maleic anhydride onto a homopolymer or copolymer.

[0132] In this respect, at least one functional group of a crosslinking compound suitable for reacting with a calcium carbonate- or magnesium carbonate-containing material preferably comprises, and more preferably consists of, one or more succinic anhydride groups obtained by grafting maleic anhydride onto a homopolymer or copolymer. For example, at least one functional group of a crosslinking compound suitable for reacting with a calcium carbonate- or magnesium carbonate-containing material preferably comprises, and more preferably consists of, one succinic anhydride group obtained by grafting maleic anhydride onto a homopolymer or copolymer. Alternatively, at least one functional group of a crosslinking compound suitable for reacting with a calcium carbonate- or magnesium carbonate-containing material preferably comprises, and more preferably consists of, two or more succinic anhydride groups, e.g., 2 to 12, particularly 2 to 9, e.g., 2 to 6, succinic anhydride groups obtained by grafting maleic anhydride onto a homopolymer or copolymer. Alternatively, at least one functional group of a crosslinking compound suitable for reacting with a calcium or magnesium carbonate-containing material preferably comprises, more preferably consists of, one triethoxysilyl or trimethoxysilyl functional group. For example, at least one functional group of a crosslinking compound suitable for reacting with a calcium or magnesium carbonate-containing material preferably comprises, more preferably consists of, two or more triethoxysilyl or trimethoxysilyl functional groups, for example, 2 to 12, in particular 2 to 9, e.g., 2 to 6, triethoxysilyl or trimethoxysilyl functional groups.

[0133] It is understood that at least one functional group of the cross-linking compound suitable for reacting with the calcium or magnesium carbonate containing material can be present as a salt, preferably in the form of a sodium or potassium salt.

[0134] In view of the above, the at least one crosslinkable compound comprising at least two functional groups can comprise two or more functional groups, for example, one or more functional groups suitable for crosslinking an elastomeric resin and one or more functional groups suitable for reacting with a calcium carbonate or magnesium carbonate-containing material.

[0135] In a preferred embodiment, the at least one crosslinking compound comprising at least two functional groups preferably comprises two functional groups, for example one functional group suitable for crosslinking an elastomeric resin and one functional group suitable for reacting with a calcium carbonate or magnesium carbonate containing material.

[0136] It is understood that the number of functional groups in the at least one cross-linking compound refers to the number of different functional groups, i.e., functional groups that do not have the same chemical structure. That is, if the at least one cross-linking compound contains, for example, two functional groups, the two functional groups are functional groups of different chemical structures, but each of the two different functional groups can be present once or multiple times.

[0137] According to one embodiment, the at least one crosslinkable compound comprising at least two functional groups is at least one graft polymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a homopolymer or copolymer comprising butadiene units and optionally styrene units.

[0138] The term "graft" or "grafted with maleic anhydride" refers to the double bond of maleic anhydride and the substituent R containing the carbon-carbon double bond. 1 and / or R 2This means that succinic anhydride is obtained after reaction with maleic anhydride. Accordingly, the terms "grafted homopolymer" and "grafted copolymer" refer to the corresponding homopolymer and copolymer, respectively, having succinic anhydride moieties formed from the reaction of the double bonds of maleic anhydride with carbon-carbon double bonds. It is understood that at least one graft polymer or a polymer grafted with maleic anhydride can also be referred to as a "maleic anhydride-functionalized polymer, e.g., maleic anhydride-functionalized polybutadiene" or a "maleic anhydride-added polymer, e.g., maleic anhydride-added polybutadiene."

[0139] That is, the at least one crosslinking compound containing at least two functional groups is preferably a grafted polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer, or a grafted polybutadiene-styrene copolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene-styrene copolymer. More preferably, the at least one crosslinking compound containing at least two functional groups is a grafted polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer.

[0140] According to an alternative embodiment, the at least one crosslinkable compound comprising at least two functional groups is a sulfur-containing trialkoxysilane, preferably a compound comprising two trialkoxysilylalkyl groups linked to a polysulfide.

[0141] When the at least one crosslinking compound comprising at least two functional groups is a grafted polybutadiene homopolymer comprising at least one succinic anhydride group obtained by grafting a polybutadiene homopolymer with maleic anhydride, this grafted polybutadiene homopolymer preferably has: (i) a number average molecular weight M measured by gel permeation chromatography of 1000 to 20000 g / mol, preferably 1400 to 15000 g / mol, more preferably 2000 to 10000 g / mol, measured in accordance with EN ISO 16014-1:2019; n and / or (ii) the number of functional groups per chain is in the range of 2 to 12, preferably 2 to 9, more preferably 2 to 6, and / or (iii) an anhydride equivalent weight in the range of 400 to 2200, preferably 500 to 2000, more preferably 550 to 1800;

[0142] In one embodiment, the grafted polybutadiene homopolymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer preferably has: (i) a number average molecular weight M measured by gel permeation chromatography of 1000 to 20000 g / mol, preferably 1400 to 15000 g / mol, more preferably 2000 to 10000 g / mol, measured in accordance with EN ISO 16014-1:2019; n , or (ii) the number of functional groups per chain ranges from 2 to 12, preferably from 2 to 9, more preferably from 2 to 6; or (iii) an anhydride equivalent weight in the range of 400 to 2200, preferably 500 to 2000, more preferably 550 to 1800;

[0143] In a preferred embodiment, the grafted polybutadiene homopolymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer preferably has: (i) a number average molecular weight M measured by gel permeation chromatography of 1000 to 20000 g / mol, preferably 1400 to 15000 g / mol, more preferably 2000 to 10000 g / mol, measured in accordance with EN ISO 16014-1:2019; n , and (ii) the number of functional groups per chain is in the range of 2 to 12, preferably 2 to 9, more preferably 2 to 6, and (iii) an anhydride equivalent weight in the range of 400 to 2200, preferably 500 to 2000, more preferably 550 to 1800;

[0144] Additionally or alternatively, the grafted polybutadiene homopolymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer has an acid number, measured according to ASTM D974-14, in the range of 10 to 300 meq KOH / g of grafted polybutadiene homopolymer, preferably 20 to 200 meq KOH / g, more preferably 30 to 150 meq KOH / g.

[0145] Thus, in one embodiment, the grafted polybutadiene homopolymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer has: (i) a number average molecular weight M measured by gel permeation chromatography of 1000 to 20000 g / mol, preferably 1400 to 15000 g / mol, more preferably 2000 to 10000 g / mol, measured in accordance with EN ISO 16014-1:2019; n , and (ii) the number of functional groups per chain is in the range of 2 to 12, preferably 2 to 9, more preferably 2 to 6, and (iii) an anhydride equivalent weight in the range of 400 to 2200, preferably 500 to 2000, more preferably 550 to 1800, and (iv) an acid number, measured according to ASTM D974-14, in the range of 10 to 300 meq KOH / g of grafted polybutadiene homopolymer, preferably 20 to 200 meq KOH / g, more preferably 30 to 150 meq KOH / g.

[0146] Additionally or alternatively, the grafted polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto the polybutadiene homopolymer has a Brookfield viscosity at 25° C. in the range of 3,000 to 70,000 cPs, preferably in the range of 5,000 to 50,000 cPs. Alternatively, the maleic anhydride grafted polybutadiene homopolymer has a Brookfield viscosity at 55° C. in the range of 100,000 to 170,000 cPs, preferably in the range of 120,000 to 160,000 cPs.

[0147] Thus, in one embodiment, the grafted polybutadiene homopolymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer has: (i) a number average molecular weight M measured by gel permeation chromatography of 1000 to 20000 g / mol, preferably 1400 to 15000 g / mol, more preferably 2000 to 10000 g / mol, measured in accordance with EN ISO 16014-1:2019; n , and (ii) the number of functional groups per chain is in the range of 2 to 12, preferably 2 to 9, more preferably 2 to 6, and (iii) an anhydride equivalent weight in the range of 400 to 2200, preferably 500 to 2000, more preferably 550 to 1800, and (iv) an acid number, measured according to ASTM D974-14, in the range of 10 to 300 meq KOH / g of grafted polybutadiene homopolymer, preferably 20 to 200 meq KOH / g, more preferably 30 to 150 meq KOH / g; and (v) a Brookfield viscosity at 25°C in the range of 3,000 to 70,000 cPs, preferably in the range of 5,000 to 50,000 cPs.

[0148] For example, a grafted polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer has a number average molecular weight M measured by gel permeation chromatography of 1000 to 20000 g / mol, preferably 1400 to 15000 g / mol, more preferably 2000 to 10000 g / mol. n and an acid number in the range of 20 to 200 meq KOH / g, preferably 30 to 150 meq KOH / g, as measured according to ASTM D974-14. In another embodiment, the grafted polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto the polybutadiene homopolymer has a number average molecular weight M measured by gel permeation chromatography of 2000 to 5000 g / mol. n and an acid number in the range of 30 to 100 meq KOH / g as measured in accordance with ASTM D974-14.

[0149] In one embodiment, the grafted polybutadiene homopolymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer has a number average molecular weight M of 2000 to 10000 g / mol, preferably 2000 to 4500 g / mol or 4500 to 7000 g / mol, as measured by gel permeation chromatography. n a number of functional groups per chain of 2 to 6, preferably 2 to 4 or 4 to 6; an anhydride equivalent weight in the range of 550 to 1800, preferably 550 to 1000 or 1000 to 1800; and a Brookfield viscosity at 25°C in the range of 5000 to 50,000 cPs, preferably 5000 to 10,000 cPs or 35,000 to 50,000 cPs.

[0150] For example, a grafted polybutadiene homopolymer containing at least one succinic anhydride group, obtained by grafting maleic anhydride onto a polybutadiene homopolymer, has a number average molecular weight M of 2000 to 4500 g / mol as measured by gel permeation chromatography. n a functionality of 2 to 4 per chain; an anhydride equivalent weight in the range of 1000 to 1800; and a Brookfield viscosity at 25° C. in the range of 5000 to 10000 cPs. In an alternative embodiment, a grafted polybutadiene homopolymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer has a number average molecular weight Mn of 4500 to 7000 g / mol, as measured by gel permeation chromatography; a functionality of 4 to 6 per chain; an anhydride equivalent weight in the range of 550 to 1000; and a Brookfield viscosity at 25° C. in the range of 35000 to 50000 cPs. In an alternative embodiment, the grafted polybutadiene homopolymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer has a number average molecular weight Mn of 2500 to 4500 g / mol as measured by gel permeation chromatography; a functionality per chain of 2 to 4; an anhydride equivalent weight in the range of 550 to 1000; and a Brookfield viscosity at 25°C in the range of 120,000 to 160,000 cPs.

[0151] Additionally or alternatively, the at least one crosslinking compound comprising at least two functional groups is a grafted polybutadiene-styrene copolymer comprising at least one succinic anhydride group obtained by grafting a polybutadiene-styrene copolymer with maleic anhydride and has: (i) a number average molecular weight M measured by gel permeation chromatography of 1000 to 20000 g / mol, preferably 1400 to 15000 g / mol, more preferably 2000 to 10000 g / mol, measured in accordance with EN ISO 16014-1:2019; n and / or (ii) the number of functional groups per chain is in the range of 2 to 12, preferably 2 to 9, more preferably 2 to 6, and / or (iii) an anhydride equivalent weight in the range of 400 to 2200, preferably 500 to 2000, more preferably 550 to 1800, and / or (iv) a 1,2-vinyl content of 20 to 80 mol %, preferably 20 to 40 mol %, based on the total weight of the grafted polybutadiene-styrene copolymer.

[0152] In one embodiment, the grafted polybutadiene-styrene copolymer comprising at least one succinic anhydride group obtained by grafting a polybutadiene-styrene copolymer with maleic anhydride has: (i) a number average molecular weight M measured by gel permeation chromatography of 1000 to 20000 g / mol, preferably 1400 to 15000 g / mol, more preferably 2000 to 10000 g / mol, measured in accordance with EN ISO 16014-1:2019; n , or (ii) the number of functional groups per chain ranges from 2 to 12, preferably from 2 to 9, more preferably from 2 to 6; or (iii) an anhydride equivalent weight in the range of 400 to 2200, preferably 500 to 2000, more preferably 550 to 1800; or (iv) a 1,2-vinyl content of 20 to 80 mol %, preferably 20 to 40 mol %, based on the total weight of the grafted polybutadiene-styrene copolymer.

[0153] In a preferred embodiment, the grafted polybutadiene-styrene copolymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene-styrene copolymer has: (i) a number average molecular weight M measured by gel permeation chromatography of 1000 to 20000 g / mol, preferably 1400 to 15000 g / mol, more preferably 2000 to 10000 g / mol, measured in accordance with EN ISO 16014-1:2019; n , and (ii) the number of functional groups per chain is in the range of 2 to 12, preferably 2 to 9, more preferably 2 to 6, and (iii) an anhydride equivalent weight in the range of 400 to 2200, preferably 500 to 2000, more preferably 550 to 1800, and (iv) a 1,2-vinyl content of 20 to 80 mol %, preferably 20 to 40 mol %, based on the total weight of the grafted polybutadiene-styrene copolymer.

[0154] Additionally or alternatively, the grafted polybutadiene-styrene copolymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene-styrene copolymer has a Brookfield viscosity at 45°C in the range of 100,000 to 200,000 cPs, preferably in the range of 150,000 to 200,000 cPs.

[0155] In one embodiment, the grafted polybutadiene-styrene copolymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene-styrene copolymer has a number average molecular weight M as measured by gel permeation chromatography of 2000 to 10000 g / mol. n , the number of functional groups per chain ranging from 2 to 6, an anhydride equivalent weight ranging from 550 to 1800, and a Brookfield viscosity at 45°C ranging from 150,000 to 200,000 cPs.

[0156] According to yet another embodiment of the present invention, the at least one crosslinking compound is a sulfur-containing trialkoxysilane.

[0157] In one embodiment, the sulfur-containing trialkoxysilane is preferably selected from the group comprising, preferably consisting of, mercaptopropyltrimethoxysilane (MPTS), mercaptopropyltriethoxysilane, bis(triethoxysilylpropyl)disulfide (TESPD), bis(triethoxysilylpropyl)tetrasulfide (TESPT), 3-aminopropyltrimethoxysilane (APTMS), 3-aminopropyltriethoxysilane, and mixtures thereof.

[0158] In one embodiment, the sulfur-containing trialkoxysilane is preferably a compound containing two trialkoxysilyl alkyl groups bonded to a polysulfide. For example, the compound containing two trialkoxysilyl alkyl groups bonded to a polysulfide is selected from bis(triethoxysilylpropyl) disulfide (TESPD), bis(triethoxysilylpropyl) tetrasulfide (TESPT), and mixtures thereof. Preferably, the compound containing two trialkoxysilyl alkyl groups bonded to a polysulfide is bis(triethoxysilylpropyl) tetrasulfide (TESPT).

[0159] The composition of the present invention is formed from a calcium carbonate or magnesium carbonate-containing material and 0.5 to 20 wt % of a surface treatment composition based on the total weight of the calcium carbonate or magnesium carbonate-containing material, the surface treatment composition including at least one crosslinking compound having at least two functional groups, wherein at least one functional group is suitable for crosslinking an elastomer resin and at least one functional group is suitable for reacting with the calcium carbonate or magnesium carbonate-containing material.

[0160] Thus, the surface treatment composition may comprise, or preferably consist of, a grafted polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer, or a grafted polybutadiene-styrene copolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene-styrene copolymer, preferably a polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer. Thus, by contacting a calcium carbonate- or magnesium carbonate-containing material with this surface treatment composition, a treatment layer is formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material. Preferably, a treatment layer is formed on the surface of at least one calcium carbonate or magnesium carbonate-containing material by contacting the calcium carbonate or magnesium carbonate-containing material with the surface treatment composition in an amount of 0.5 to 20 wt %, more preferably 0.5 to 10 wt %, even more preferably 0.5 to 8 wt %, and most preferably 0.6 to 7 wt %, based on the total weight of the calcium carbonate or magnesium carbonate-containing material.

[0161] Alternatively, the calcium carbonate or magnesium carbonate-containing material is applied to the surface of the calcium carbonate or magnesium carbonate-containing material. 2 0.1 to 10 mg per unit, preferably 1 m 2 0.1 to 8 mg per unit, more preferably 1 m 2 A treatment layer is formed on the surface of at least one calcium carbonate- or magnesium carbonate-containing material by contacting the surface with the surface treatment composition in an amount of 0.11 to 3 mg per 1000 mg of the calcium carbonate- or magnesium carbonate-containing material.

[0162] For example, the treatment layer on at least a portion of the surface of the calcium carbonate or magnesium carbonate-containing material can be formed by contacting the calcium carbonate or magnesium carbonate-containing material with a grafted polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer, and the grafted polybutadiene homopolymer has a number average molecular weight M of 1,000 to 20,000 g / mol, preferably 1,400 to 15,000 g / mol, more preferably 2,000 to 10,000 g / mol, as measured by gel permeation chromatography. n having an acid number, measured in accordance with ASTM D974-14, in the range of 20 to 200 meq KOH per gram of grafted polybutadiene homopolymer, preferably 30 to 150 meq KOH per gram, and in an amount of 0.5 to 20 wt. %, more preferably 0.5 to 10 wt. %, even more preferably 0.5 to 8 wt. %, and most preferably 0.6 to 7 wt. %, based on the total weight of the calcium carbonate or magnesium carbonate containing material, or on the surface of the calcium carbonate or magnesium carbonate containing material; 2 0.1 to 10 mg per unit, preferably 1 m 2 0.1 to 8 mg per unit, more preferably 1 m 2 The calcium carbonate or magnesium carbonate-containing material may be contacted with the calcium carbonate or magnesium carbonate-containing material in an amount of 0.11 to 3 mg per 1000 mg of the calcium carbonate or magnesium carbonate-containing material.

[0163] Alternatively, the surface treatment layer on at least a portion of the calcium carbonate or magnesium carbonate-containing material can be formed by contacting the calcium carbonate or magnesium carbonate-containing material with a grafted polybutadiene-styrene copolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene-styrene copolymer, and the grafted polybutadiene-styrene copolymer has a number average molecular weight M measured by gel permeation chromatography of 1,000 to 20,000 g / mol, preferably 1,400 to 15,000 g / mol, more preferably 2,000 to 10,000 g / mol. nan acid number, measured according to ASTM D974-14, in the range of 20 to 200 meq KOH per gram of grafted polybutadiene homopolymer, preferably 30 to 150 meq KOH per gram; and / or a molar amount of 1,2-vinyl groups in the range of 20 to 80 mol %, preferably 20 to 40 mol %, in an amount of 0.5 to 20 wt %, more preferably 0.5 to 10 wt %, even more preferably 0.5 to 8 wt %, most preferably 0.6 to 7 wt %, based on the total weight of the calcium carbonate or magnesium carbonate containing material, or on the surface of the calcium carbonate or magnesium carbonate containing material 2 0.1 to 10 mg per unit, preferably 1 m 2 0.1 to 8 mg per unit, more preferably 1 m 2 The calcium carbonate or magnesium carbonate-containing material may be contacted with the calcium carbonate or magnesium carbonate-containing material in an amount of 0.11 to 3 mg per 1000 mg of the calcium carbonate or magnesium carbonate-containing material.

