Process for preparing a crude surface-treated filler material product

Abstract

The present invention relates to a process for preparing a surface-treated filler material product, the surface-treated filler material product and an article comprising the surface-treated filler material product.

Description

Technical Field

[0001] The present invention relates to a method for preparing a surface-treated filler material product, the surface-treated filler material product, and an article comprising the surface-treated filler material product. Background Technology

[0002] In practice, filler materials, and especially calcium carbonate-containing filler materials, are commonly used as particulate fillers in polymer articles typically made of polyethylene (PE), polypropylene (PP), polyurethane (PU), polyvinyl chloride (PVC), polyester (PES), and / or polyamide (PA). However, the introduction of additives can provide a coating to the filler material and improve the dispersibility of the mineral filler material within the polymer matrix of the polymer composition, and may improve the processability of this polymer composition and / or the properties of the final polymer article. Eliminating such additives would unacceptably reduce the quality of the resulting polymer article.

[0003] Several attempts have been made in the art to improve the suitability of filler materials, particularly calcium carbonate-containing filler materials, for example by treating such filler materials with surface treatment agents. For example, WO 00 / 20336 relates to an ultrafine natural calcium carbonate, which may optionally be treated with one or more fatty acids or one or more salts or mixtures thereof, and used as a rheology modifier for polymer compositions.

[0004] Similarly, US 4,407,986 relates to a precipitated calcium carbonate surface-treated with a dispersant, the dispersant possibly comprising higher fatty acids and their metal salts, to limit the addition of lubricant additives and prevent the formation of calcium carbonate aggregates that limit the impact strength of the polypropylene when this calcium carbonate is kneaded together.

[0005] EP 0 998 522 relates to a surface-treated calcium carbonate filler for a breathable membrane using a fatty acid with at least 10 carbon atoms, wherein the filler must be substantially free of moisture in the range of less than 0.1 wt.% before and after the treatment process.

[0006] The paper "Improved thermoplastic composites by optimized surface treatment of the mineral fillers" by DeArmitt et al. (Institute for Surface Chemistry, August 2000) describes a wet treatment method in which a batch suspension comprising mineral filler material is contacted with a dispersant at room temperature for one hour. However, this wet treatment method has the disadvantage that the wetting of the dried product used for treatment and the subsequent drying consume energy and are costly.

[0007] In EP 0 325 114, which relates to a non-sagging automotive undersealing composition based on polyvinyl chloride (with improved rheological and adhesive properties), Example 7 discloses a mixture of 12-hydroxystearic acid ammonium salt and fatty acid (in a weight ratio of 1:1) for treating mineral fillers.

[0008] WO 03 / 082966 relates to a crosslinkable and / or crosslinkable nanofiller composition, which, in optional embodiments, may additionally comprise fillers that may or may not be coated with stearic acid, stearates, silanes, siloxanes, and / or titanates. Such nanofiller compositions are used to increase barrier properties, strength, and heat distortion temperature, thereby enabling the nanofiller compositions to be used in medical, automotive, electrical, construction, and food applications.

[0009] US 2002 / 0102404 describes dispersible calcium carbonate particles coated on a surface using a combination of saturated and unsaturated aliphatic carboxylic acids and their salts, along with organic compounds such as phthalates. These dispersible calcium carbonate particles are used in adhesive compositions to improve viscosity stability and adhesive properties. Furthermore, US 2002 / 0102404 requires the implementation of mixtures of saturated and unsaturated aliphatic carboxylic acids / salts. The presence of unsaturated aliphatic carboxylic acids / salts increases the risk of undesirable in-situ side reactions with double bonds during the handling of any material comprising unsaturated aliphatic carboxylic acids / salts. Additionally, the presence of unsaturated aliphatic carboxylic acids / salts may cause discoloration or the development of undesirable odors, particularly foul odors, in the materials in which they are applied.

[0010] Claim 11 of WO 92 / 02587 indicates that a saponified sodium salt solution of at least one high molecular weight unsaturated fatty acid or a combination of at least one high molecular weight unsaturated fatty acid and at least one high molecular weight unsaturated fatty acid may be added to a preheated slurry for precipitating calcium carbonate to ultimately produce a desired level of fatty acid coating on the calcium carbonate before proceeding to further process steps.

[0011] The abstract of JP54162746 discloses a composition comprising a given relative amount of rigid vinyl chloride resin, fatty acid-treated colloidal calcium carbonate, and barium stearate for improving the thermal stability of vinyl chloride compositions.

[0012] US 4,520,073 describes a mineral filler material with an improved hydrophobic coating, prepared by pressure coating of a porous mineral using steam as a carrier for the coating material. In other options, the coating material may be selected from long-chain aliphatic fatty acids and their salts.