[0164] In one embodiment, the surface treatment composition comprises a grafted polybutadiene homopolymer comprising at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer having a Brookfield viscosity at 25°C in the range of 1,000 to 300,000 mPa·s, and / or an acid number in the range of 10 to 300 mg KOH per gram of grafted polybutadiene homopolymer, and / or an iodine number in the range of 100 to 1,000 g iodine per 100 g of grafted polybutadiene homopolymer. For example, the surface treatment composition comprises a grafted polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer having a Brookfield viscosity at 25°C in the range of 1,000 to 300,000 mPa·s, an acid value in the range of 10 to 300 mg KOH per gram of grafted polybutadiene homopolymer, or an iodine value in the range of 100 to 1,000 g iodine per 100 g of grafted polybutadiene homopolymer. Alternatively, the surface treatment composition comprises a grafted polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer having a Brookfield viscosity at 25°C in the range of 1,000 to 300,000 mPa·s, an acid value in the range of 10 to 300 mg KOH per gram of grafted polybutadiene homopolymer, and an iodine value in the range of 100 to 1,000 g iodine per 100 g of grafted polybutadiene homopolymer.

[0165] In view of the above, it is understood that the composition of the present invention is a composition formed from a calcium carbonate or magnesium-containing material selected from the group consisting of deposited ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), surface-reacted calcium carbonate (SRCC), precipitated hydromagnesite, and mixtures thereof, and 0.5 to 20 wt % of a surface-treatment composition, based on the total weight of the calcium carbonate or magnesium carbonate-containing material, wherein the surface-treatment composition comprises at least one crosslinking compound having at least two functional groups, at least one functional group being suitable for crosslinking an elastomeric resin and at least one functional group being suitable for reacting with the calcium carbonate or magnesium-containing material, and the calcium carbonate or magnesium-containing material is preferably a surface-treated calcium carbonate or magnesium-containing material selected from the group consisting of deposited ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), surface-reacted calcium carbonate (SRCC), precipitated hydromagnesite, and mixtures thereof.

[0166] It is understood that the composition of the present invention is preferably formed from a surface treatment composition comprising, and preferably consisting of, at least one crosslinking compound comprising at least two functional groups, wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with the calcium carbonate or magnesium carbonate-containing material.

[0167] In one embodiment, the surface treatment composition further comprises at least one additional surface treatment agent selected from the group consisting of: (I) a blend of phosphoric acid esters of one or more phosphoric acid monoesters and / or salts thereof, and / or one or more phosphoric acid diesters and / or salts thereof, and / or (II) at least one saturated or unsaturated aliphatic linear or branched carboxylic acid and / or salt thereof, preferably at least one aliphatic carboxylic acid and / or salt thereof having a total number of carbon atoms of C4 to C24, more preferably at least one aliphatic carboxylic acid and / or salt thereof having a total number of carbon atoms of C12 to C20, most preferably at least one aliphatic carboxylic acid and / or salt thereof having a total number of carbon atoms of C16 to C18, and / or (III) at least one mono-substituted succinic anhydride and / or a salt thereof, which is a succinic anhydride mono-substituted with a group selected from a linear group, a branched group, an aliphatic group, and a cyclic group having a total carbon atom number of at least C2 to C30 in the substituent, and / or (IV) at least one polydialkylsiloxane, and (V) A mixture of one or more materials according to (I) to (IV).

[0168] According to one embodiment of the present invention, the surface treatment composition comprises a further surface treatment agent which is a phosphate ester blend of one or more phosphoric acid monoesters and / or salts thereof, and / or one or more phosphoric acid diesters and / or salts thereof. In one embodiment of the present invention, the one or more phosphoric acid monoesters comprise an o-phosphoric acid molecule esterified with an alcohol selected from saturated, branched or straight-chain, aliphatic or aromatic alcohols having a total number of carbon atoms in the alcohol substituent from C6 to C30. For example, the one or more phosphoric acid monoesters comprise an o-phosphoric acid molecule esterified with an alcohol selected from saturated, branched or straight-chain, aliphatic or aromatic alcohols having a total number of carbon atoms in the alcohol substituent from C8 to C22, more preferably from C8 to C20, and most preferably from C8 to C18.

[0169] Alkyl esters of phosphoric acid are well known in industry, especially as surfactants, lubricants and antistatic agents (Die Tenside; Kosswig und Stache, Carl Hanser Verlag Munchen, 1993).

[0170] The synthesis of alkyl esters of phosphoric acid by different methods and the surface treatment of minerals with alkyl esters of phosphoric acid are well known to those skilled in the art, for example from the following documents: Pesticide Formulations and Application Systems: 17th Volume; Collins HM, Holl FR, Hopkinson M, STP1268; Published: 1996; U.S. Pat. No. 3,897,519 A, U.S. Pat. No. 4,921,990 A, U.S. Pat. No. 4,350,645 A, U.S. Pat. No. 6,710,199 B2, U.S. Pat. No. 4,126,650 A, U.S. Pat. No. 5,554,781 A, EP 1 092 000 B1 and WO 2008 / 023076 A1.

[0171] In one embodiment of the present invention, the one or more phosphoric acid monoesters contain C6 to C6 phosphate groups in the alcohol substituent. 30 For example, the one or more phosphoric acid monoesters comprise an o-phosphoric acid molecule esterified with an alcohol selected from saturated, linear or branched aliphatic alcohols having a total number of carbon atoms in the alcohol substituent from C8 to C22, more preferably C8 to C20, and most preferably C8 to C18.

[0172] In one embodiment of the present invention, the one or more phosphoric acid monoesters consist of an o-phosphoric acid molecule esterified with an alcohol selected from saturated, straight-chain aliphatic alcohols having a total number of carbon atoms in the alcohol substituent from C6 to C30, preferably C8 to C22, more preferably C8 to C20, and most preferably C8 to C18. Alternatively, the one or more phosphoric acid monoesters consist of an o-phosphoric acid molecule esterified with an alcohol selected from saturated, branched aliphatic alcohols having a total number of carbon atoms in the alcohol substituent from C6 to C30, preferably C8 to C22, more preferably C8 to C20, and most preferably C8 to C18.

[0173] In one embodiment of the present invention, the one or more phosphoric acid monoesters are selected from the group comprising hexyl phosphoric acid monoester, heptyl phosphoric acid monoester, octyl phosphoric acid monoester, 2-ethylhexyl phosphoric acid monoester, nonyl phosphoric acid monoester, decyl phosphoric acid monoester, undecyl phosphoric acid monoester, dodecyl phosphoric acid monoester, tetradecyl phosphoric acid monoester, hexadecyl phosphoric acid monoester, heptylnonyl phosphoric acid monoester, octadecyl phosphoric acid monoester, 2-octyl-1-decyl phosphoric acid monoester, 2-octyl-1-dodecyl phosphoric acid monoester and mixtures thereof.

[0174] For example, the one or more phosphoric acid monoesters are selected from the group comprising 2-ethylhexyl phosphoric acid monoester, hexadecyl phosphoric acid monoester, heptylnonyl phosphoric acid monoester, octadecyl phosphoric acid monoester, 2-octyl-1-decyl phosphoric acid monoester, 2-octyl-1-dodecyl phosphoric acid monoester, and mixtures thereof. In one embodiment of the present invention, the one or more phosphoric acid monoesters are 2-octyl-1-dodecyl phosphoric acid monoester.

[0175] The expression "one or more" phosphoric acid diesters is understood to mean that one or more types of phosphoric acid diesters may be present in the treatment layer of the surface treatment material product and / or in the phosphoric acid ester blend.

[0176] Therefore, it should be noted that the one or more phosphoric acid diesters may be a single type of phosphoric acid diester. Alternatively, the one or more phosphoric acid diesters may be a mixture of two or more types of phosphoric acid diesters. For example, the one or more phosphoric acid diesters may be a mixture of two or three types of phosphoric acid diesters, such as two types of phosphoric acid diesters.

[0177] In one embodiment of the present invention, the one or more phosphoric acid diesters comprise an o-phosphoric acid molecule esterified with two alcohols selected from saturated, branched or straight-chain, aliphatic or aromatic alcohols having a total number of carbon atoms in the alcohol substituent from C6 to C30. For example, the one or more phosphoric acid diesters comprise an o-phosphoric acid molecule esterified with two fatty alcohols selected from saturated, branched or straight-chain, aliphatic or aromatic alcohols having a total number of carbon atoms in the alcohol substituent from C8 to C22, more preferably from C8 to C20, and most preferably from C8 to C18.

[0178] It is understood that the two alcohols used to esterify the phosphoric acid can be independently selected from the same or different saturated, branched or straight-chain, aliphatic or aromatic alcohols having a total number of carbon atoms in the alcohol substituents of C6 to C30. In other words, one or more phosphoric acid diesters may contain two substituents derived from the same alcohol, or a phosphoric acid diester molecule may contain two substituents derived from different alcohols.

[0179] In one embodiment of the present invention, the one or more phosphoric acid diesters comprise an o-phosphoric acid molecule esterified with two alcohols selected from the same or different, saturated, linear or branched aliphatic alcohols having a total number of carbon atoms in the alcohol substituent from C6 to C30. For example, the one or more phosphoric acid diesters comprise an o-phosphoric acid molecule esterified with two alcohols selected from the same or different, saturated, linear or branched aliphatic alcohols having a total number of carbon atoms in the alcohol substituent from C8 to C22, more preferably from C8 to C20, and most preferably from C8 to C18.

[0180] In one embodiment of the present invention, the one or more phosphoric acid diesters comprise an o-phosphoric acid molecule esterified with two alcohols selected from the same or different, saturated, straight-chain aliphatic alcohols having a total number of carbon atoms in the alcohol substituent from C6 to C30, preferably C8 to C22, more preferably C8 to C20, and most preferably C8 to C18. Alternatively, the one or more phosphoric acid diesters comprise an o-phosphoric acid molecule esterified with two alcohols selected from the same or different, saturated, branched aliphatic alcohols having a total number of carbon atoms in the alcohol substituent from C6 to C30, preferably C8 to C22, more preferably C8 to C20, and most preferably C8 to C18.

[0181] In one embodiment of the present invention, the one or more phosphoric acid diesters are selected from the group comprising hexyl phosphoric acid diester, heptyl phosphoric acid diester, octyl phosphoric acid diester, 2-ethylhexyl phosphoric acid diester, nonyl phosphoric acid diester, decyl phosphoric acid diester, undecyl phosphoric acid diester, dodecyl phosphoric acid diester, tetradecyl phosphoric acid diester, hexadecyl phosphoric acid diester, heptylnonyl phosphoric acid diester, octadecyl phosphoric acid diester, 2-octyl-1-decyl phosphoric acid diester, 2-octyl-1-dodecyl phosphoric acid diester and mixtures thereof.

[0182] For example, the one or more phosphoric acid diesters are selected from the group comprising 2-ethylhexyl phosphoric acid diester, hexadecyl phosphoric acid diester, heptylnonyl phosphoric acid diester, octadecyl phosphoric acid diester, 2-octyl-1-decyl phosphoric acid diester, 2-octyl-1-dodecyl phosphoric acid diester, and mixtures thereof. In one embodiment of the present invention, the one or more phosphoric acid diesters are 2-octyl-1-dodecyl phosphoric acid diester.

[0183] In one embodiment of the present invention, the one or more phosphoric acid monoesters are selected from the group comprising 2-ethylhexyl phosphoric acid monoester, hexadecyl phosphoric acid monoester, heptylnonyl phosphoric acid monoester, octadecyl phosphoric acid monoester, 2-octyl-1-decyl phosphoric acid monoester, 2-octyl-1-dodecyl phosphoric acid monoester, and mixtures thereof; and the one or more phosphoric acid diesters are selected from the group comprising 2-ethylhexyl phosphoric acid diester, hexadecyl phosphoric acid diester, heptylnonyl phosphoric acid diester, octadecyl phosphoric acid diester, 2-octyl-1-decyl phosphoric acid diester, 2-octyl-1-dodecyl phosphoric acid diester, and mixtures thereof.

[0184] According to another embodiment of the present invention, the surface treatment composition further comprises a surface treatment agent, which is at least one saturated or unsaturated aliphatic, linear or branched carboxylic acid and / or salt thereof, preferably at least one aliphatic carboxylic acid and / or salt thereof having a total number of carbon atoms from C4 to C24, more preferably at least one aliphatic carboxylic acid and / or salt thereof having a total number of carbon atoms from C12 to C20, and most preferably at least one aliphatic carboxylic acid and / or salt thereof having a total number of carbon atoms from C16 to C18.

[0185] Carboxylic acids in the sense of the present invention can be selected from one or more linear, branched, saturated or unsaturated, and / or alicyclic carboxylic acids. Preferably, the aliphatic carboxylic acids are monocarboxylic acids, i.e., they are characterized by the presence of only one carboxyl group, which is located at the end of the carbon skeleton.

[0186] In one embodiment of the present invention, the aliphatic linear or branched carboxylic acid and / or salt thereof is selected from saturated unbranched carboxylic acids, preferably selected from the group of carboxylic acids consisting of pentanoic acid, hexanoic acid, heptanoic acid, octanoic acid, nonanoic acid, decanoic acid, undecanoic acid, lauric acid, tridecanoic acid, myristic acid, pentadecanoic acid, palmitic acid, heptadecanoic acid, stearic acid, nonadecanoic acid, arachidic acid, heneicosylic acid, behenic acid, tricosylic acid, lignoceric acid, salts thereof, anhydrides thereof and mixtures thereof.

[0187] In another embodiment of the present invention, the aliphatic linear or branched carboxylic acid and / or salt thereof is selected from the group consisting of octanoic acid, decanoic acid, lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, and mixtures thereof. Preferably, the aliphatic carboxylic acid is selected from the group consisting of myristic acid, palmitic acid, stearic acid, salts thereof, anhydrides thereof, and mixtures thereof.

[0188] Preferably, the aliphatic carboxylic acid and / or its salt or anhydride is stearic acid and / or a stearate or stearic anhydride.

[0189] Alternatively, the unsaturated aliphatic straight-chain or branched carboxylic acid is preferably selected from the group consisting of myristoleic acid, palmitoleic acid, sapienic acid, oleic acid, elaidic acid, vaccenic acid, linoleic acid, α-linolenic acid, eicosapentaenoic acid, docosahexaenoic acid, and mixtures thereof. More preferably, the unsaturated aliphatic straight-chain or branched carboxylic acid is selected from the group consisting of myristoleic acid, palmitoleic acid, sapienic acid, oleic acid, elaidic acid, vaccenic acid, linoleic acid, α-linolenic acid, and mixtures thereof. Most preferably, the unsaturated aliphatic straight-chain or branched carboxylic acid is oleic acid and / or linoleic acid, preferably oleic acid or linoleic acid, and most preferably linoleic acid.

[0190] Additionally or alternatively, the surface treatment agent is a salt of an unsaturated aliphatic straight or branched chain carboxylic acid.

[0191] The term "salt of an unsaturated aliphatic linear or branched carboxylic acid" refers to an unsaturated fatty acid in which the active acid groups are partially or fully neutralized. The term "partially neutralized" unsaturated aliphatic linear or branched carboxylic acid refers to a degree of neutralization of the active acid groups in the range of 40-95 mol%, preferably 50-95 mol%, more preferably 60-95 mol%, and most preferably 70-95 mol%. The term "fully neutralized" unsaturated aliphatic linear or branched carboxylic acid refers to a degree of neutralization of the active acid groups of >95 mol%, preferably >99 mol%, more preferably >99.8 mol%, and most preferably 100 mol%. Preferably, the active acid groups are partially or fully neutralized.

[0192] The salt of the unsaturated aliphatic linear or branched carboxylic acid is preferably a compound selected from the group consisting of its sodium, potassium, calcium, magnesium, lithium, strontium, primary amine, secondary amine, tertiary amine and / or ammonium salts, wherein the amine salt is linear or cyclic. For example, the unsaturated aliphatic linear or branched carboxylic acid is a salt of oleic acid and / or linoleic acid, preferably oleic acid or linoleic acid, most preferably linoleic acid.

[0193] According to another embodiment of the present invention, the surface treatment composition comprises an additional surface treatment agent, which is at least one mono-substituted succinic anhydride mono-substituted with a group selected from linear, branched, aliphatic, and cyclic groups having a total of at least C2 to C30 carbon atoms in the substituent, and / or a salt thereof. Preferably, the surface treatment composition comprises an additional surface treatment agent, which is at least one mono-substituted succinic anhydride mono-substituted with a linear aliphatic group having a total of at least C2 to C30 carbon atoms in the substituent, and / or a salt thereof. Additionally or alternatively, the surface treatment composition comprises an additional surface treatment agent, which is at least one mono-substituted succinic anhydride mono-substituted with a branched aliphatic group having a total of at least C3 to C30 carbon atoms in the substituent, and / or a salt thereof. Additionally or alternatively, the surface treatment composition includes a further surface treatment agent, which is at least one mono-substituted succinic anhydride consisting of succinic anhydride and / or salts thereof mono-substituted with a group that is a cycloaliphatic group having a total number of carbon atoms in the substituent of at least C5 to C30.

[0194] Therefore, it should be noted that the at least one mono-substituted succinic anhydride may be one type of mono-substituted succinic anhydride. Alternatively, the at least one mono-substituted succinic anhydride may be a mixture of two or more types of mono-substituted succinic anhydrides. For example, the at least one mono-substituted succinic anhydride may be a mixture of two or three types of mono-substituted succinic anhydrides, such as two types of mono-substituted succinic anhydrides.

[0195] In one embodiment of the present invention, the at least one mono-substituted succinic anhydride is one kind of mono-substituted succinic anhydride.

[0196] It is understood that the at least one mono-substituted succinic anhydride corresponds to a surface treatment agent and is composed of succinic anhydride mono-substituted with a group selected from any linear group, branched group, aliphatic group, and cyclic group having a total carbon atom number of C2 to C30 in the substituent.

[0197] In one embodiment of the present invention, the at least one mono-substituted succinic anhydride is a succinic anhydride mono-substituted with a group selected from a linear group, a branched group, an aliphatic group, and a cyclic group having a total of C3 to C20 carbon atoms in the substituent. For example, the at least one mono-substituted succinic anhydride is a succinic anhydride mono-substituted with a group selected from a linear group, a branched group, an aliphatic group, and a cyclic group having a total of C4 to C18 carbon atoms in the substituent. Preferably, the surface treatment composition includes an additional surface treatment agent, and this additional surface treatment agent is at least one mono-substituted succinic anhydride and / or a salt thereof mono-substituted with a group that is a linear aliphatic group having a total of C3 to C20 carbon atoms in the substituent, more preferably C4 to C18 carbon atoms. Additionally or alternatively, the surface treatment composition comprises a further surface treatment agent, the further surface treatment agent being at least one mono-substituted succinic anhydride consisting of succinic anhydride and / or a salt thereof mono-substituted with a group that is a branched aliphatic group having a total number of carbon atoms in the substituent of C3 to C30, more preferably C4 to C18. Additionally or alternatively, the surface treatment composition comprises a further surface treatment agent, the further saturated surface treatment agent comprising at least one mono-substituted succinic anhydride consisting of succinic anhydride and / or a salt thereof mono-substituted with a group that is a cyclic aliphatic group having a total number of carbon atoms in the substituent of C5 to C20, more preferably C5 to C18.

[0198] In one embodiment of the present invention, the at least one mono-substituted succinic anhydride consists of succinic anhydride mono-substituted with one group which is a linear aliphatic group having a total number of carbon atoms in the substituent from C2 to C30, preferably C3 to C20, and most preferably C4 to C18. Additionally or alternatively, the at least one mono-substituted succinic anhydride consists of succinic anhydride mono-substituted with one group which is a branched aliphatic group having a total number of carbon atoms in the substituent from C3 to C30, preferably C3 to C20, and most preferably C4 to C18.

[0199] Therefore, it is preferred that the at least one mono-substituted succinic anhydride consists of succinic anhydride mono-substituted with one group which is a linear alkyl group having a total number of carbon atoms of C2 to C30, preferably C3 to C20, most preferably C4 to C18 in the substituent. Additionally or alternatively, it is preferred that the at least one mono-substituted succinic anhydride consists of succinic anhydride mono-substituted with one group which is a branched alkyl group having a total number of carbon atoms of C3 to C30, preferably C3 to C20, most preferably C4 to C18 in the substituent.

[0200] For example, the at least one mono-substituted succinic anhydride comprises succinic anhydride mono-substituted with one group which is a linear alkyl group having a total number of carbon atoms in the substituent from C2 to C30, preferably from C3 to C20, and most preferably from C4 to C18. Additionally or alternatively, the at least one mono-substituted succinic anhydride comprises succinic anhydride mono-substituted with one group which is a branched alkyl group having a total number of carbon atoms in the substituent from C3 to C30, preferably from C3 to C20, and most preferably from C4 to C18.

[0201] In one embodiment of the present invention, the at least one mono-substituted succinic anhydride is at least one linear or branched alkyl mono-substituted succinic anhydride, for example, the at least one alkyl mono-substituted succinic anhydride is selected from the group comprising ethylsuccinic anhydride, propylsuccinic anhydride, butylsuccinic anhydride, triisobutylsuccinic anhydride, pentylsuccinic anhydride, hexylsuccinic anhydride, heptylsuccinic anhydride, octylsuccinic anhydride, nonylsuccinic anhydride, decylsuccinic anhydride, dodecylsuccinic anhydride, hexadecanylsuccinic anhydride, octadecanylsuccinic anhydride, and mixtures thereof.

[0202] Thus, for example, the term "butylsuccinic anhydride" is understood to include one or more linear and branched butylsuccinic anhydrides. One specific example of one or more linear butylsuccinic anhydrides is n-butylsuccinic anhydride. One specific example of one or more branched butylsuccinic anhydrides is isobutylsuccinic anhydride, sec-butylsuccinic anhydride, and / or tert-butylsuccinic anhydride.

[0203] Further, for example, the term "hexadecanyl succinic anhydride" is understood to include one or more linear and branched hexadecanyl succinic anhydrides. One specific example of one or more linear hexadecanyl succinic anhydrides is n-hexadecanyl succinic anhydride. Specific examples of one or more branched hexadecanyl succinic anhydrides include 14-methylpentadecanyl succinic anhydride, 13-methylpentadecanyl succinic anhydride, 12-methylpentadecanyl succinic anhydride, 11-methylpentadecanyl succinic anhydride, 10-methylpentadecanyl succinic anhydride, 9-methylpentadecanyl succinic anhydride, 8-methylpentadecanyl succinic anhydride, 7-methylpentadecanyl succinic anhydride, 6-methylpentadecanyl succinic anhydride, 8 ...9-methylpentadecanyl succinic anhydride, 8-methylpentadecanyl succinic anhydride, 9-methylpentadecanyl succinic anhydride, 9-methylpentadecanyl succinic anhydride, 9-methylpentadecanyl succinic anhydride, 9-methylpentadecanyl succinic anhydride, 9-methylpentadecanyl succinic anhydride, 9-methylpentadecanyl succinic anhydride, 9-methylpentadecanyl succinic anhydride, 9-methylpentadecanyl succinic anhydride, 9-methylpent Butadecanyl succinic anhydride, 5-methylpentadecanyl succinic anhydride, 4-methylpentadecanyl succinic anhydride, 3-methylpentadecanyl succinic anhydride, 2-methylpentadecanyl succinic anhydride, 1-methylpentadecanyl succinic anhydride, 13-ethylbutadecanyl succinic anhydride, 12-ethylbutadecanyl succinic anhydride, 11-ethylbutadecanyl succinic anhydride, 10-ethylbutadecanyl succinic anhydride, 9-ethylbutadecanyl succinic anhydride Succinic acid, 8-ethylbutadecanyl succinic anhydride, 7-ethylbutadecanyl succinic anhydride, 6-ethylbutadecanyl succinic anhydride, 5-ethylbutadecanyl succinic anhydride, 4-ethylbutadecanyl succinic anhydride, 3-ethylbutadecanyl succinic anhydride, 2-ethylbutadecanyl succinic anhydride, 1-ethylbutadecanyl succinic anhydride, 2-butyldodecanyl succinic anhydride, 1-hexyl-2-decanyl succinic anhydride succinic anhydride, 2-hexyldecanyl succinic anhydride, 6,12-dimethylbutadecanyl succinic anhydride, 2,2-diethyldodecanyl succinic anhydride, 4,8,12-trimethyltridecanyl succinic anhydride, 2,2,4,6,8-pentamethylundecanyl succinic anhydride, 2-ethyl-4-methyl-2-(2-methylpentyl)-heptyl succinic anhydride and / or 2-ethyl-4,6-dimethyl-2-propylnonyl succinic anhydride.

[0204] Further, for example, the term "octadecanyl succinic anhydride" is understood to include one or more linear and branched octadecanyl succinic anhydrides. One specific example of one or more linear octadecanyl succinic anhydrides is n-octadecanyl succinic anhydride. Specific examples of one or more branched octadecanyl succinic anhydrides include 16-methylheptadecanyl succinic anhydride, 15-methylheptadecanyl succinic anhydride, 14-methylheptadecanyl succinic anhydride, 13-methylheptadecanyl succinic anhydride, 12-methylheptadecanyl succinic anhydride, 11-methylheptadecanyl succinic anhydride, 10-methylheptadecanyl succinic anhydride, 9-methylheptadecanyl succinic anhydride, ...5-methylheptadecanyl succinic anhydride, 14-methylheptadecanyl succinic anhydride, 13-methylheptadecanyl succinic anhydride, 12-methylheptadecanyl succinic anhydride, 11-methylheptadecanyl succinic anhydride, 10-methylheptadecanyl succinic anhydride, 9-methylheptadecanyl succinic anhydride, 15-methylheptadecanyl succinic anhydride, 14-methyl 1-Methylheptadecanyl succinic anhydride, 8-methylheptadecanyl succinic anhydride, 7-methylheptadecanyl succinic anhydride, 6-methylheptadecanyl succinic anhydride, 5-methylheptadecanyl succinic anhydride, 4-methylheptadecanyl succinic anhydride, 3-methylheptadecanyl succinic anhydride, 2-methylheptadecanyl succinic anhydride, 1-methylheptadecanyl succinic anhydride, 14-ethyl Hexadecanyl succinic anhydride, 13-ethylhexadecanyl succinic anhydride, 12-ethylhexadecanyl succinic anhydride, 11-ethylhexadecanyl succinic anhydride, 10-ethylhexadecanyl succinic anhydride, 9-ethylhexadecanyl succinic anhydride, 8-ethylhexadecanyl succinic anhydride, 7-ethylhexadecanyl succinic anhydride, 6-ethylhexadecanyl succinic anhydride, 5-ethylhexadecanyl succinic anhydride hexylhexadecanyl succinic anhydride, 4-ethylhexadecanyl succinic anhydride, 3-ethylhexadecanyl succinic anhydride, 2-ethylhexadecanyl succinic anhydride, 1-ethylhexadecanyl succinic anhydride, 2-hexyldodecanyl succinic anhydride, 2-heptylundecanyl succinic anhydride, isooctadecanyl succinic anhydride and / or 1-octyl-2-decanyl succinic anhydride.

[0205] In one embodiment of the present invention, the at least one alkyl mono-substituted succinic anhydride is selected from the group comprising butylsuccinic anhydride, hexylsuccinic anhydride, heptylsuccinic anhydride, octylsuccinic anhydride, hexadecanylsuccinic anhydride, octadecanylsuccinic anhydride and mixtures thereof.

[0206] In one embodiment of the present invention, the at least one mono-substituted succinic anhydride is one type of alkyl mono-substituted succinic anhydride. For example, the one alkyl mono-substituted succinic anhydride is butyl succinic anhydride. Alternatively, the one alkyl mono-substituted succinic anhydride is hexyl succinic anhydride. Alternatively, the one alkyl mono-substituted succinic anhydride is heptyl succinic anhydride or octyl succinic anhydride. Alternatively, the one alkyl mono-substituted succinic anhydride is hexadecanyl succinic anhydride. For example, the one alkyl mono-substituted succinic anhydride is a linear hexadecanyl succinic anhydride such as n-hexadecanyl succinic anhydride, or a branched hexadecanyl succinic anhydride such as 1-hexyl-2-decanyl succinic anhydride. Alternatively, the one alkyl mono-substituted succinic anhydride is octadecanyl succinic anhydride. For example, the one alkyl mono-substituted succinic anhydride is a linear octadecanyl succinic anhydride such as n-octadecanyl succinic anhydride, or a branched octadecanyl succinic anhydride such as isooctadecanyl succinic anhydride or 1-octyl-2-decanyl succinic anhydride.

[0207] In one embodiment of the present invention, the one alkyl mono-substituted succinic anhydride is a butylsuccinic anhydride, such as n-butylsuccinic anhydride.

[0208] In one embodiment of the present invention, the at least one mono-substituted succinic anhydride is a mixture of two or more alkyl mono-substituted succinic anhydrides, for example, the at least one mono-substituted succinic anhydride is a mixture of two or three alkyl mono-substituted succinic anhydrides.

[0209] According to another embodiment of the present invention, the surface treatment composition comprises an additional surface treatment agent which is at least one polydialkylsiloxane.

[0210] Preferred polydialkylsiloxanes are described, for example, in US Patent Application Publication No. 2004 / 0097616 A1. Most preferred are polydialkylsiloxanes selected from the group consisting of polydimethylsiloxanes, preferably dimethicone, polydiethylsiloxane and polymethylphenylsiloxane and / or mixtures thereof.

[0211] For example, the at least one polydialkylsiloxane is preferably polydimethylsiloxane (PDMS).

[0212] Preferably, the at least one calcium carbonate- or magnesium carbonate-containing material and the at least one cross-linking compound are provided as a physical mixture and / or the at least one calcium carbonate- or magnesium carbonate-containing material is contacted with the at least one cross-linking compound to form the composition of the present invention, whereby a treated layer comprising the at least one cross-linking compound and / or a salt-containing reaction product thereof is formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material. For example, the at least one calcium carbonate- or magnesium carbonate-containing material and the at least one cross-linking compound are provided as a physical mixture or the at least one calcium carbonate- or magnesium carbonate-containing material is contacted with the at least one cross-linking compound to form the composition of the present invention, whereby a treated layer comprising the at least one cross-linking compound and / or a salt-containing reaction product thereof is formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material. Preferably, the composition of the present invention is formed by contacting at least one calcium carbonate- or magnesium carbonate-containing material with at least one cross-linking compound, whereby a treatment layer comprising the at least one cross-linking compound and / or a salt-containing reaction product thereof is formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material. Thus, the composition of the present invention is preferably a surface-treated calcium carbonate- or magnesium carbonate-containing material comprising a treatment layer comprising at least one cross-linking compound and / or a salt-containing reaction product thereof formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material.

[0213] In a further embodiment, the at least one calcium carbonate- or magnesium carbonate-containing material, the at least one crosslinkable compound, and the additional surface treatment agent are provided as a physical mixture and / or the at least one calcium carbonate- or magnesium carbonate-containing material is contacted with the at least one crosslinkable compound and the additional surface treatment agent to form a composition of the present invention, whereby a treatment layer comprising the at least one crosslinkable compound and / or a salt-containing reaction product thereof and the additional surface treatment agent and / or a salt-containing reaction product thereof is formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material. For example, the at least one calcium carbonate- or magnesium carbonate-containing material, the at least one crosslinkable compound, and the additional surface treatment agent are provided as a physical mixture or the at least one calcium carbonate- or magnesium carbonate-containing material is contacted with the at least one crosslinkable compound and the additional surface treatment agent to form a composition of the present invention, whereby a treatment layer comprising the at least one crosslinkable compound and / or a salt-containing reaction product thereof and the additional surface treatment agent and / or a salt-containing reaction product thereof is formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material. Preferably, the composition of the present invention is formed by contacting at least one calcium carbonate- or magnesium carbonate-containing material with at least one crosslinking compound and a further surface treatment agent, whereby a treatment layer comprising the at least one crosslinking compound and / or a salt-containing reaction product thereof and the further surface treatment agent and / or a salt-containing reaction product thereof is formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material. In this embodiment, the composition of the present invention is preferably a surface-treated calcium carbonate- or magnesium carbonate-containing material comprising a treatment layer comprising the at least one crosslinking compound and / or a salt-containing reaction product thereof and the further surface treatment agent and / or a salt-containing reaction product thereof formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material.

[0214] It is understood that the treatment layer on at least a portion of the calcium carbonate or magnesium carbonate-containing material is formed by contacting the calcium carbonate or magnesium carbonate-containing material with the above-mentioned additional surface treatment agent. 2 0.1 to 10 mg per unit, preferably 1 m 2 0.1 to 8 mg per unit, more preferably 1 m 2 The calcium carbonate- or magnesium carbonate-containing material is contacted with 0.11 to 3 mg of the surface treatment composition per 1000 mg of the calcium carbonate- or magnesium carbonate-containing material. That is, a chemical reaction can occur between the calcium carbonate- or magnesium carbonate-containing material and the surface treatment agent. In other words, the treatment layer can contain the surface treatment agent and / or a salt-containing reaction product thereof.

[0215] The term "salt-containing reaction product" of an additional surface treatment agent refers to a product obtained by contacting a calcium carbonate- or magnesium carbonate-containing material with a surface treatment composition that includes an additional surface treatment agent. This reaction product is formed between at least a portion of the applied additional surface treatment agent and reactive molecules located on the surface of the calcium carbonate- or magnesium carbonate-containing material.

[0216] Method for producing the composition Methods for producing the compositions described herein, in particular methods for surface treatment of fillers, are known to those skilled in the art and are described, for example, in EP 3 192 837 A1, EP 2 770 017 A1, and WO 2016 / 023937. According to one aspect of the present invention, the compositions of the present invention can be obtained by a dry process comprising at least the following steps: (a) providing a calcium carbonate or magnesium carbonate-containing material selected from the group consisting of ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), surface-reacted calcium carbonate (SRCC), precipitated hydromagnesite, and mixtures thereof; (b) at least one crosslinking compound containing at least two functional groups in an amount of 0.1 to 10 mg / m based on the total weight of the calcium carbonate or magnesium carbonate-containing material; 2 wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with the calcium carbonate or magnesium carbonate containing material; (c) optionally providing at least one further surface treatment agent as defined herein; (d) optionally, heating the at least one crosslinkable compound; and (e) contacting, in one or more steps, the calcium carbonate or magnesium carbonate-containing material with the at least one cross-linking compound while mixing; (f) heating the at least one further surface treatment agent, if present, to a temperature at or above its melting point, thereby obtaining a molten surface treatment agent, and in one or more steps contacting the molten surface treatment agent with the at least one crosslinking compound simultaneously or subsequently with the calcium carbonate or magnesium carbonate-containing material while mixing.

[0217] It is understood that the calcium carbonate- or magnesium carbonate-comprising material in step (a) is preferably provided in dry form. Additionally or alternatively, the at least one graft polymer material in step (b) is preferably provided in dry form. Preferably, the calcium carbonate-comprising material in step (a) is provided in dry form, and the at least one crosslinking compound in step (b) is provided in dry form. Thus, in a preferred embodiment, the composition of the present invention is thus produced by a dry method. It should be noted that, with respect to this method, the terms "dry form" or "dry method" mean that the calcium carbonate-comprising material in step (a) and / or the at least one crosslinking compound in step (b) are provided without the use of a solvent, such as water.

[0218] It is understood that the at least one crosslinkable compound may be in a solid, highly viscous, or liquid state. Typically, the at least one crosslinkable compound is in a highly viscous or liquid state. Preferably, the at least one crosslinkable compound is provided in a liquid state in method step (e). Therefore, the at least one crosslinkable compound can be optionally heated to provide the at least one crosslinkable compound in a liquid state, i.e., a low-viscosity state. Thus, in one embodiment, the method includes a step of heating the at least one crosslinkable compound. Such a heating step (d) is preferably performed when the at least one crosslinkable compound is solid or highly viscous. However, even if the at least one crosslinkable compound in step (b) is in a liquid state, it may be preferable to perform the heating step (d) to accelerate and increase the reaction.

[0219] Generally, step (e) is carried out at a temperature of 5 to 200° C., preferably 20 to 150° C., most preferably 40 to 150° C., for example 80 to 150° C. If the method includes step (d) of heating the at least one crosslinkable compound, steps (d) and (e) are preferably carried out at a temperature of 40 to 150° C., for example 80 to 150° C. It is understood that the temperature in optional steps (d) and (e) is adjusted so that the at least one crosslinkable compound is in a liquid state but does not thermally decompose the at least one crosslinkable compound.

[0220]

[0033] When step (d) is present, steps (d) and (e) can be carried out simultaneously or separately. When steps (d) and (e) are carried out separately, step (d) is preferably carried out after step (e). When step (d) is carried out after step (e), the at least one crosslinking compound of step (b) is preferably added in dry form and heated upon contact with the calcium carbonate-comprising material of step (a) (i.e., the at least one crosslinking compound becomes non-viscous). It is also possible to contact the calcium carbonate-comprising material with the at least one crosslinking compound while mixing in one or more steps, followed by heating.

[0221] When present, steps (d) and (e) are preferably carried out simultaneously, preferably in the same vessel, i.e. by heating the mixture of at least one calcium carbonate- or magnesium carbonate-containing material and at least one crosslinking compound to a temperature of 5 to 200°C, preferably 20 to 150°C, most preferably 40 to 150°C, for example 80 to 150°C.

[0222] Step (e) and optional step (f) are carried out with mixing. It is understood that mixing can be carried out by any method or in any container known to those skilled in the art that can result in a homogeneous composition. For example, step (e) and optional step (f) can be carried out in a high-speed mixer or pin mill.

[0223] When the dry method includes a step of contacting the calcium carbonate- or magnesium carbonate-containing material with an additional surface treatment agent, step (f) is carried out at a temperature that is at least 2°C, preferably at least 5°C, and most preferably at least 10°C higher than the melting point of the additional surface treatment agent, preferably at a temperature of 5 to 200°C, for example 20 to 150°C. Such a temperature results in a molten surface treatment agent. It is understood that the temperature in step (f) is adjusted so that the additional surface treatment agent is in a molten state but does not thermally decompose the additional surface treatment agent.

[0224] Such dry processes result in preferred compositions of the present invention in that the resulting compositions have advantageous residual total moisture content and moisture absorption susceptibility. It is understood that a low residual total moisture content results in favorable mechanical properties of the elastomer when the compositions of the present invention are incorporated into the elastomer. Furthermore, it should be noted that such dry processes may leave residual functional groups of at least one crosslinking compound that have not reacted or only partially reacted with the calcium carbonate- or magnesium carbonate-containing material, which may be advantageous for use in the elastomer. In this regard, it is believed that the residual functional groups of at least one crosslinking compound that have not reacted or only partially reacted with the calcium carbonate- or magnesium carbonate-containing material can act as a processing aid during compounding. In contrast, wet processes, i.e., when processing is carried out in a slurry, do not achieve additional benefits when the composition is incorporated into an elastomer.