[0013] WO 01 / 32787 describes a particulate alkaline earth metal carbonate material product having a hydrophobic coating on its particles, the coating comprising a composition formed of: (a) a first component comprising a reaction product of an alkaline earth metal carbonate and at least one given aliphatic carboxylic acid; and (b) a second component having a carbonate release temperature substantially higher than that of the first component, the first component comprising the formula CH3(CH2). m COOR compounds.

[0014] WO 2008 / 077156 A2 relates to spun fibers comprising at least one polymer resin and at least one filler, said filler having an average particle size less than or equal to about 5 micrometers and / or an overcut less than about 15 micrometers, wherein the at least one filler is present in an amount of less than about 40% by weight relative to the total weight of the spun fibers. The filler coating is described as at least one organic material selected from fatty acids and their salts and esters (e.g., stearic acid, stearates, ammonium stearate, and calcium stearate).

[0015] GB 2 336 366 A relates to filled thermoplastic compositions, and more particularly to filled low-density polyethylene compositions formed into products or articles by extrusion. Further described, if the particulate mineral filler has a neutral to alkaline surface reaction, such as calcium carbonate, the hydrophobic agent is preferably an organic carboxylic acid having at least one saturated or unsaturated hydrocarbon chain having 8 to 28 carbon atoms, or a partially or completely neutralized salt thereof.

[0016] EP2159258A1 relates to a treated mineral filler product comprising: a) at least one mineral filler; b) a treated layer on the surface of the mineral filler, the treated layer comprising: at least one saturated C8 to C24 aliphatic carboxylic acid; and at least one divalent and / or trivalent cation salt of one or more saturated C8 to C24 aliphatic carboxylic acids; characterized in that: the weight ratio of all or more of the aliphatic carboxylic acid salts to all or more of the aliphatic carboxylic acids is 51:49 to 75:25; and the treated layer comprises at least 2.5 mg / m³ of the mineral filler. 2 The quantity exists.

[0017] EP1980588A1 relates to a method for preparing a treated mineral filler product, the method comprising the steps of: (a) treating at least one dry mineral filler with at least one Group II or Group III salt of a C8 to C24 aliphatic monocarboxylic acid to produce an intermediate mineral filler product; and then (b) treating the intermediate mineral filler product of step (a) with at least one C8 to C24 aliphatic monocarboxylic acid to produce a treated mineral filler product.

[0018] WO 2016 / 023937 A1 relates to a method for producing a breathable membrane, the method comprising the steps of: a) providing a composition comprising at least one thermoplastic polymer and a surface-treated filler material product; b) forming a membrane from the composition of step a); and c) stretching the membrane obtained in step b) to at least one orientation, wherein the surface-treated filler material product comprises: A) at least one filler material comprising milled calcium carbonate having a median weight particle size d 50 The particle size ranges from 0.1 μm to 7 μm, with a top-cut particle size <15 μm and a specific surface area (BET) of 0.5 m². 2 / g to 150m 2 / g, as measured using nitrogen and BET methods according to ISO 9277, and the residual total moisture content <1 wt.% based on the total dry weight of the at least one filler material comprising milled calcium carbonate, and B) a treatment layer on the surface of at least one filler material comprising wet-milled calcium carbonate, comprising at least one monosubstituted succinic anhydride and / or at least one monosubstituted succinic acid and / or one or more of its salt-containing reaction products, wherein the surface-treated filler material product comprises an amount of 0.1 wt.% to 3 wt.% of the treatment layer based on the total dry weight of the at least one filler material comprising milled calcium carbonate.

[0019] However, standard treatment of filler materials, including calcium carbonate, involves applying fatty acids to fine particles. This treatment requires complex and expensive methods due to the high melting point of fatty acids and the fineness of the filler material. For specific applications, such as in the polymer field, there is a trend towards coarser particles. However, the cost of standard fatty acid treatment of coarse particles is too high and not widely accepted, resulting in a scarcity of surface-treated coarse filler materials. Furthermore, in current surface treatment methods, the mechanical wear caused by the spinning / coating processes in the equipment reduces the size of the coarse feed material, leading to a significant amount of unwanted fine particles. Summary of the Invention

[0020] Therefore, an object of the present invention is to provide a method for preparing coarse, surface-treated filler material products. Furthermore, it is desirable to provide a method for preparing surface-treated filler material products that does not result in the generation of excessive fine particles. In addition, it is desirable to provide a method for preparing surface-treated filler material products that does not affect the particle size distribution of the initial filler material. Further objectives can be gleaned from the following description of the invention.

[0021] The foregoing and other objectives are achieved by means of the subject matter as defined in claim 1.

[0022] Advantageous embodiments of the method of the present invention for preparing surface-treated filler material products are defined in the corresponding dependent claims.