[0225] Preferably, the composition has a residual total moisture content of ≦2 wt.-%, more preferably ≦1.5 wt.-%, even more preferably ≦1.2 wt.-%, and most preferably ≦0.8 wt.-%, based on the total dry weight of the at least one calcium carbonate-comprising material. In one embodiment, the composition has a residual total moisture content of 0.001 wt.-% to 2 wt.-%, preferably 0.001 wt.-% to 1.5 wt.-%, more preferably 0.002 wt.-% to 1.2 wt.-%, and most preferably 0.005 wt.-% to 0.8 wt.-%, based on the total dry weight of the at least one calcium carbonate-comprising material. This is particularly true when the calcium carbonate-comprising material is heaped ground calcium carbonate (GCC) and / or precipitated calcium carbonate (PCC). When the calcium carbonate-comprising material is surface-reacted calcium carbonate or the magnesium carbonate-comprising material is precipitated hydromagnesite, the composition preferably has a total residual moisture content of 0.01 wt. % to 10 wt. %, preferably 0.01 wt. % to 8 wt. %, more preferably 0.02 wt. % to 6 wt. %, and most preferably 0.03 wt. % to 4 wt. %, based on the total dry weight of the calcium carbonate- or magnesium carbonate-comprising material.

[0226] In a preferred embodiment, the composition is formed from a calcium or magnesium carbonate-containing material and at least one crosslinking compound, the surface treatment composition comprising, and preferably consisting of, at least one crosslinking compound comprising at least two functional groups, wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting only with the calcium or magnesium carbonate-containing material.

[0227] In this embodiment, the method of the present invention comprises at least the following steps: (a) providing a calcium carbonate or magnesium carbonate-containing material selected from the group consisting of ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), surface-reacted calcium carbonate (SRCC), precipitated hydromagnesite, and mixtures thereof; (b) at least one crosslinking compound containing at least two functional groups in an amount of 0.1 to 10 mg / m based on the total weight of the calcium carbonate or magnesium carbonate-containing material; 2 wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with the calcium carbonate or magnesium carbonate containing material; (c) optionally, heating the at least one crosslinkable compound; and (d) contacting, in one or more steps, said calcium carbonate or magnesium carbonate containing material with said at least one cross-linking compound while mixing.

[0228] In this embodiment, the surface treatment layer is formed by contacting the calcium carbonate or magnesium carbonate-containing material with only at least one cross-linking compound, and thus the surface treatment composition consists of at least one cross-linking compound.

[0229] It is understood that step (d) is preferably carried out at a temperature of 5 to 200° C., more preferably 20 to 150° C., most preferably 40 to 150° C., for example 80 to 150° C. If the optional heating step (c) is present, step (c) is preferably carried out at a temperature of 40 to 150° C., for example 80 to 150° C.

[0230] In another preferred embodiment, the composition is formed from a calcium or magnesium carbonate-containing material and a surface treatment composition, the surface treatment composition comprising, and preferably consisting of, at least one crosslinking compound comprising at least two functional groups, wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with the calcium or magnesium carbonate-containing material and further surface treatment agents.

[0231] In this embodiment, the method of the present invention comprises at least the following steps: (a) providing a calcium carbonate or magnesium carbonate-containing material selected from the group consisting of ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), surface-reacted calcium carbonate (SRCC), precipitated hydromagnesite, and mixtures thereof; (b) at least one crosslinking compound containing at least two functional groups in an amount of 0.1 to 10 mg / m based on the total weight of the calcium carbonate or magnesium carbonate-containing material; 2 wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with the calcium carbonate or magnesium carbonate containing material; (c) providing at least one additional surface treatment; (d) optionally, heating the at least one crosslinkable compound; and (e) contacting, in one or more steps, the calcium carbonate or magnesium carbonate-containing material with the at least one cross-linking compound while mixing; (f) heating the at least one further surface treatment agent to a temperature at or above its melting point, thereby obtaining a molten surface treatment agent, and in one or more steps contacting the molten surface treatment agent with the at least one crosslinking compound simultaneously or subsequently, preferably subsequently, while mixing, with the calcium carbonate or magnesium carbonate-containing material.

[0232] When the surface treatment composition includes an additional surface treatment agent, the at least one crosslinking compound and the additional surface treatment agent can be provided as a mixture before contacting the calcium carbonate- or magnesium carbonate-containing material with the surface treatment composition. In this embodiment, the calcium carbonate- or magnesium carbonate-containing material is contacted with the molten surface treatment agent simultaneously with the at least one crosslinking compound. Alternatively, the calcium carbonate- or magnesium carbonate-containing material may be contacted with the at least one crosslinking compound and the additional surface treatment agent sequentially in any order. That is, the surface treatment layer is formed in a subsequent step by contacting the calcium carbonate- or magnesium carbonate-containing material with the at least one crosslinking compound and the molten additional surface treatment agent. It is understood that the calcium carbonate- or magnesium carbonate-containing material is preferably contacted with the molten surface treatment agent before contacting the calcium carbonate- or magnesium carbonate-containing material with the at least one crosslinking compound.

[0233] In a preferred embodiment, process steps (e) and (f) are carried out sequentially, and the calcium or magnesium carbonate-containing material is first contacted with the molten surface treatment agent, followed by contact with at least one crosslinking compound.

[0234] In an alternative embodiment, process steps (e) and (f) are performed sequentially, and the calcium- or magnesium carbonate-containing material is first contacted with the at least one crosslinking compound and subsequently with the molten surface treatment agent.

[0235] It is understood that step (f) is preferably carried out at a temperature that is at least 2° C., preferably at least 5° C., and most preferably at least 10° C. higher than the melting point of the one or more additional surface treatment agents. For example, step (f) is carried out at a temperature that is 2° C. to 30° C., preferably 5° C. to 25° C., and most preferably 10° C. to 20° C. higher than the melting point of the one or more additional surface treatment agents.

[0236] In one embodiment, optional steps (d), (e) and (f) are carried out at a temperature of 5 to 200°C, preferably 20 to 150°C, most preferably 40 to 150°C, for example 80 to 150°C.

[0237] product Another aspect of the present invention relates to a curable elastomer mixture comprising an elastomer resin and 5 to 300 wt %, preferably 10 to 150 wt %, more preferably 20 to 110 wt %, and most preferably 40 to 100 wt %, based on the total weight of the elastomer resin, of a composition as defined herein, wherein the composition is dispersed in the elastomer resin.

[0238] The elastomeric resins of the present invention are crosslinkable polymers that result in elastomers exhibiting elastomeric properties. Therefore, it is understood that the elastomeric resins of the present invention are suitable for forming crosslinks of crosslinkable polymers, also called elastomeric precursors. Any crosslinking method, such as chemical crosslinking with a crosslinking agent, vulcanization, crosslinking by ultraviolet radiation, electron beam radiation, nuclear radiation, gamma radiation, microwave radiation, and / or ultrasonic radiation, is suitable for the purposes of the present invention.

[0239] The elastomeric resin of the present invention can comprise any type of natural or synthetic rubber. For example, the elastomeric resin can be selected from acrylic rubber, butadiene rubber, acrylonitrile-butadiene rubber, epichlorohydrin rubber, isoprene rubber, ethylene-propylene rubber, ethylene-propylene-diene rubber, nitrile-butadiene rubber, butyl rubber, styrene-butadiene rubber, polyisoprene, hydrogenated nitrile-butadiene rubber, carboxylated nitrile-butadiene rubber, chloroprene rubber, isoprene-isobutylene rubber, chloro-isobutene-isoprene rubber, brominated isobutene-isoprene rubber, silicone rubber, fluorocarbon rubber, polyurethane rubber, polysulfide rubber, thermoplastic rubber, and mixtures thereof. These types of rubbers are well known to those skilled in the art (see Winnacker / Kuechler, "Chemische Technik. Prozesse und Produkte", 5th vol., 5th Ed., Wiley-VCH 2005, Ch. 4, pp. 821-896). Generally, rubbers are designated in abbreviated form according to DIN ISO-R 1629:2015-03 or ASTM D1418-17. The elastomeric resins according to the present invention are suitable for crosslinking suitable elastomeric precursors as described below.

[0240] Natural rubber (NR) in the sense of the present invention is a polymeric material containing polyisoprene, which may be obtained from natural sources such as rubber tree (Hevea Brasiliensis), sparge (Euphorbia spp.), dandelion (Taxacum Officinale and Taxacum Kok-saghyz), Parchium gutta, rubber fig (Ficus Elastica), bulletwood (Manilkara Bidentata) or guayule (Parthenium Argentatum). Depending on the source of the natural rubber, the rubber may be present, for example, as cauchuk (cis-1,4-polyisoprene), gutta-percha (trans-1,4-polyisoprene), or chicle (generally a mixture of cis-1,4-polyisoprene and trans-1,4-polyisoprene).

[0241] Synthetic rubbers are generally produced by radical, anionic, cationic or coordination polymerization of synthetic monomers, followed by crosslinking. The polymerization reaction can be carried out, for example, as a polymerization in emulsion, solution or suspension.

[0242] For example, ethylene-propylene rubber (EPR) is typically formed by radical copolymerization of ethylene and propylene. Optionally, a small amount (e.g., less than 10 mol %, preferably less than 5 mol %, based on the total amount of monomers) of a diene monomer, such as butadiene, dicyclopentadiene, ethylidene, norbornene, or norbornadiene, may be present. When a diene monomer is present during copolymerization, the resulting ethylene-propylene rubber is referred to as ethylene-propylene-diene rubber (EPDM) and contains unsaturated carbon moieties that can facilitate crosslinking of the resulting rubber. Alternatively, EPDM can be synthesized by coordination polymerization using a vanadium-based catalyst such as VCl4 or VOCl3. Commercially available EPDMs include, for example, EPDM Vistalon® 2504 from ExxonMobile or EPDM Keltan® 6950C from ARLANXEO Netherlands BV.

[0243] Butadiene rubber (BR) is typically formed from the coordination polymerization of butadiene in the presence of a Ziegler-Natta catalyst, and also by anionic polymerization. The butadiene rubber thus obtained may have different structural units, such as cis-1,4-, trans-1,4-, and 1,2-butadiene structural units, and the 1,2-butadiene structural units may be present in syndiotactic, isotactic, and / or atactic forms.

[0244] Styrene-butadiene rubber (SBR) is a copolymer of styrene and butadiene, and can exist as a random copolymer or a block copolymer. Specific examples include E-SBR (i.e., SBR obtained by emulsion polymerization) and L-SBR (i.e., SBR obtained by anionic polymerization in solution).

[0245] Nitrile-butadiene rubber (NBR) is typically a statistical copolymer of acrylonitrile and butadiene and may contain various amounts of cis-1,4-, trans-1,4-, and 1,2-butadiene and acrylonitrile structural units. Those skilled in the art know how to adjust the emulsion copolymerization conditions, such as the monomer ratio, reaction time, reaction temperature, emulsifiers, accelerators (e.g., thiurams, dithiocarbamates, sulfonamides, benzothiazole disulfides), and chain terminators (e.g., dimethyldithiocarbamate and diethylhydroxylamine), to obtain the appropriate distribution of these structural units. NBR has a number average molecular weight M ranging from 1500 g / mol to 1500 kg / mol, e.g., from 3000 g / mol to 1000 kg / mol, or from 5000 g / mol to 500 kg / mol. n The acrylonitrile content can range from 10 mol% to 75 mol%, preferably from 15 to 60 mol%, based on the total amount of monomer units. NBR is resistant to oil, fuel, and other non-polar chemicals, and is therefore commonly applied in fuel and oil handling hoses, seals, grommets, and self-sealing fuel tanks, protective gloves, footwear, sponges, expanding foams, mats, and aviation applications. Mixtures of NBR with other rubbers, such as EPDM, or thermoplastic polymers, such as PVC, can also be used.

[0246] Hydrogenated nitrile-butadiene rubber (HNBR) can be obtained by hydrogenation of NBR in the presence of a hydrogenation catalyst such as a cobalt-, rhodium-, ruthenium-, iridium-, or palladium-based system.

[0247] In another embodiment of the present invention, carboxylated NBR (XNBR) can be used, which can be obtained by copolymerizing butadiene and acrylonitrile with a small amount (e.g., less than 10 mol %, preferably less than 5 mol %, based on the total amount of monomers) of acrylic acid or methacrylic acid. In addition to or instead of the crosslinking methods described below, XNBR can be crosslinked by adding a metal salt, preferably a polyvalent metal salt, such as a calcium salt, zinc salt, magnesium salt, zirconium salt, or aluminum salt.

[0248] Polyisoprene, also known as isoprene rubber (IR), can be synthesized by anionic or Ziegler-Natta polymerization of isoprene and can contain cis-1,4-, trans-1,4-, 1,2-, and 3,4-isoprene structural units. Those skilled in the art know how to adjust the reaction conditions to obtain the appropriate molar distribution of this building block.

[0249] Isobutene-isoprene rubber (IIR), also known as butyl rubber, is typically synthesized by cationic polymerization starting from isobutene and isoprene monomer units in the presence of a catalyst such as aluminum trichloride or dialkylaluminum chloride. Halogenated IIR, such as chlorinated IIR (CIIR) or brominated IIR (BIIR), can be suitably obtained by post-polymerization modification of IIR, e.g., chlorination using chlorine or bromination using bromine, typically carried out under the exclusion of light and at temperatures ranging from 40 to 60°C. The halogen content of the halogenated IIR is preferably in the range of 0.5 to 5 wt%, more preferably 1.0 to 2.5 wt%, based on the total weight of the halogenated IIR.

[0250] Polychloroprene, also referred to as chloroprene rubber (CR), can be produced by radical emulsion polymerization of chloroprene (2-chlorobutadiene). This polymer can contain various amounts of predominantly trans-1,4-chloroprene and 1,2-chloroprene units, depending on the polymerization conditions, which can be appropriately adapted by those skilled in the art. In addition to or instead of the crosslinking methods described below, CR can be crosslinked at higher temperatures due to the injection of hydrochloric acid, optionally in the presence of an acid acceptor such as a metal oxide or hydroxide, preferably zinc oxide, magnesium oxide, or a combination thereof. This acid acceptor can be introduced into the elastomer already during polymerization or during mixing of the elastomer precursor with the remaining components of the elastomer composition.

[0251] Acrylic rubbers (ACMs) can be synthesized by emulsion or suspension radical polymerization. Typical monomers include acrylic ester monomers, preferably containing saturated or unsaturated, linear or branched groups containing 1 to 20 carbon atoms, preferably 1 to 8 carbon atoms. Suitable ACMs are commercially available, for example, under the trade names Noxtite® ACM or Nipol® AR.

[0252] Epichlorohydrin rubbers can be obtained by ring-opening polymerization of epichlorohydrin, optionally further containing monomers selected from the group including ethylene oxide, propylene oxide, and allyl glycidyl ether, typically in the presence of a catalyst such as trialkylaluminum.

[0253] Silicone rubbers are typically poly(diorganyl)siloxanes, which can be formed, for example, by the hydrolysis-condensation of diorganyldihalogenide siloxanes. The organyl groups can be selected from the group including alkyl, aryl, and alkenyl groups.

[0254] Polyurethane rubbers contain urethane structural building blocks formed from the reaction of isocyanates (ie, diisocyanates and polyisocyanates) with alcohols (ie, diols, triols, polyols).

[0255] Polysulfide rubber is a compound of dihalides (XRX) and sodium polysulfide (Na-S x -Na, x≧2). Representative examples include Thiokol® A, Thiokol® FA, and Thiokol® ST.

[0256] Thermoplastic rubbers (TPR or TPE) within the meaning of the present invention are materials that exhibit the elastic and processing properties of thermoplastic materials. They can be selected from the group comprising block copolymers such as styrene-diene block copolymers, styrene-ethylene-butylene rubbers, polyester TPEs, polyurethane TPEs or polyamide TPEs, blends of elastomers and non-elastomers such as blends of EPDM with PP and / or PE, blends of NR with polyolefins or blends of IIR with polyolefins, and ionomeric polymers such as zinc salts of sulfonated and maleated EPDM.

[0257] "Fluorocarbon rubbers" in the sense of the present invention are fluorine-containing polymers that have a low Tg value, for example, below 0°C, preferably below -5°C, more preferably below -10°C, and most preferably below -15°C, and exhibit rubber-like elasticity (see IUPAC, Compendium of Chemical Terminology, 2nd Ed. ("Gold Book"), 1997, "Elastomers"). Fluorocarbon rubbers can be classified according to ASTM D1418 - "Standard Practice for Rubber and Rubber Latices - Nomenclature". ASTM D1418 defines three classes of fluorocarbon rubbers:

[0258] FKM Fluorocarbon Rubber: Polymethylene type fluororubber using vinylidene fluoride as a comonomer and having fluoro, alkyl, perfluoroalkyl or perfluoroalkoxy groups as substituents in the polymer chain, with or without cure site monomers; FFKM fluorocarbon rubber: a polymethylene type perfluororubber having all the substituents on the polymer chain either fluoro, perfluoroalkyl, or perfluoroalkoxy groups; FEPM Fluorocarbon Rubber: A polymethylene-type fluororubber containing alkyl, perfluoroalkyl, and / or perfluoroalkoxy groups as one or more monomers, with or without cure site monomers (having reactive pendant groups). Most preferably, the crosslinkable fluorocarbon rubber is a copolymer of vinylidene fluoride, hexafluoropropylene, and tetrafluoroethylene.

[0259] Methods for producing crosslinkable fluorine-containing polymers are known in the art. Alternatively, crosslinkable fluorine-containing polymers are commercially available. Examples of commercially available fluorocarbon rubbers are Viton®, Viton® Extreme®, and Kalrez® fluorocarbon rubber from DuPont, Dyneon® fluorocarbon rubber from 3M, DAI-EL® fluorocarbon rubber from Daikin Industries, Ltd., Technoflon® from Solvay SA, and Aflas® from Asahi Glass Co., Ltd. Those skilled in the art will select an appropriate grade of these fluorocarbon rubber brands according to their needs.

[0260] Preferred elastomer resins according to the present invention are NBR, EPDM, CIIR, BIIR and CR, with NBR and EPDM being particularly preferred.

[0261] The curable elastomeric mixture may further comprise additives such as color pigments, fibers, e.g., cellulose, glass or wood fibers, dyes, waxes, lubricants, oxidation- and / or UV-stabilizers, plasticizers, curing agents, crosslinking coagents, antioxidants and other fillers.

[0262] According to one embodiment, the curable elastomeric mixture comprises a filler different from the calcium carbonate- or magnesium carbonate-containing material of the composition of the present invention, preferably this other filler being selected from the group comprising carbon black, silica, deposited ground calcium carbonate, precipitated calcium carbonate, nanofillers, graphite, clay, talc, diatomaceous earth, barium sulfate, titanium dioxide, wollastonite, and mixtures thereof. Preferably, the curable elastomeric mixture comprises another filler such as carbon black, TiO2, mica, clay, precipitated silica, talc, or calcined kaolin.

[0263] Preferably, the other filler is present in the curable elastomeric mixture in a volume ratio with the calcium carbonate or magnesium carbonate containing material in the range of from 10:90 to 90:10, preferably from 25:75 to 75:25, and more preferably from 40:60 to 60:40, for example 50:50.

[0264] In a preferred embodiment, the elastomeric composition further comprises a crosslinking coagent, which is preferably selected from the group consisting of peroxide crosslinking agents and / or sulfur-based crosslinking agents.

[0265] When the coagent is a peroxide, it can be selected from a wide variety of materials, including peresters, perketals, hydroperoxides, peroxydicarbonates, diacyl peroxides, and ketone peroxides. Examples of such peroxides include t-butyl peroctanoate, perbenzoate, methyl ethyl ketone peroxide, cyclohexanone peroxide, acetylacetone peroxide, dibenzoyl peroxide, bis(4-t-butylcyclohexyl)peroxydicarbonate, dicumyl peroxide, 1,1-bis(tert-butylperoxy)-3,3,5-trimethylcyclohexane, 2,5-bis(t-butylperoxy)-2,5-dimethylhexane, 2,5-bis(t-butylperoxy)-2,5-dimethylhexyne, or α,α'-bis(t-butylperoxy)diisopropylbenzene, diisopropylperoxy. dicarbonate, 1,1-bis(tert-hexylperoxy)-3,5,5-trimethylcyclohexane, 2,5-dimethylhexane-2,5-dihydroperoxide, di-tert-butyl peroxide, tert-butylcumyl peroxide, 2,5-dimethyl-2,5-bis(tert-butylperoxy)hexane, 2,5-dimethyl-2,5-bis(tert-butylperoxy)-3-hexyne, tert-butylperoxybenzoate, 2,5-dimethyl-2,5-bis(benzoylperoxy)hexane, tert-butyl peroxymaleate, or tert-hexylperoxyisopropyl monocarbonate, etc. Mixtures of two or more peroxides can be used if desired.

[0266] Preferably, the peroxide coagent can be used in combination with 1,2-polybutadiene, ethylene glycol dimethacrylate, triallyl phosphate, triallyl isocyanurate, m-phenylenediamine-bis-maleimide, or triallyl cyanurate.

[0267] The sulfur-based crosslinking coagent can be elemental sulfur or a sulfur-containing system, such as thiourea, for example, ethylenethiourea, N,N-dibutylthiourea, N,N-diethylthiourea, etc.; thiuram monosulfides and disulfides, for example, tetramethylthiuram monosulfide (TMTMS), tetrabutylthiuram disulfide (TBTDS), tetramethylthiuram disulfide (TMTDS), tetraethylthiuram monosulfide (TETMS), dipentamethylenethiuram hexasulfide (DPTH), etc.; benzothiazole sulfenamides, for example, N-oxydiethylene-2-benzothiazole sulfenamide, N-cyclohexyl-2-benzothiazole sulfenamide, N,N-diisopropyl ... Examples of suitable crosslinking accelerators include benzothiazole sulfenamide, N-tert-butyl-2-benzothiazole sulfenamide (TBBS), 2-mercaptoimidazoline, N-diphenylguanadine, and N,N-di-(2-methylphenyl)-guanadine. Thiazole accelerators include 2-mercaptobenzothiazole, 2-(morpholinodithio)benzothiazole disulfide, and zinc 2-mercaptobenzothiazole. Dithiocarbamate accelerators include tellurium diethyldithiocarbamate, copper dimethyldithiocarbamate, bismuth dimethyldithiocarbamate, cadmium diethyldithiocarbamate, lead dimethyldithiocarbamate, zinc diethyldithiocarbamate, and zinc dimethyldithiocarbamate. Mixtures of two or more sulfur-based crosslinking accelerators can be used, if desired.

[0268] Alternatively, the crosslinking coagent can be selected from bisphenol-based crosslinking agents, or amine or diamine-based crosslinking agents. Examples of suitable amine crosslinking agents include butylamine, dibutylamine, piperidine, trimethylamine, or diethylcyclohexylamine. Examples of suitable diamine crosslinking agents include bis-cinnamylidene hexamethylenediamine, hexamethylenediamine carbamate, bis-peroxycarbamate, such as hexamethylene-N,N'-bis(tert-butylperoxycarbamate) or methylenebis-4-cyclohexyl-N,N'-(tert-butylperoxycarbamate), piperazine, triethylenediamine, tetramethylethyldiamine, or diethylenetriamine.

[0269] Examples of suitable bisphenol crosslinkers are 2,2-bis(4-hydroxyphenyl)hexafluoropropane, substituted hydroquinones, 4,4'-disubstituted bisphenols, or hexafluoro-bisphenol A.

[0270] It should be understood that the coagent may react with the elastomeric resin during the crosslinking process and thus form part of the elastomer in the elastomeric product. Furthermore, the elastomeric product may thus include the reaction product of the coagent. Additionally or alternatively, a coagent, such as a peroxide, may act as a radical source and thus provide initiating radicals for crosslinking the elastomeric resin.

[0271] It will be appreciated that the present invention further relates to cured elastomeric products formed from the curable elastomeric mixture as defined herein.

[0272] The cured elastomeric product can be prepared by any method known to those skilled in the art. A suitable method for producing the cured elastomeric product includes the following steps: (a) providing an elastomeric resin; (b) providing as a filler 5 to 300 wt. % of at least one calcium carbonate or magnesium carbonate-containing material based on the total weight of the elastomeric resin; (c) 0.1 to 10 mg / m based on the total weight of calcium carbonate or magnesium carbonate-containing materials 2 providing at least one crosslinkable compound comprising at least two functional groups, wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with said calcium carbonate or magnesium carbonate containing material; (d) optionally providing at least one additional surface treatment agent as defined herein; (e) optionally providing further additives such as color pigments, fibers, e.g., cellulose, glass or wood fibers, dyes, waxes, lubricants, oxidation- and / or UV-stabilizers, plasticizers, hardeners, crosslinking coagents, antioxidants, and other fillers, e.g., carbon black, TiO2, mica, clay, precipitated silica, talc, or calcined kaolin; (f) contacting, in any order, the components of steps (a), (b), (c) and optionally steps (d) and (e); and (g) curing the mixture resulting from step (f), thereby forming a cured elastomeric product.

[0273] In one embodiment, the cured elastomeric product includes the additive. Accordingly, a suitable method for producing the cured elastomeric product comprises the following steps: (a) providing an elastomeric resin; (b) providing as a filler 5 to 300 wt. % of at least one calcium carbonate or magnesium carbonate-containing material based on the total weight of the elastomeric resin; (c) 0.1 to 10 mg / m based on the total weight of calcium carbonate or magnesium carbonate-containing materials 2providing at least one crosslinkable compound comprising at least two functional groups, wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with said calcium carbonate or magnesium carbonate containing material; (e) providing further additives such as color pigments, fibers, e.g., cellulose, glass or wood fibers, dyes, waxes, lubricants, oxidation- and / or UV-stabilizers, plasticizers, hardeners, crosslinking coagents, antioxidants, and other fillers, e.g., carbon black, TiO2, mica, clay, precipitated silica, talc, or calcined kaolin; (f) contacting, in any order, the components of steps (a), (b), (c), and (e); and (g) curing the mixture resulting from step (f), thereby forming a cured elastomeric product.

[0274] In one embodiment, the cured elastomeric product includes, in addition to the additive, at least one additional surface treatment agent. Thus, a suitable method for producing the cured elastomeric product includes the following steps: (a) providing an elastomeric resin; (b) providing as a filler 5 to 300 wt. % of at least one calcium carbonate or magnesium carbonate-containing material based on the total weight of the elastomeric resin; (c) 0.1 to 10 mg / m based on the total weight of calcium carbonate or magnesium carbonate-containing materials 2 providing at least one crosslinkable compound comprising at least two functional groups, wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with said calcium carbonate or magnesium carbonate containing material; (d) providing at least one additional surface treatment agent as defined herein; (e) providing further additives such as color pigments, fibers, e.g., cellulose, glass or wood fibers, dyes, waxes, lubricants, oxidation- and / or UV-stabilizers, plasticizers, hardeners, crosslinking coagents, antioxidants, and other fillers, e.g., carbon black, TiO2, mica, clay, precipitated silica, talc, or calcined kaolin; (f) contacting, in any order, the components of steps (a), (b), (c), (d), and (e); and (g) curing the mixture resulting from step (f), thereby forming a cured elastomeric product.

[0275] According to step (f) of the method of the present invention, the components of steps (a), (b) and (c) are contacted in any order. Preferably, the contacting is carried out by mixing the components to form a mixture. During the mixing step (f), optionally, at least one additional surface treatment agent and / or one or more additives known to those skilled in the art can be added to the mixture as described herein above.

[0023] Preferably, in the contacting step (f), firstly, in one or more steps, the at least one calcium carbonate- or magnesium carbonate-comprising material of step (b) is contacted with the at least one crosslinking compound of step (c) and, if present, subsequently or simultaneously with the at least one further surface treatment agent of step (d), while mixing, so that a surface treatment layer comprising the at least one crosslinking compound and / or a salt-containing reaction product thereof, and optionally comprising the at least one further surface treatment agent and / or a salt-containing reaction product thereof, is formed on the surface of the at least one calcium carbonate- or magnesium carbonate-comprising material of step (b), and secondly, in one or more steps, this surface-treated calcium carbonate- or magnesium carbonate-comprising material is contacted with the elastomeric resin of step (a) while mixing.

[0276] For example, in the contacting step (f), first, in one or more steps, the at least one calcium carbonate- or magnesium carbonate-containing material of step (b) is contacted with the at least one crosslinking compound of step (c) while mixing, so that a surface-treated layer comprising the at least one crosslinking compound and / or a salt-containing reaction product thereof is formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material of step (b), and second, in one or more steps, the surface-treated calcium carbonate- or magnesium carbonate-containing material is contacted with the elastomeric resin of step (a) while mixing.

[0277] Alternatively, in the contacting step (f), first, in one or more steps, the at least one calcium carbonate- or magnesium carbonate-containing material of step (b) is contacted with the at least one crosslinking compound of step (c) and subsequently or simultaneously, preferably subsequently, with the at least one further surface treatment agent of step (d) while mixing, so that a surface treatment layer comprising the at least one crosslinking compound and / or a salt-containing reaction product thereof and the at least one further surface treatment agent and / or a salt-containing reaction product thereof is formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material of step (b), and second, in one or more steps, this surface-treated calcium carbonate- or magnesium carbonate-containing material is contacted with the elastomeric resin of step (a) while mixing.

[0278] In view of the above, it is preferred to first contact the components of steps (b), (c) and optional step (d) to obtain the composition of the present invention. With regard to process conditions, reference is made to the information above when providing detailed information on the method for producing this composition. In a further step, the composition obtained by mixing the components of steps (b), (c) and optional step (d) is then contacted with the elastomer resin of step (a) and further additives of optional step (e).

[0279]

[0033] Before or after, preferably after, contacting with mixing the surface-treated calcium or magnesium carbonate-comprising material with the elastomeric resin of step (a) in one or more steps, the further additives of step (e), if present, are contacted with the surface-treated calcium or magnesium carbonate-comprising material in one or more steps while mixing.

[0280] It is understood that the optional step (e) additional additive can be contacted with the components of step (a), step (b), step (c) and optional step (d) in one or more steps. For example, the optional step (e) additional additive can be contacted with the components of step (a), step (b), step (c) and optional step (d) in several steps. For example, the optional step (e) additional additive, such as a crosslinking coagent, can be added before and during step (g).

[0281] The contacting step (f) can be carried out by any means known to those skilled in the art, including, but not limited to, blending, extruding, kneading, and high speed mixing.

[0282] Preferably, the contacting step (f) is carried out in an internal mixer and / or an external mixer, wherein the external mixer is preferably a cylindrical mixer.

[0283] The mixture of step (f) is cured to form a cured elastomeric product in step (g). Curing can be accomplished by any method known to those skilled in the art that results in curing, i.e., crosslinking, of the elastomeric resin.

[0284] For example, step (g) can be carried out by adding a crosslinking coagent and then thermal crosslinking. The mixture is heated to a temperature high enough to allow the crosslinking coagent to react with the crosslinkable polymer and at least one crosslinkable compound containing at least two functional groups, for example, at least 100°C, preferably at least 150°C, and more preferably at least 180°C. Optionally, the curing step can be carried out by a combination of compression molding, injection molding, or extrusion. During compression molding, pressure is applied to force the mixture into the desired shape of the mold, ensuring contact with all areas of the mold and crosslinking the mixture within the mold so that the elastomer composition retains the desired shape. Preferably, compression molding is carried out at a pressure of at least 10 MPa (100 bar), preferably at least 15 MPa (150 bar), and more preferably at least 20 MPa (200 bar).

[0285] Suitable crosslinking coagents are those mentioned herein above.

[0286] In another preferred embodiment of the present invention, the curing, i.e. crosslinking, in step (g) is carried out by energy intensity radiation such as ultraviolet radiation, electron beam radiation, nuclear radiation, gamma radiation, microwave radiation, temperature induced radiation and / or ultrasonic radiation.

[0287] In one embodiment, the contacting step (f) is carried out during the curing step (g), and the at least one crosslinking compound is contacted with the elastomeric resin of step (a) while mixing, either before or after, preferably after, adding the at least one calcium carbonate or magnesium carbonate-containing material.

[0288] It is understood that the method may include further steps such as processing / molding the cured elastomeric product into any desired shape. Such steps of processing / molding are well known to those skilled in the art and can be carried out, for example, by molding the cured elastomeric product.

[0289] In another aspect, the present invention relates to the use of at least one crosslinking compound comprising at least two functional groups, wherein at least one functional group is suitable for crosslinking the elastomer resin and at least one calcium carbonate or magnesium carbonate containing material as a filler, in the formulation of an elastomer formed from an elastomer resin and at least one calcium carbonate or magnesium carbonate containing material, wherein at least one functional group is suitable for crosslinking the elastomer resin and at least one functional group is suitable for reacting with the calcium carbonate or magnesium carbonate containing material, The present invention relates to the use of a compounded elastomer for improving the mechanical properties of the compounded elastomer compared to the same elastomer formed from the same elastomer resin and at least one calcium carbonate or magnesium carbonate containing material, but without the at least one crosslinking compound comprising at least two functional groups, at least one of which is suitable for crosslinking the elastomer resin and at least one of which is suitable for reacting with said calcium carbonate or magnesium carbonate containing material.

[0290] In a further aspect, the present invention relates to an article formed from the cured elastomeric product, wherein the article is selected from the group including tubeless articles, membranes, sealings, gloves, pipes, cables, electrical connectors, oil hoses, shoe soles, O-ring seals, shaft seals, gaskets, tubing, valve stem seals, fuel hoses, tank seals, diaphragms, flexible liners for pumps, mechanical seals, pipe fittings, valve lines, military flare blenders, electrical connectors, fuel joints, roll covers, firewall seals, clips for jet engines, and the like.

[0291] The scope and benefits of the present invention will be better understood based on the following examples, which are intended to illustrate certain specific embodiments of the invention and are not limiting. [Example]

[0292] 1.Measurement method The measurement methods used in the examples are described below.

[0293] Particle size distribution Volume median particle size d 50 and volume top cut particle size d 98 is assessed using a Malvern Mastersizer 3000 Laser Diffraction System. 50 or d 98 The values ​​indicate the diameter values ​​at which 50% or 98% by volume of the particles have a diameter less than this value, respectively. The raw data obtained by the measurement are analyzed using Mie theory, assuming a particle refractive index of 1.57 and an absorption coefficient of 0.005.

[0294] Weight median particle size d 50 (wt) and weight top cut particle size d 98 The weight percent (wt) is determined by the sedimentation method, which is an analysis of sedimentation behavior in a gravimetric field. Measurements are performed using a Sedigraph® 5120 from Micromeritics Instrument Corporation. This method and instrument is known to those skilled in the art and is commonly used to determine particle size of fillers and pigments. Measurements are performed in an aqueous solution of 0.1 wt% Na4P2O7. The sample was dispersed using a high-speed stirrer and sonicated.

[0295] These methods and instruments are known to those skilled in the art and are commonly used to determine particle size of fillers and pigments.

[0296] Specific surface area (SSA) The specific surface area was measured by the BET method according to ISO 9277:2010 on a Micromeritics ASAP 2460 instrument from Micromeritics, using nitrogen as the adsorption gas. Prior to the measurement, the samples were heated at 150 °C for 60 min and then stored in vacuum (10 -5 It was pretreated with bar.

[0297] Porosimetry (void measurement) Specific pore volumes were measured using mercury intrusion porosimetry using a Micromeritics Autopore V 9620 mercury porosimeter with a maximum applied mercury pressure of 414 MPa (60,000 psi), equivalent to a Laplace throat diameter of 0.004 μm (~nm). An equilibration time of 20 seconds was used for each pressure step. Sample materials were loaded onto a 3 cm 3 The powder is sealed in the chamber and the data are corrected for mercury compression, penetrometer expansion, and sample material compression using the software Pore-Comp (Gane, PAC, Kettle, JP, Matthews, GP, and Ridgway, CJ, "Void Space Structure of Compressible Polymer Spheres and Consolidated Calcium Carbonate Paper-Coating Formulations", Industrial and Engineering Chemistry Research, 35(5), 1996, pp. 1753-1764).

[0298] The total pore volume seen in the integrated intrusion data can be separated into two regions with intrusion data ranging from 214 μm down to approximately 1-4 μm, indicating a strong contribution from coarse packing of the sample between any aggregate structures. Below these diameters, there is fine interparticle packing of the particles themselves. If the particles also contain intraparticle pores, this region is bimodal, and the intraparticle specific pore volume is defined as the specific pore volume of mercury intruded into pores narrower than the inflection point of the bimodal transition. The sum of these three regions gives the total pore volume of the powder, but is heavily influenced by the precipitation of powder at the coarse pore end of the original sample compaction / distribution.

[0299] Taking the first derivative of the cumulative intrusion curve reveals a pore size distribution based on the equivalent Laplace diameter, which necessarily includes pore obscuration. The derivative curve clearly shows the coarse aggregate pore structure region, the interparticle pore region, and, if present, the intraparticle pore region. Once the intraparticle pore size range is known, it is possible to subtract the remaining interparticle and interaggregate pore volumes from the total pore volume to obtain only the desired pore volume of the internal pores as pore volume per unit mass (specific pore volume). Of course, the same subtraction principle applies to isolating any other pore size region of interest.

[0300] Amount of surface treatment layer The amount of the treatment layer of magnesium ion- and / or calcium ion-containing material is theoretically calculated from the BET value of the untreated magnesium ion- and / or calcium ion-containing material and the amount of one or more compounds used for the surface treatment, with 100% of the one or more compounds being present as a surface treatment layer on the surface of the magnesium ion- and / or calcium ion-containing material.

[0301] molecular weight Number average molecular weight M n is determined by gel permeation chromatography according to ISO 16014-1:2019 and ISO 16014-2 / 2019.

[0302] Acid value Acid number is measured according to ASTM D974-14.

[0303] Iodine value The iodine number is determined in accordance with DIN 53241 / 1.

[0304] Total Residual Moisture Content The total residual moisture content was measured by thermogravimetric analysis (TGA). The TGA was performed using a Mettler-Toledo TGA / DSC1 (TGA 1 STARe System) with a 900 μL aluminum oxide crucible. The method consisted of several heating steps (80 mL / min) under air. The first step was heating from 25 to 105 °C at a heating rate of 20 °C / min (Step 1). The temperature was then maintained at 105 °C for 10 min (Step 2). Heating was then continued from 105 to 400 °C at a heating rate of 20 °C / min (Step 3). The temperature was then maintained at 400 °C for 10 min (Step 4). Finally, heating was continued from 400 to 600 °C at a heating rate of 20 °C / min (Step 5). The total residual moisture content was the cumulative weight loss after Steps 1 and 2.

[0305] Analysis of crosslinked elastomer product samples For all tests on cured polymer product samples, a minimum of 16 hours was allowed between molding and testing the product samples. The samples were kept in a controlled environment (temperature: 23±2°C, relative humidity (RH): 50±5%).

[0306] Tensile strength, elongation at break, modulus M300 and modulus M100: Tensile strength, elongation at break, modulus M300 and modulus M100 were measured according to NF ISO 37 on a Zwick T2000, Zwick Z005 or Zwick Z100 machine using the parameters outlined in Table 1 below.

[0307] [Table 1]

[0308] Tear resistance Tear resistance (DELFT) was measured according to NF ISO 34-2 on Zwick T2000, Zwick Z005, and Zwick Z100 instruments using the parameters outlined in Table 2.

[0309] [Table 2]

[0310] Shore A hardness Hardness (Shore A) was measured according to NF ISO 7619-1 on a Bareiss Digitest II instrument using the parameters outlined in Table 3.

[0311] [Table 3]

[0312] IRHD hardness Hardness (IRHD) was measured according to NF ISO 48-1 on a Wallace IRHD H14 / 1 + Gibitre-PC type N automatic device using the parameters outlined in Table 4.

[0313] [Table 4]

[0314] Compression set These tests were performed on cylindrical molded rubber specimens, Compression Set Plot Type B. The specimens had a diameter of 13.0±0.5 mm and a thickness of 6.3±0.3 mm. Testing was performed at 100°C for 72 hours using the parameters outlined in Table 5.

[0315] [Table 5]

[0316] electrical resistivity Electrical resistivity was measured in accordance with ISO 14309 using a Keithley electrometer, type 6517B, with the parameters outlined in Table 6.

[0317] [Table 6]

[0318] 2. Materials used The materials used for the present invention had the following properties:

[0319] Treatment agent A Treating agent A is a grafted polybutadiene homopolymer containing at least one succinic anhydride group (M), obtained by grafting a polybutadiene homopolymer with maleic anhydride, commercially available from Cray Valley under the trade name RICON® 130MA8. n = 3100 Da, Brookfield viscosity (25°C) = 6500 cPs ± 3500, functional groups / chain = 2, anhydride equivalent weight 1238; acid number: 40.1-51.5 meq KOH / g, total acid: 7-9 wt%, microstructure (mol % of butadiene): 20-35% 1,2-vinyl functionality.

[0320] Treatment agent B Treating agent B is a grafted polybutadiene homopolymer containing at least one succinic anhydride group (M), obtained by grafting a polybutadiene homopolymer with maleic anhydride, commercially available from Cray Valley under the trade name RICON® 131MA10. n = 5000 Da, Brookfield viscosity (25°C) = 48000 cPs, functional groups / chain = 5, anhydride equivalent weight 981).

[0321] Treatment Agent C Treating agent C is a grafted polybutadiene homopolymer containing at least one succinic anhydride group (M), obtained by grafting a polybutadiene homopolymer with maleic anhydride, commercially available from Cray Valley Corporation under the trade name RICON® 156MA17. n = 2500 Da, Brookfield viscosity (55°C) = 140000 cPs, functional groups / chain = 3, anhydride equivalent weight 583).

[0322] Treatment Agent D Treating agent D is a low molecular weight grafted polybutadiene-styrene copolymer containing at least one succinic anhydride group obtained by grafting a polybutadiene-styrene copolymer with maleic anhydride (M), commercially available from Cray Valley under the trade name RICON® 184MA6. n = 9900 Da, Brookfield viscosity (45°C) = 170000 cPs, functional groups / chain = 6, anhydride equivalent weight 1651, acid value = 28.5 to 40 meq KOH / g, styrene content: 17 to 27 wt%.

[0323] Treatment Agent E Treating agent E was (bis[3-(triethoxysilyl)propyl]tetrasulfide) from Sigma-Aldrich (CAS: 40372-72-3).

[0324] Treatment Agent F Treatment F is a mono-substituted alkenyl succinic anhydride (2,5-furandione, dihydro-, mono-C), which is a blend of predominantly branched octadecenyl succinic anhydride (CAS No. 28777-98-2) and predominantly branched hexadecenyl succinic anhydride (CAS No. 32072-96-1). 15-20 The blend consisted of branched octadecenyl succinic anhydride (a branched octadecenyl succinic anhydride derivative, CAS No. 68784-12-3). More than 80% of this blend was branched octadecenyl succinic anhydride. The purity of the blend was >95 wt%. The residual olefin content was less than 3 wt%.

[0325] Treatment Agent G Treatment G was a fatty acid mixture that was a 1:1 mixture of stearic acid and palmitic acid.

[0326] Treatment Agent H Treating agent H is a maleic anhydride functionalized low molecular weight vinyl butadiene (M) commercially available under the trade name RICOBOND® 1031 (Cray Valley).n = 5000 g / mol, Brookfield viscosity (25°C): 48000 cps, 28 wt% 1,2-vinyl functionality; functional groups / chain = 5).

[0327] Calcium carbonate-containing filler material 1 (powder 1) Powder 1 is dry-laid ground calcium carbonate (d 50 (wt) = 3.4 μm, d 98 (wt)=14μm, BET specific surface area=2.6m 2 / g).

[0328] Calcium carbonate-containing filler material 2 (powder 2) Powder 2 is a dry-laid ground calcium carbonate surface-treated with stearic acid from Italy (d 50 (wt) = 3.4 μm, d 98 (wt)=14μm, BET specific surface area=2.6m 2 / g).

[0329] Filler material 3 (powder 3) containing surface-treated calcium carbonate 900 g of Powder 1 was placed in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) and mixed for 10 minutes at 2000 rpm and 120°C. Then, 0.8 parts by weight of Treating Agent A (7.2 g) per 100 parts by weight of CaCO3 was added to the mixture. Stirring and heating were then continued for an additional 20 minutes at 120°C and 2000 rpm. The mixture was then allowed to cool, and a free-flowing powder was recovered (Powder 3).

[0330] Filler material 4 (powder 4) containing surface-treated calcium carbonate 900 g of Powder 1 was placed in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) and mixed for 10 minutes at 2000 rpm and 120°C. Then, 0.8 parts by weight of Treating Agent B (7.2 g) per 100 parts by weight of CaCO3 was added to the mixture. Stirring and heating were then continued for an additional 20 minutes at 120°C and 2000 rpm. The mixture was then allowed to cool, and a free-flowing powder was recovered (Powder 4).

[0331] Filler material 5 (powder 5) containing surface-treated calcium carbonate 900 g of Powder 1 was placed in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) and mixed for 10 minutes at 2000 rpm and 120°C. Then, 0.8 parts by weight of Treating Agent C (7.2 g) per 100 parts by weight of CaCO3 was added to the mixture. Stirring and heating were then continued for an additional 20 minutes at 120°C and 2000 rpm. The mixture was then allowed to cool, and a free-flowing powder was recovered (Powder 5).

[0332] Filler material 6 (powder 6) containing surface-treated calcium carbonate 900 g of Powder 1 was placed in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) and mixed for 10 minutes at 2000 rpm and 120°C. Then, 0.8 parts by weight of Treating Agent D (7.2 g) per 100 parts by weight of CaCO3 was added to the mixture. Stirring and heating were then continued for an additional 20 minutes at 120°C and 2000 rpm. The mixture was then allowed to cool, and a free-flowing powder was recovered (Powder 6).

[0333] Filler material 7 (powder 7) containing surface-treated calcium carbonate 900 g of Powder 1 was placed in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) and mixed for 10 minutes at 2000 rpm and 120°C. Then, 0.4 parts by weight of Treating Agent A (3.6 g) per 100 parts by weight of CaCO3 and 0.4 parts by weight of Treating Agent G (3.6 g) per 100 parts by weight of CaCO3 were added directly to the mixture in the given order. Stirring and heating were then continued for an additional 20 minutes at 120°C and 2000 rpm. The mixture was then allowed to cool, and a free-flowing powder was recovered (Powder 7).

[0334] Filler material 8 (powder 8) containing surface-treated calcium carbonate 900 g of Powder 1 was placed in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) and mixed for 10 minutes at 2000 rpm and 120°C. Then, 0.4 parts by weight of Treating Agent A (3.6 g) per 100 parts by weight of CaCO3 and 0.4 parts by weight of Treating Agent F (3.6 g) per 100 parts by weight of CaCO3 were added directly to the mixture in the given order. Stirring and heating were then continued for an additional 20 minutes at 120°C and 2000 rpm. The mixture was then allowed to cool, and a free-flowing powder was recovered (Powder 8).

[0335] Surface-treated calcium carbonate-containing filler material 9 (powder 9) Powder 9 was a wet-ground and dry-seed ground calcium carbonate from Norway that had been partially treated with treating agent G (0.6 wt%) (d 50 (wt) = 0.3 μm, d 98 (wt) = 1.4 μm (measured by sedigraph), BET specific surface area = 14.4 m 2 / g).

[0336] Filler material 10 (powder 10) containing surface-treated calcium carbonate 400 g of Powder 9 was placed in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) and mixed for 5 minutes at 800 rpm and 120°C. Then, 2.5 parts by weight of Treating Agent A (10 g) per 100 parts by weight of CaCO3 were added to the mixture. Stirring and heating were then continued for an additional 10 minutes at 120°C and 800 rpm. The mixture was then allowed to cool, and a free-flowing powder was recovered (Powder 10). The resulting material had a residual total moisture content of 0.08 wt. % based on the total dry weight of the at least one calcium carbonate-containing material.

[0337] Filler material 11 (powder 11) containing surface-treated calcium carbonate 400 g of Powder 9 was placed in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) and mixed for 5 minutes at 1000 rpm and 90°C. Then, 2.5 parts by weight of Treating Agent E (10 g) per 100 parts by weight of CaCO3 was added to the mixture. Stirring and heating were then continued for an additional 15 minutes at 90°C and 1000 rpm. The mixture was then allowed to cool, and a free-flowing powder was recovered (Powder 11).

[0338] Filler material 12 (powder 12) containing precipitated calcium carbonate Powder 12 was precipitated calcium carbonate from Austria (d 50 (wt) = 1.5 μm, d 98 (wt) = 8 μm (measured by sedigraph), BET specific surface area = 34.4 m 2 / g).

[0339] Filler material 13 (powder 13) containing surface-treated precipitated calcium carbonate Powder 13 was prepared by surface treating Powder 12 with 2.5 wt % of Treating Agent A. To carry out this treatment, Treating Agent A (25 g) was first dispersed in 200 mL of deionized water, heated to 60° C., and neutralized to pH 10 with sodium hydroxide solution. A suspension of Powder 12 (1.00 kg in 7 L of deionized water) was prepared in a 10 L ESCO batch reactor and heated to 85°C. The pH was adjusted to 10 with Ca(OH)2, and then the neutralized treating agent was added with vigorous stirring. Mixing was continued at 85°C for 45 minutes, and then the suspension was transferred to a metal tray and dried in an oven (110°C). The dried cake was then deagglomerated using a Retsch SR300 rotor beater mill.

[0340] Filler material 14 (powder 14) containing precipitated calcium carbonate Powder 14 was precipitated calcium carbonate from Austria (d 50 (wt) = 2.7 μm, d 98 (wt) = 3.9 μm (measured by sedigraph), BET specific surface area = 70.8 m 2 / g).

[0341] Filler material 15 (powder 15) containing surface-treated precipitated calcium carbonate Powder 15 was prepared by surface treating Powder 14 with 2.5 wt % of Treating Agent A. To carry out this treatment, Treating Agent A (25 g) was first dispersed in 200 mL of deionized water, heated to 60° C., and neutralized to pH 10 with sodium hydroxide solution. A suspension of Powder 14 (1.00 kg in 7 L of deionized water) was prepared in a 10 L ESCO batch reactor and heated to 85°C. The pH was adjusted to 10 with Ca(OH)2, and then the neutralized treating agent was added with vigorous stirring. Mixing was continued at 85°C for 45 minutes, and then the suspension was transferred to a metal tray and dried in an oven (110°C). The dried cake was then deagglomerated using a Retsch SR300 rotor beater mill.

[0342] Filler material 16 (powder 16) containing calcined kaolin Powder 16 has a d of 2 μm 50 The kaolin was a high purity fully calcined kaolin from Imerys (Polestar 200P) with a % wt (measured by sedigraph).

[0343] Filler material 17 containing carbon black (powder 17) Powder 17 was N550 carbon black filler obtained from Orion engineered Carbons GmbH (Purex® HS 45, iodine number: 43±5 mg / g; STSA surface area (according to ASTM D 6556): 39±5 m). 2 / g).

[0344] Filler material 18 (powder 18) containing precipitated silica Powder 18 is 180m 2 The silica was precipitated silica from Evonik (Ultrasil VN3) with a BET specific surface area of ​​0.1g / g.

[0345] Filler material 19 (powder 19) containing calcined kaolin Powder 19 has a d of 2 μm 50 The kaolin was a high purity fully calcined kaolin from Imerys (Polestar 200R) with

[0346] Filler material 20 (powder 20) containing calcium carbonate Powder 20 has a d of 2.4 μm 50 , 9 μm d 98 , and 2.0m 2 The calcium carbonate was from Imerys (Micronic O) with a BET specific surface area of ​​0.15 g / g.

[0347] Filler 21 (powder 21) containing surface-reacted calcium carbonate Powder 21 is a surface-reacted calcium carbonate (BET = 85m) consisting of 80% hydroxyapatite and 20% calcite. 2 / g, d 50 (vol) = 6.1 μm, d 98 (vol)=13.8 μm; measured by laser diffraction) and was prepared in the following manner: 350 litres of an aqueous suspension of (sediment) ground calcium carbonate was prepared in a mixing vessel by adjusting the solids content of ground marble calcium carbonate from Hustadmarmor, Norway, having a particle size distribution of 90% by weight below 2 μm, as measured by sedimentation, to give a solids content of 10% by weight, based on the total weight of the aqueous suspension. While the suspension was being mixed, 62 kg of 30% concentrated phosphoric acid was added to the suspension over a period of 10 minutes at a temperature of 70° C. Finally, after the phosphoric acid was added, the slurry was stirred for an additional 5 minutes before being removed from the vessel and allowed to dry.

[0348] Filler 22 (powder 22) containing surface-treated surface-reacted calcium carbonate Powder 22 was prepared by surface treating Powder 21 with 7.5% Treating Agent E. The surface treatment was carried out in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany). Powder 21 (300 g) was placed in the mixer and stirred at 500 rpm and room temperature. Treating Agent E (7.5 wt %, 24 g) was then added dropwise to the mixture, and stirring was continued for an additional 10 minutes. The mixture was then allowed to cool, and the powder was collected.

[0349] Precipitated Hydromagnesite Filler 23 (Powder 23) Powder 23 was precipitated hydromagnesite (BET specific surface area: 84.2 m 2 / g, d 50 (vol) = 7.6 μm, d 95 (vol)=20.6 μm).

[0350] Surface-treated precipitated hydromagnesite filler 24 (powder 24) Powder 24 was prepared by surface treating Powder 23 with 2.5 wt % of Treating Agent A. To perform this treatment, Treating Agent A (25 g) was first dispersed in 100 mL of deionized water, heated to 60°C, and neutralized to a pH of 9-10 with sodium hydroxide solution. A suspension of Powder 23 (1 kg in 7.5 L deionized water) was prepared in a 10 L ESCO batch reactor (ESCO-Labor AG, Switzerland) and heated to 85 °C. The pH was adjusted to 10-11 with Ca(OH)2, and the neutralized treatment agent was then added with vigorous stirring. Mixing continued at 85 °C for 45 min, after which the suspension was transferred to a metal tray and dried in an oven (110 °C). The dried cake was then deagglomerated using an SR300 rotor beater mill (Retsch GmbH, Germany).

[0351] Calcined kaolin-containing filler material 25 (powder 25) Powder 25 has a d of 0.6 μm 50 was a fine calcined kaolin from Imerys (Polestar 400) with

[0352] Filler material 26 (powder 26) containing surface-treated calcium carbonate Powder 26 was a wet-ground and dry-heap ground calcium carbonate from Norway treated with Treatment Agent G (3.6 wt%) (d 50 (wt) = 0.3 μm, d 98 (wt)=1.4μm, BET specific surface area=14.4m 2 / g). The material had a residual total moisture content of 0.08 wt. % based on the total dry weight of the at least one calcium carbonate-containing material.

[0353] Precipitated Hydromagnesite Filler 27 (Powder 27) Powder 27 was precipitated hydromagnesite (BET specific surface area = 46.7 m 2 / g, d 50 (vol) = 8.75 μm, d 98 (vol)=29 μm). The material had a residual total moisture content of 3.76 wt. %, based on the total dry weight of the at least one calcium carbonate-containing material.

[0354] Surface-treated precipitated hydromagnesite filler 28 (powder 28) Powder 28 was prepared by surface treating Powder 27 with 3 wt. % of Treating Agent G and 3 wt. % of Treating Agent A. To perform this treatment, Treating Agent G (25 g) was first dispersed in 500 mL of deionized water, heated to 80 °C, and a solution of 5.4 g of sodium hydroxide dissolved in 100 mL of water was added. The corresponding sodium salt was dissolved in water. In parallel, Treating Agent A (24 g) was first dispersed in 400 mL of deionized water, heated to 60 °C, and neutralized to pH 9-10 with sodium hydroxide. A suspension of Powder 27 (800 g in 5 L of deionized water) was then prepared in a 10 L ESCO batch reactor (ESCO-Labor AG, Switzerland) and heated to 85°C. The neutralized treating agent prepared above was then added with vigorous stirring. Mixing was continued at 80°C for 45 minutes. The suspension was then filtered on a filter press, and the filter cake was then transferred to a metal tray and dried in an oven (110°C). The dried cake was then deagglomerated using an SR300 rotor beater mill equipped with a 200 μm sieve (Retsch GmbH, Germany). This material had a residual total moisture content of 1.48 wt. %, based on the total dry weight of the at least one calcium carbonate-containing material.

[0355] Carbon Black Filler Material 29 (Powder 29) Powder 29 is N220 carbon black filler commercially available from Cabot Corporation as Vulcan® 6, with an iodine value of 121 mg / kg and an STSA surface area (according to ASTM D 6556) of 104 m 2 / g.

[0356] Calcium carbonate-containing filler material 30 (powder 30) Powder 30 is a ground calcium carbonate powder (Micromya-OM) manufactured in France, 50 (wt) = 2.4 μm, d 98 (wt)=20 μm. The material had a residual total moisture content of 0.01 wt. %, based on the total dry weight of the at least one calcium carbonate-containing material.

[0357] Filler 31 (powder 31) containing surface-treated surface-reacted calcium carbonate ) Powder 31 was prepared by surface treating Powder 21 with 7 wt. % Treating Agent F. The surface treatment was carried out in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany). Powder 21 (500 g) was placed in the mixer and stirred at 500 rpm and 120°C. Treating Agent F (7 wt. %, 35 g) was then added dropwise to the mixture, and stirring was continued for an additional 15 minutes. The mixture was then allowed to cool, and the powder was recovered. The resulting material had a residual total moisture content of 1.09 wt. % based on the total dry weight of the at least one calcium carbonate-containing material, and a moisture absorption of 17 mg / g.

[0358] Filler 32 (powder 32) containing surface-treated, surface-reacted calcium carbonate Powder 32 was prepared by surface treating Powder 21 with 8 wt% of Treating Agent E. The surface treatment was carried out in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany). Powder 21 (500 g) was placed in the mixer and stirred at 500 rpm and 70°C. Treating Agent E (8 wt%, 40 g) was then added dropwise to the mixture, and stirring was continued for an additional 15 minutes. The mixture was then allowed to cool, and the powder was collected.

[0359] Filler 33 (powder 33) containing surface-treated, surface-reacted calcium carbonate Powder 33 was prepared by surface treating Powder 21 with 7.5 wt % of Treating Agent H. To perform this treatment, the treating agent (60 g) was first dispersed in 400 mL of deionized water, heated to 60°C, and neutralized to a pH of 9-10 with sodium hydroxide. A suspension of Powder 21 (0.8 kg in 6 L deionized water) was prepared in a 10 L ESCO batch reactor (ESCO-Labor AG, Switzerland) and heated to 85 °C. The pH was adjusted to 10-11 with Ca(OH)2, and then the neutralized treatment agent was added with vigorous stirring. Mixing was continued at 85 °C for 45 minutes. The suspension was then filtered using a filter press (approximately 6 bar). The filter cake was then transferred to a metal tray and dried in an oven (110 °C). The dried cake was then deagglomerated using an SR300 rotor beater mill (Retsch GmbH, Germany). The resulting material had a residual total moisture content of 1.43 wt. % based on the total dry weight of the at least one calcium carbonate-containing material.

[0360] Precipitated Hydromagnesite Filler 34 (Powder 34) Powder 34 was precipitated hydromagnesite (BET specific surface area = 46.7 m 2 / g, d 50 (vol) = 8.8 μm, d 98 (vol)=29 μm, moisture absorption=27.2 mg / g). The material had a residual total moisture content of 3.74 wt. %, based on the total dry weight of the at least one calcium carbonate-containing material.

[0361] Surface-treated precipitated hydromagnesite filler 35 (powder 35) Powder 35 was prepared by surface treating Powder 34 with 7.5 wt. % of Treating Agent A. To carry out this treatment, the treating agent (64 g) was first dispersed in 400 mL of deionized water, heated to 60° C., and neutralized to a pH of 10 with sodium hydroxide solution. A suspension of Powder 34 (850 g in 6 L of deionized water) was prepared in a 10 L ESCO batch reactor and heated to 85°C. The pH was adjusted to 10 with Ca(OH)2, and then the neutralized treating agent was added with vigorous stirring. Mixing was continued at 85°C for 45 minutes, after which the suspension was filtered on a filter press and dried overnight in an oven (110°C). The dried filter cake was then deagglomerated using a Retsch SR300 rotor beater mill. The resulting material had a residual total moisture content of 1.78 wt. % based on the total dry weight of the at least one calcium carbonate-containing material.

[0362] Surface-treated precipitated hydromagnesite filler 36 (powder 36) Powder 36 was prepared by treating precipitated hydromagnesite powder with treating agent E. The surface treatment was carried out in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany). Untreated precipitated hydromagnesite powder (400 g) was placed in the mixer and stirred at 500 rpm and 70°C. Treating agent E (7.5 wt%, 30 g) was then added dropwise to the mixture, and stirring was continued for an additional 15 minutes. The mixture was then allowed to cool, and the powder was recovered (BET specific surface area = 32.8 m). 2 / g, d 50 (vol) = 8.6 μm, d 98 (vol)=45 μm).

[0363] Surface-treated precipitated calcium carbonate filler 37 (powder 37) Powder 37 is a precipitated calcium carbonate (BET surface area = 70 m) from Austria. 2 / g, d 50 The surface treatment was carried out in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany). Untreated precipitated calcium carbonate (400 g) was placed in the mixer and stirred at 500 rpm and 70°C. Treatment agent E (7.5 wt%, 75 g) was then added dropwise to the mixture, and stirring was continued for a further 15 minutes. Afterwards, it was allowed to cool and the powder was recovered (BET specific surface area = 50 m 2 / g). The resulting material had a residual total moisture content of 1.3 wt. %, based on the total dry weight of the at least one calcium carbonate-containing material.

[0364] Filler material 38 (powder 38) containing surface-treated calcium carbonate Powder 38 is ultrafine ground calcium carbonate (BET specific surface area = 16 m) produced from eggshells. 2 / g, d 50 (wt) = 0.7 μm, d 98 A calcium carbonate powder (wt = 4.1 μm) was prepared by treating it with 0.6% treating agent F, 1.2% treating agent A, and 1% treating agent E. The surface treatment was carried out in a high-speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany). Untreated calcium carbonate powder (1 kg) was placed in the mixer and stirred at 500 rpm and 120°C. These treating agents were then added successively to the mixture, and stirring was continued for another 15 minutes. After that, it was allowed to cool and the powder was recovered (BET specific surface area = 12 m). 2 / g). The resulting material had a residual total moisture content of 0.30 wt. % based on the total dry weight of the at least one calcium carbonate-containing material.

[0365] Filler 39 (powder 39) containing surface-reacted calcium carbonate Powder 39 is a surface-reacted calcium carbonate (BET specific surface area = 139 m 2 / g, d 50 (vol) = 6.1 μm, d 98 (vol)=14.2 μm) and was prepared in the following manner: 350 litres of an aqueous suspension of natural ground calcium carbonate was prepared in a mixing vessel by adjusting the solids content of ground marble calcium carbonate from Hustadmarmor, Norway, having a particle size distribution of 90% by weight below 2 μm, as determined by sedimentation, to give a solids content of 10% by weight based on the total weight of the aqueous suspension. While the suspension was being mixed, 62 kg of 30% concentrated phosphoric acid was added to the suspension over a period of 10 minutes at a temperature of 70° C. Additionally, during the phosphoric acid addition, 1.9 kg of citric acid was rapidly added (approximately 30 seconds) to the slurry. Finally, after the phosphoric acid addition, the slurry was stirred for an additional 5 minutes before being removed from the vessel and allowed to dry.

[0366] Filler 40 (powder 40) containing surface-treated, surface-reacted calcium carbonate Powder 40 was prepared by surface treating Powder 39 with 5 wt. % of Treating Agent A. To perform this treatment, the treating agent (35 g) was first dispersed in 300 mL of deionized water, heated to 60° C., and neutralized to pH 10 with sodium hydroxide. A suspension of Powder 39 (700 g in 7 L of deionized water) was prepared in a 10 L ESCO batch reactor and heated to 85°C. The pH was adjusted to 10 with Ca(OH)2, and then the neutralized treating agent was added with vigorous stirring. Mixing was continued at 85°C for 45 minutes, after which the suspension was filtered through a Buchner funnel and dried overnight in an oven (110°C). The dried filter cake was then deagglomerated using a Retsch SR300 rotor beater mill.

[0367] Precipitated Hydromagnesite Filler 41 (Powder 41) Powder 41 was precipitated hydromagnesite (BET specific surface area = 46.7 m 2 / g, d 50 (vol) = 8.75 μm, d 98 (vol) = 29 μm).

[0368] Surface-treated precipitated hydromagnesite filler 42 (powder 42) Powder 42 was prepared by surface treating Powder 41 with 5 wt. % of Treating Agent A. To carry out this treatment, the treating agent (35 g) was first dispersed in 400 mL of deionized water, heated to 60° C., and neutralized to pH 10 with sodium hydroxide. A suspension of Powder 41 (700 g in 6 L of deionized water) was prepared in a 10 L ESCO batch reactor and heated to 85°C. The pH was adjusted to 10 with Ca(OH)2, and then the neutralized treating agent was added with vigorous stirring. Mixing continued at 85°C for 45 minutes, after which the suspension was filtered on a filter press and dried overnight in an oven (110°C). The dried filter cake was then deagglomerated using a Retsch SR300 rotor beater mill.

[0369] Precipitated Hydromagnesite Filler 43 (Powder 43) Powder 43 was produced by wet milling powder 41 (BET specific surface area = 46.5 m 2 / g, d 50 (vol) = 7.9 μm; d 98 (vol)=27 μm). The material had a residual total moisture content of 1.2 wt. %, based on the total dry weight of the at least one calcium carbonate-containing material.

[0370] Filler 44 (Powder 44) containing surface-treated, surface-reacted calcium carbonate Powder 44 was prepared by surface treating Powder 21 with 5 wt. % of Treating Agent A. To perform this treatment, the treating agent (35 g) was first dispersed in 400 mL of deionized water, heated to 60°C, and neutralized with sodium hydroxide to a pH of 9-10. A suspension of Powder 21 (0.7 kg in 6 L deionized water) was prepared in a 10 L ESCO batch reactor (ESCO-Labor AG, Switzerland) and heated to 85 °C. The pH was adjusted to 10-11 with Ca(OH)2, and then the neutralized treatment agent was added with vigorous stirring. Mixing was continued at 85 °C for 45 min. The suspension was then filtered using a filter press (approximately 6 bar). The filter cake was then transferred to a metal tray and dried in an oven (110 °C). The dried cake was then deagglomerated using an SR300 rotor beater mill (Retsch GmbH, Germany).

[0371] Filler material 45 (powder 45) containing surface-treated calcium carbonate Powder 45 is ultrafine ground calcium carbonate (BET specific surface area = 44.1 m) surface treated with 2% Treatment Agent A and 15% Treatment Agent G.2 / g). The resulting material had a residual total moisture content of 0.5 wt. %, based on the total dry weight of the at least one calcium carbonate-comprising material.

[0372] 3. Working Example Example Series A: Elastomer Compounds Formula: Process 1: Internal mixing The first step is a 300cm boiler equipped with a Banbury rotor. 3 Each batch was mixed in a HAAKE internal mixer with a capacity of 1000 ml. The temperature was set at 40° C. at the beginning of each mix and increased to 90° C. during processing, depending on the filler incorporated. For each batch, the mixing procedure shown in Table 7 below was used (Table 7).

[0373] [Table 7]

[0374] Process 2-External mixing In the second step, mixing with the peroxide curing agent was performed in an instrumented cylinder mixer (150 x 350). All rubbers were mixed for the same time, cylinder speed, and cylinder spacing to avoid affecting the comparison of their rheological properties. The cooling system was set to 25°C, and the metal guides were set to allow the rubber to occupy 70% of the cylinder surface. Between the two accelerations, the cylinder was cleaned and allowed to cool. The detailed procedure for this process is described in Table 8 below.

[0375] [Table 8]

[0376] Process 3: Molding Then, at 160°C or 180°C, 100 kg / cm 2Pieces were formed by compression molding at a pressure of 150 x 150 x 2 mm. Small sheets of 150 x 150 x 2 mm were prepared in this manner. The setting time, which determines the molding time, was determined by a rheological MDR test. Examples of Series A are shown in Table 9 below.

[0377] [Table 9]

[0378] The effects on the mechanical properties - tensile test - and various other mechanical properties of the Series A elastomer compounds are shown in Tables 10 and 11 below.

[0379] [Table 10]

[0380] [Table 11]

[0381] Example Series B: EPDM, Sulfur-Cured Formulations Formula: Process 1: Internal mixing The first step is a 300cm boiler equipped with a Banbury rotor. 3 Each batch was mixed in a HAAKE internal mixer with a capacity of 1000. The temperature was set at 40° C. at the beginning of each mix and increased to 90° C. during processing, depending on the filler incorporated. The mixing procedure shown in Table 12 below was used for each batch.

[0382] [Table 12]

[0383] Process 2-External mixing In the second step, mixing with the peroxide curative was performed in an instrumented cylinder mixer (150 x 350). All rubbers were mixed for the same time, cylinder speed, and cylinder spacing to avoid affecting the comparison of their rheological properties. The cooling system was set to 25°C, and the metal guides were set to allow the rubber to occupy 70% of the cylinder surface. Between the two accelerations, the cylinder was cleaned and allowed to cool. The detailed procedure for this process is described in Table 13 below.

[0384] [Table 13]

[0385] Process 3: Molding Then, at 160°C or 180°C, 100 kg / cm 2 Pieces were formed by compression molding at a pressure of 150 x 150 x 2 mm. Small sheets of 150 x 150 x 2 mm were prepared in this manner. The setting time, which determines the molding time, was determined by a rheological MDR test. Examples of Series B are shown in Table 14 below.

[0386] [Table 14]

[0387] The effects on the mechanical properties - tensile test - and various other mechanical properties of the Series B elastomer compounds are shown in Tables 15 and 16 below.

[0388] [Table 15]

[0389] [Table 16]

[0390] Example Series C: Simple EPDM Formulations Formula: Process 1: Internal mixing The first step is a 300cm boiler equipped with a Banbury rotor. 3 Each batch was mixed in a HAAKE internal mixer with a capacity of 1000 ml. The temperature was set at 40° C. at the beginning of each mix and increased to 90° C. during processing, depending on the filler incorporated. The mixing procedure shown in Table 17 below was used for each batch.

[0391] [Table 17]

[0392] Process 2-External mixing In the second step, mixing with the peroxide curative was performed in an instrumented cylinder mixer (300 x 700 or 150 x 350). All rubbers were mixed for the same time, cylinder speed, and cylinder spacing to avoid affecting the comparison of their rheological properties. The cooling system was set to 25°C, and the metal guides were set to allow the rubber to occupy 70% of the cylinder surface. Between the two accelerations, the cylinder was cleaned and allowed to cool. The detailed procedure for this process is described in Table 18 below.

[0393] [Table 18]

[0394] Process 3: Molding The pieces were then compression molded at 160°C and 200 bar pressure. Small 150 x 150 x 2 mm sheets were prepared in this manner. The curing time, which determines the molding time, was determined by rheological MDR testing. Examples of Series C are shown in Table 19 below.

[0395] [Table 19]

[0396] The effects on various mechanical properties of the Series C elastomer compounds are shown in Tables 20, 21 and 22 below.

[0397] [Table 20]

[0398] [Table 21]

[0399] [Table 22]

[0400] Example Series D: Elastomer Compounds Formula: The formulations were carried out in a similar manner as described in Example Series A.

[0401] [Table 23]

[0402] The effects on the mechanical properties - tensile test - and various other mechanical properties of the Series D elastomer compounds are shown in Tables 24 and 25 below.

[0403] [Table 24]

[0404] [Table 25]

[0405] Example Series E: Tire Tread Sulfur Cured SBR Compounds Process 1: Internal mixing As a first step, batches of SBR rubber and filler were mixed in a 2 L Banbury internal mixer according to the mixing procedure shown below in Table 26. The temperature was set at 40°C at the start of each mix and increased to 150°C during processing, depending on the filler being incorporated.

[0406] [Table 26]

[0407] Process 2: External mixing For the second step, mixing with the curing system was performed in an external mixer, Agila (300 x 400). All elastomer precursors were mixed for the same time, cylinder speed, and cylinder spacing. The cooling system was set to 40°C, and the metal guides were set to allow the elastomer precursors to occupy 70% of the cylinder surface. The detailed procedure for this process is described in Table 27 below.

[0408] [Table 27]

[0409] Step 3 - Compression molding The sheet of the elastomer composition was heated at 160°C or 180°C and 100 kg / cm 2 The resin was produced by compression molding at a pressure of 1000 kJ / cm. In this way, small plates of 300 x 300 x 2 mm were prepared. The crosslinking time, which determines the molding time, was determined through a rheological MDR test. Following the above procedure, the following elastomer compositions were obtained: Tables 28 and 29. All elastomer compositions had equal volumes of filler. The amount of filler was adjusted depending on the density of the filler to match the volume occupied by 40 phr of carbon black (Powder 29) (indicated by an asterisk in Tables 28 and 29).

[0410] [Table 28]

[0411] [Table 29]

[0412] The resulting elastomer composition had the following mechanical properties, summarized in Table 30 below:

[0413] [Table 30]

[0414] Example Series F: EPDM Elastomer Compounds Process 1: Internal mixing As a first step, each batch was mixed in a 2 L Banbury internal mixer. The temperature was set at 40° C. at the beginning of each mix and increased to 150° C. during processing, depending on the filler incorporated. The following mixing procedure was used for each batch (Table 31):

[0415] [Table 31]

[0416] Process 2: External mixing For the second step, mixing with the peroxide crosslinker was performed in a cylinder mixer (300 x 700). All elastomer precursors were mixed for the same time, cylinder speed, and cylinder spacing. The cooling system was set to 40°C, and the metal guides were set to allow the elastomer precursor to occupy 70% of the cylinder surface. The detailed procedure for this process is described in Table 32 below.

[0417] [Table 32]

[0418] Process 3: Molding Sheets of the elastomer composition were produced by compression molding at 180°C and 200 bar pressure. Small plates measuring 300 x 300 x 2 mm were produced in this way. The curing time, which determines the molding time, was determined by rheological testing in the MDR. The T98 value was taken as the curing time of the press plate. Compression set test specimens were prepared using the same procedure as compression molding. The curing time used was T98 plus 10 minutes, since the thickness of these test specimens was greater than that of the press plate.

[0419] EPDM elastomer composition Following the above method, the following elastomer compositions were obtained: Table 33. All elastomer compositions had equal volumes of filler. All fillers were combined with carbon black at a 50 / 50% volume ratio. Thus, the carbon black reference batch contains 100 phr of N550. The other batches contained 50 phr of N550 and slightly varying amounts of mineral filler depending on their densities, thereby having an amount of mineral filler equal to the volume of 50 phr of carbon black (denoted with an asterisk in Table 33).

[0420] [Table 33]

[0421] The resulting elastomer compositions had the properties shown in Tables 34, 35 and 36 below:

[0422] [Table 34]

[0423] [Table 35]

[0424] [Table 36] The invention disclosed herein includes the following aspects: [1] A calcium carbonate or magnesium carbonate-containing material selected from the group consisting of ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), surface-reacted calcium carbonate (SRCC), precipitated hydromagnesite, and mixtures thereof; a surface treatment composition in an amount of 0.5 to 20% by weight based on the total weight of the calcium carbonate or magnesium carbonate-containing material; A composition formed from the surface treatment composition comprises at least one crosslinking compound containing at least two functional groups, wherein at least one functional group is suitable for crosslinking an elastomeric resin and at least one functional group is suitable for reacting with the calcium carbonate or magnesium carbonate-containing material; composition. [2] The composition according to [1] above, wherein the calcium carbonate-containing material is selected from the group consisting of sedimentary ground calcium carbonate (GCC), marble, limestone, dolomite, chalk, and mixtures thereof, or the precipitated calcium carbonate (PCC) is selected from the group consisting of mineralogical crystal forms of aragonite, vaterite, and calcite, colloidal PCC, and mixtures thereof, preferably. [3] The composition according to [1] or [2] above, wherein the calcium carbonate-containing material is a deposited ground calcium carbonate (GCC) and / or a precipitated calcium carbonate (PCC), and the composition comprises: (i) a weight median particle size d measured by a precipitation method in the range of 0.1 μm to 10 μm, preferably in the range of 0.15 μm to 5 μm, more preferably in the range of 0.2 μm to 3 μm, and most preferably in the range of 0.25 μm to 3 μm, for example, 0.3 μm to 2 μm or 0.3 μm to 1.5 μm; 50 and / or (ii) a top cut (d) measured by sedimentation method of ≦45 μm, preferably ≦30 μm, more preferably ≦20 μm, and most preferably ≦15 μm 98 ); and / or (iii) Nitrogen and 0.5 to 150 m, measured using the BET method according to ISO 9277:2010 2 / g, preferably 1 to 80m 2 / g specific surface area (BET); and / or (iv) a total residual moisture content of ≦2 wt.-%, preferably ≦1.5 wt.-%, more preferably ≦1.2 wt.-%, and most preferably ≦0.8 wt.-%, relative to the total dry weight of said at least one calcium carbonate-comprising material. [4] The calcium carbonate-containing material is a mixture of (sedimentary) ground calcium carbonate or precipitated calcium carbonate and carbon dioxide and one or more H 3 O + surface-reacted calcium carbonate (SRCC), which is a reaction product of the carbon dioxide with the ion donor, 3 O + formed in situ by treatment with an ion donor and / or provided from an external source; or The composition according to [1] above, wherein the magnesium carbonate-containing material is precipitated hydromagnesite and comprises: (i) a volume median particle size d of 0.1 to 75 μm, preferably 0.5 to 50 μm, more preferably 1 to 40 μm, even more preferably 1.2 to 30 μm, and most preferably 1.5 to 15 μm 50 and / or (ii) a volume top cut particle size d of 0.2 to 150 μm, preferably 1 to 100 μm, more preferably 2 to 80 μm, even more preferably 2.4 to 60 μm, and most preferably 3 to 30 μm 98 and / or (iii) 15m measured using nitrogen and BET methods 2 / g~200m 2 / g, preferably 20m 2 / g~180m 2 / g, more preferably 25m 2 / g~140m 2 / g, and even more preferably 27m 2 / g~120m 2 / g, most preferably 30m 2 / g~100m 2 / g specific surface area. [5] The composition according to any one of the above [1] to [3], wherein the at least one functional group of the crosslinking compound suitable for reacting with the calcium carbonate or magnesium carbonate-containing material comprises one or more terminal triethoxysilyl, trimethoxysilyl, and / or organic acid anhydride and / or salts thereof, and / or carboxylic acid group and / or salts thereof. [6] The composition according to any one of the above [1] to [5], wherein the crosslinkable compound is at least one graft polymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a homo- or copolymer containing butadiene units and optionally styrene units, or a compound containing two trialkoxysilylalkyl groups bonded to a sulfur-containing trialkoxysilane, preferably a polysulfide. [7] The composition according to [6] above, wherein the at least one graft polymer is: (a) a grafted polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a polybutadiene homopolymer and having: (i) a number average molecular weight M measured by gel permeation chromatography of 1,000 to 20,000 g / mol, preferably 1,400 to 15,000 g / mol, and more preferably 2,000 to 10,000 g / mol; n and / or (ii) the number of functional groups per chain is in the range of 2 to 12, preferably 2 to 9, more preferably 2 to 6, and / or (iii) an anhydride equivalent weight in the range of 400 to 2200, preferably 500 to 2000, more preferably 550 to 1800; or (b) A grafted polybutadiene-styrene copolymer containing at least one succinic anhydride group obtained by grafting a polybutadiene-styrene copolymer with maleic anhydride and having a 1,2-vinyl content of 20 to 80 mol %, preferably 20 to 40 mol %, based on the total weight of the grafted polybutadiene-styrene copolymer. [8] The composition according to any one of the above items [1] to [7], wherein the composition is formed by providing the at least one calcium carbonate- or magnesium carbonate-containing material and the at least one crosslinking compound as a physical mixture and / or by contacting the at least one calcium carbonate- or magnesium carbonate-containing material with the at least one crosslinking compound, whereby a surface treatment layer comprising the at least one crosslinking compound and / or a salt-containing reaction product thereof is formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material. [9] The composition according to any one of [1] to [8] above, wherein the surface treatment composition comprises at least one additional surface treatment agent selected from the group consisting of: (I) a blend of phosphoric acid esters of one or more phosphoric acid monoesters and / or salts thereof, and / or one or more phosphoric acid diesters and / or salts thereof, and / or (II) at least one saturated or unsaturated aliphatic linear or branched carboxylic acid and / or salt thereof, preferably at least one aliphatic carboxylic acid and / or salt thereof having a total number of carbon atoms of C4 to C24, more preferably at least one aliphatic carboxylic acid and / or salt thereof having a total number of carbon atoms of C12 to C20, most preferably at least one aliphatic carboxylic acid and / or salt thereof having a total number of carbon atoms of C16 to C18, and / or (III) at least one mono-substituted succinic anhydride and / or a salt thereof, which is a succinic anhydride mono-substituted with a group selected from a linear group, a branched group, an aliphatic group, and a cyclic group having a total carbon atom number of at least C2 to C30 in the substituent, and / or (IV) at least one polydialkylsiloxane, and (V) A mixture of one or more materials according to (I) to (IV).

[10] A dry production method for the composition according to any one of [1] to [9] above, comprising at least the following steps: (a) providing a calcium carbonate or magnesium carbonate-containing material selected from the group consisting of ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), surface-reacted calcium carbonate (SRCC), precipitated hydromagnesite, and mixtures thereof; (b) adding at least one crosslinking compound containing at least two functional groups to the calcium carbonate- or magnesium carbonate-containing material in an amount of 0.1 to 10 mg / m based on the total weight of the calcium carbonate- or magnesium carbonate-containing material; 2 wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with said calcium carbonate or magnesium carbonate containing material; (c) optionally providing at least one further surface treatment agent as described in [9] above; (d) optionally, heating the at least one crosslinkable compound; and (e) contacting, with mixing, said calcium carbonate or magnesium carbonate-containing material with said at least one cross-linking compound in one or more steps; ; (f) heating the at least one further surface treatment agent, if present, to a temperature at or above its melting point, thereby obtaining a molten surface treatment agent, and in one or more steps contacting the molten surface treatment agent with the at least one crosslinking compound simultaneously or subsequently with the calcium carbonate or magnesium carbonate-containing material while mixing.

[11] A curable elastomer mixture comprising: (a) an elastomeric resin, and (b) the composition according to any one of the above [1] to [9], in an amount of 5 to 300% by weight, preferably 10 to 150% by weight, more preferably 20 to 110% by weight, and most preferably 40 to 100% by weight, based on the total weight of the elastomer resin; wherein the composition is dispersed in the elastomer resin. Curable elastomer mixture.

[12] The curable elastomer mixture according to

[11] above, wherein the elastomer resin is selected from natural or synthetic rubber, preferably from the group consisting of acrylic rubber, butadiene rubber, acrylonitrile-butadiene rubber, epichlorohydrin rubber, isoprene rubber, ethylene-propylene rubber, ethylene-propylene-diene rubber, nitrile-butadiene rubber, butyl rubber, styrene-butadiene rubber, polyisoprene, hydrogenated nitrile-butadiene rubber, carboxylated nitrile-butadiene rubber, chloroprene rubber, isoprene-isobutylene rubber, chloro-isobutene-isoprene rubber, brominated isobutene-isoprene rubber, silicone rubber, fluorocarbon rubber, polyurethane rubber, polysulfide rubber, thermoplastic rubber, and mixtures thereof.

[13] The mixture may contain color pigments, fibers, such as cellulose, glass or wood fibers, dyes, waxes, lubricants, oxidation- and / or UV-stabilizers, plasticizers, curing agents, crosslinking aids, antioxidants, and other fillers, such as carbon black, TiO 2 , mica, clay, precipitated silica, talc, or calcined kaolin.

[14] A cured elastomer product formed from the curable elastomer mixture according to any one of

[11] to

[13] above.

[15] A method for producing the cured elastomer product according to

[14] above, comprising the steps of: (a) providing an elastomeric resin; (b) providing as a filler 5 to 300 wt. % of at least one calcium carbonate or magnesium carbonate-containing material based on the total weight of the elastomeric resin; (c) 0.1 to 10 mg / m based on the total weight of the calcium carbonate or magnesium carbonate-containing material 2 providing at least one crosslinkable compound comprising at least two functional groups, wherein at least one functional group is suitable for crosslinking the elastomeric resin and at least one functional group is suitable for reacting with said calcium carbonate or magnesium carbonate containing material; (d) optionally providing at least one further surface treatment agent as described in [9] above; (e) optionally, color pigments, fibers, such as cellulose, glass or wood fibers, dyes, waxes, lubricants, oxidation- and / or UV-stabilizers, plasticizers, hardeners, crosslinking aids, antioxidants, and other fillers, such as carbon black, TiO 2 providing further additives such as mica, clay, precipitated silica, talc, or calcined kaolin; (f) contacting, in any order, the components of steps (a), (b), (c) and optionally steps (d) and (e); and (g) curing the mixture resulting from step (f), thereby forming a cured elastomeric product.

[16] The method according to

[15] above, wherein in the contacting step (f), first, in one or more steps, the at least one calcium carbonate- or magnesium carbonate-containing material of step (b) is contacted with the at least one crosslinking compound of step (c) and, if present, subsequently or simultaneously with the at least one further surface treatment agent of step (d), while mixing, so that a surface treatment layer comprising the at least one crosslinking compound and / or a salt-containing reaction product thereof, and optionally the at least one further surface treatment agent and / or a salt-containing reaction product thereof, is formed on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material of step (b); and second, in one or more steps, the surface-treated calcium carbonate- or magnesium carbonate-containing material is contacted with the elastomeric resin of step (a) while mixing.

[17] The method according to

[16] above, wherein in one or more steps, before or after, preferably after, contacting the surface-treated calcium carbonate or magnesium carbonate-containing material with the elastomeric resin in step (a) while mixing, the further additive in step (e) is contacted with the calcium carbonate or magnesium carbonate-containing material while mixing in one or more steps.

[18] The method according to

[15] above, wherein the contacting step (f) is carried out during the curing step (g), in which the at least one crosslinking compound is contacted with the elastomeric resin of step (a) while mixing before or after, preferably after, adding the at least one calcium carbonate or magnesium carbonate-containing material.

[19] Use of at least one crosslinking compound containing at least two functional groups, wherein in the elastomer formulation formed from an elastomer resin and at least one calcium carbonate- or magnesium carbonate-containing material as a filler, at least one functional group is suitable for crosslinking the elastomer resin and at least one functional group is suitable for reacting with the calcium carbonate- or magnesium carbonate-containing material; Use for improving the mechanical properties of an elastomer so formulated compared to the same elastomer formed from the same elastomeric resin and at least one calcium carbonate or magnesium carbonate containing material, but not comprising said at least one crosslinking compound comprising at least two functional groups, at least one functional group being suitable for crosslinking the elastomeric resin and at least one functional group being suitable for reacting with said calcium carbonate or magnesium carbonate containing material.

[20] An article formed from the cured elastomeric product of

[14] above, the article being selected from the group including tubeless articles, membranes, sealings, gloves, pipes, cables, electrical connectors, oil hoses, shoe soles, O-ring seals, shaft seals, gaskets, tubing, valve stem seals, fuel hoses, tank seals, diaphragms, flexible liners for pumps, mechanical seals, pipe couplings, valve lines, military flare blenders, electrical connectors, fuel joints, roll covers, firewall seals, jet engine clips, and the like.

Claims

1. a calcium carbonate or magnesium carbonate containing material selected from the group consisting of ground calcium carbonate (GCC), precipitated hydromagnesite, and mixtures thereof; 0.5 to 20% by weight of a surface treatment composition based on the total weight of the calcium carbonate or magnesium carbonate-containing material; A composition formed from the surface treatment composition comprises at least one crosslinking compound containing at least two functional groups, wherein at least one functional group is a group for crosslinking an elastomeric resin and at least one functional group is a group for reacting with the calcium carbonate or magnesium carbonate-containing material; the at least one functional group of the crosslinking compound for reacting with the calcium carbonate or magnesium carbonate-containing material comprises one or more terminal triethoxysilyl, trimethoxysilyl, and / or organic acid anhydride and / or salts thereof, and / or carboxylic acid groups and / or salts thereof; composition.

2. 10. The composition of claim 1, wherein the heaped ground calcium carbonate (GCC) is selected from the group consisting of marble, limestone, dolomite, chalk, and mixtures thereof.

3. 3. The composition of claim 1 or 2, wherein the calcium carbonate-containing material is heaped ground calcium carbonate (GCC) and comprises: (i) a weight median particle size d measured by the sedimentation method in the range of 0.1 μm to 10 μm 50 and / or (ii) Top cut (d) measured by sedimentation method of ≦45 μm 98 ); and / or (iii) 0.5 to 150 m, measured using nitrogen and the BET method according to ISO 9277:2010 2 / g specific surface area (BET); and / or (iv) a total residual moisture content of ≦2 wt.-%, based on the total dry weight of said at least one calcium carbonate-comprising material.

4. The composition of claim 1, wherein the magnesium carbonate-containing material is precipitated hydromagnesite and has: (i) a volume median particle size d of 0.1 to 75 μm 50 and / or (ii) a volume top cut particle size d of 0.2 to 150 μm 98 and / or (iii) 15 m measured using nitrogen and BET methods 2 / g to 200m 2 / g specific surface area.

5. 5. The composition according to claim 1, wherein the crosslinking compound is at least one graft polymer containing at least one succinic anhydride group obtained by grafting maleic anhydride onto a homo- or copolymer containing butadiene units and optionally styrene units, or a sulfur-containing trialkoxysilane.

6. 6. The composition of claim 5, wherein the at least one graft polymer is: (a) a grafted polybutadiene homopolymer containing at least one succinic anhydride group obtained by grafting a polybutadiene homopolymer with maleic anhydride and having: (i) a number average molecular weight M measured by gel permeation chromatography of 1,000 to 20,000 g / mol n and / or (ii) a number of functional groups per chain ranging from 2 to 12; and / or (iii) an anhydride equivalent weight in the range of 400 to 2200; or (b) a grafted polybutadiene-styrene copolymer containing at least one succinic anhydride group obtained by grafting a polybutadiene-styrene copolymer with maleic anhydride and having a 1,2-vinyl content of 20 to 80 mol %, based on the total weight of the grafted polybutadiene-styrene copolymer.

7. The composition of any one of claims 1 to 6, wherein the surface treatment composition comprises at least one further surface treatment agent selected from the group consisting of: (I) a blend of phosphoric acid esters of one or more phosphoric acid monoesters and / or salts thereof, and / or one or more phosphoric acid diesters and / or salts thereof, and / or (II) at least one saturated or unsaturated aliphatic linear or branched carboxylic acid and / or salt thereof, and / or (III) at least one mono-substituted succinic anhydride and / or a salt thereof, consisting of a succinic anhydride mono-substituted with a group selected from a linear group, a branched group, an aliphatic group, and a cyclic group having a total carbon atom number of at least C2 to C30 in the substituent, and / or (IV) at least one polydialkylsiloxane, and (V) A mixture of one or more materials according to (I)-(IV).

8. A dry process for producing the composition according to any one of claims 1 to 7, comprising at least the following steps: (a) providing a calcium carbonate or magnesium carbonate containing material selected from the group consisting of heaped ground calcium carbonate (GCC), precipitated hydromagnesite, and mixtures thereof; (b) adding at least one cross-linking compound containing at least two functional groups in an amount of 0.1 to 10 mg / m based on the total weight of the calcium carbonate or magnesium carbonate-containing material; 2 Provide in an amount of wherein at least one functional group is a group for crosslinking the elastomeric resin, and at least one functional group is a group for reacting with the calcium carbonate or magnesium carbonate-containing material; the at least one functional group of the crosslinking compound for reacting with the calcium carbonate or magnesium carbonate-containing material comprises one or more terminal triethoxysilyl, trimethoxysilyl, and / or organic acid anhydride and / or salts thereof, and / or carboxylic acid groups and / or salts thereof; (c) optionally providing at least one further surface treatment agent according to claim 7; (d) optionally, heating the at least one crosslinkable compound; and (e) contacting, in one or more steps, the calcium carbonate or magnesium carbonate-containing material with the at least one cross-linking compound while mixing; (f) heating the at least one further surface treatment agent, if present, to a temperature at or above its melting point, thereby obtaining a molten surface treatment agent, and in one or more steps contacting the molten surface treatment agent with the at least one crosslinking compound simultaneously or subsequently with the calcium carbonate or magnesium carbonate-containing material while mixing.

9. A curable elastomeric mixture comprising: (a) an elastomeric resin, and (b) 5 to 300 wt. % of the composition according to any one of claims 1 to 7, based on the total weight of the elastomeric resin; wherein the composition is dispersed in the elastomer resin. Curable elastomer mixture.

10. 10. The curable elastomeric mixture of claim 9, wherein the elastomeric resin is selected from natural or synthetic rubbers.

11. The mixture may contain color pigments, fibers, such as cellulose, glass or wood fibers, dyes, waxes, lubricants, oxidation- and / or UV-stabilizers, plasticizers, hardeners, crosslinking aids, antioxidants, and other fillers, such as carbon black, TiO 2 11. The curable elastomeric mixture of claim 9 or 10, further comprising additives such as mica, clay, precipitated silica, talc, or calcined kaolin.

12. A cured elastomeric product formed from the curable elastomeric mixture of any one of claims 9 to 11.

13. 13. A method for producing the cured elastomeric product of claim 12, comprising the steps of: (a) providing an elastomeric resin; (b) providing as a filler 5 to 300 wt. % of at least one calcium carbonate or magnesium carbonate containing material, based on the total weight of said elastomeric resin; (c) 0.1 to 10 mg / m based on the total weight of the calcium carbonate or magnesium carbonate-containing material 2 providing at least one crosslinkable compound comprising at least two functional groups of wherein at least one functional group is a group for crosslinking the elastomeric resin, and at least one functional group is a group for reacting with the calcium carbonate or magnesium carbonate-containing material; the at least one functional group of the crosslinking compound for reacting with the calcium carbonate or magnesium carbonate-containing material comprises one or more terminal triethoxysilyl, trimethoxysilyl, and / or organic acid anhydride and / or salts thereof, and / or carboxylic acid groups and / or salts thereof; (d) optionally providing at least one further surface treatment agent according to claim 7; (e) optionally, color pigments, fibers, such as cellulose, glass or wood fibers, dyes, waxes, lubricants, oxidation- and / or UV-stabilizers, plasticizers, hardeners, crosslinking aids, antioxidants, and other fillers, such as carbon black, TiO 2 providing further additives such as mica, clay, precipitated silica, talc, or calcined kaolin; (f) contacting, in any order, the components of steps (a), (b), (c) and optionally steps (d) and (e); and (g) curing the mixture resulting from step (f), thereby forming a cured elastomeric product.

14. 14. The method of claim 13, wherein in contacting step (f), first, in one or more steps, the at least one calcium carbonate- or magnesium carbonate-containing material of step (b) is contacted with the at least one crosslinking compound of step (c) and, if present, subsequently or simultaneously with the at least one further surface treatment agent of step (d), while mixing, so that a surface treatment layer comprising the at least one crosslinking compound and / or a salt-containing reaction product thereof, and optionally the at least one further surface treatment agent and / or a salt-containing reaction product thereof, forms on the surface of the at least one calcium carbonate- or magnesium carbonate-containing material of step (b), and second, in one or more steps, the surface-treated calcium carbonate- or magnesium carbonate-containing material is contacted with the elastomeric resin of step (a) while mixing.

15. 15. The method of claim 14, wherein the further additives of step (e) are contacted with the calcium carbonate or magnesium carbonate comprising material while mixing in one or more steps before or after contacting with the elastomeric resin of step (a) while mixing in one or more steps.

16. 14. The method of claim 13, wherein contacting step (f) is carried out during curing step (g), wherein the at least one crosslinking compound is contacted with the elastomeric resin of step (a) while mixing, either before or after adding the at least one calcium carbonate or magnesium carbonate-containing material.

17. Use of at least one crosslinking compound containing at least two functional groups, wherein in the formulation of an elastomer formed from an elastomer resin and at least one calcium carbonate- or magnesium carbonate-containing material as a filler, at least one functional group is a group for crosslinking the elastomer resin and at least one functional group is a group for reacting with the calcium carbonate- or magnesium carbonate-containing material; the at least one functional group of the cross-linking compound for reacting with the calcium carbonate or magnesium carbonate-containing material comprises one or more terminal triethoxysilyl, trimethoxysilyl, and / or organic acid anhydride and / or salts thereof, and / or carboxylic acid groups and / or salts thereof; Use for improving the mechanical properties of an elastomer so formulated compared to the same elastomer formed from the same elastomeric resin and at least one calcium or magnesium carbonate containing material, but not comprising said at least one crosslinking compound comprising at least two functional groups, at least one functional group being a group for crosslinking the elastomeric resin and at least one functional group being a group for reacting with said calcium or magnesium carbonate containing material.

18. 13. An article formed from the cured elastomeric product of claim 12, the article being selected from the group including tubeless articles, membranes, sealings, gloves, pipes, cables, electrical connectors, oil hoses, shoe soles, O-ring seals, shaft seals, gaskets, tubing, valve stem seals, fuel hoses, tank seals, diaphragms, flexible liners for pumps, mechanical seals, pipe fittings, valve lines, military flare blenders, electrical connectors, fuel joints, roll covers, firewall seals, jet engine clips, and the like.

Citation Information

Patent Citations

  • Process for preparing a coarse surface treated filler material product

    EP3628705A1

  • Manufacture of calcium carbonate covered with silicon dioxide

    JP1980113619A

  • Modified low-molecular-weight diene polymer

    JP1984199702A

  • Silane coupling agent treated calcium carbonate and polymer composition

    JP2003112920A

  • Wet surface treatment of surface-modified calcium carbonate

    JP2019503331A