[0023] According to one aspect of this application, a method for preparing a surface-treated filler material product is provided. The method for preparing the surface-treated filler material product includes at least the following steps:

[0024] a) Provide at least one calcium carbonate-containing filler material, said at least one calcium carbonate-containing filler material having

[0025] i) The volume median particle size d in the range of 5 μm to 100 μm 50 value,

[0026] ii) Top cuts ranging from 30 μm to 500 μm (d 98 ),as well as

[0027] iii) Based on the total weight of the calcium carbonate-containing filler material, the residue on a 45 μm sieve greater than 0.5 wt.% as measured according to ISO 787 / 7,

[0028] b) Provide at least one surface treatment agent that is in a molten or liquid state at a temperature ranging from 18°C ​​to 45°C.

[0029] c) In one or more steps, the surface of the at least one calcium carbonate-containing filler material of step a) is brought into contact with the at least one surface treatment agent of step b) under mixing, such that a treatment layer comprising the at least one surface treatment agent and / or one or more reaction products thereof is formed on the surface of the at least one calcium carbonate-containing filler material of step a).

[0030] The obtained surface-treated filler material product, based on the total weight of the surface-treated filler material product, has a residue on a 45 μm sieve greater than 0.5 wt.% as measured according to ISO 787 / 7.

[0031] The inventors have surprisingly discovered that the above-described method for preparing surface-treated filler material products produces coarse surface-treated filler material products with a low amount of fine particles produced in the method. As a result, coarse surface-treated filler material products can be prepared that substantially retain the particle size distribution of the initial filler material, and are particularly suitable for polymer applications.

[0032] According to one embodiment, the calcium carbonate-containing filler material in step a) is selected from the group consisting of: ground calcium carbonate, preferably marble, limestone, dolomite and / or chalk, precipitated calcium carbonate (PCC), preferably aragonite, calcite and / or aragonite, surface-reacted calcium carbonate (MCC) and mixtures thereof, more preferably ground calcium carbonate.

[0033] According to another embodiment, the at least one calcium carbonate-containing filler material in step a) has a median particle size d ranging from 6 μm to 80 μm, preferably from 7 μm to 60 μm, and most preferably from 7.5 μm to 50 μm. 50 Value, b) ranging from 40 μm to 400 μm, preferably from 50 μm to 300 μm, more preferably from 50 μm to 250 μm, top cut (d) 98 (c) and (d) residues on a 45 μm sieve, in the range of 0.5 wt.% to 30 wt.%, preferably in the range of 0.75 wt.% to 25 wt.%, as measured according to ISO 787 / 7, based on the total weight of the calcium carbonate-containing filler material.

[0034] According to yet another embodiment, the amount of residue on a 45 μm sieve of the at least one calcium carbonate-containing filler material in step a) as measured according to ISO 787 / 7 differs from the amount of residue on a 45 μm sieve of the surface-treated filler material product as measured according to ISO 787 / 7 by less than 20 wt.%.

[0035] According to one embodiment, the Brookfield viscosity of the at least one surface treatment agent in step b) is ≤1000 mPa·s at 25°C.

[0036] According to another embodiment, the at least one surface treatment agent in step b) is a phosphate blend of one or more monophosphate esters and / or one or more diester phosphate esters, and / or at least one monosubstituted succinic anhydride, the at least one monosubstituted succinic anhydride being composed of succinic anhydride, the succinic anhydride being monosubstituted by a group selected from straight-chain, branched and aliphatic or cyclic groups, the total number of carbon atoms in the substituent of the straight-chain, branched and aliphatic groups being at least C2 to C20, the total number of carbon atoms in the substituent of the cyclic groups being at least C3 to C20; and / or added to contact step c) in a total amount of 0.1 wt.% to 3 wt.%, preferably 0.1 wt.% to 2 wt.%, and most preferably 0.1 wt.% to 1.5 wt.%, based on the total dry weight of the at least one calcium carbonate-containing filler material in step a).

[0037] According to yet another embodiment, contact step c) is performed in such a way that the total energy intake achieved by adding the at least one surface treatment agent of step b) to the at least one calcium carbonate-containing filler material of step a) does not exceed 15 kWh / T, preferably in the range of 2 kWh / T to 15 kWh / T.

[0038] According to one embodiment, contact step c) is performed in an Archimedes screw device such as a screw conveyor, a drum mixer, a pneumatic air conveyor system, a planetary mixer, or a Guedu mixer. Preferably, the at least one surface treatment agent of step b) is added to the at least one calcium carbonate-containing filler material of step a), and the at least one calcium carbonate-containing filler material is loaded onto the Archimedes screw device such as the screw conveyor, the drum mixer, the pneumatic air conveyor system, the planetary mixer, or the Guedu mixer.

[0039] According to another embodiment, the Archimedes spiral device operates at an angle ranging from 30° to 80°, and more preferably from 35° to 70°, and / or at a temperature ranging from 18° to 45°.

[0040] According to yet another embodiment, in the lower third of the Archimedes spiral device, the at least one surface treatment agent of step b) is added to the at least one calcium carbonate-containing filler material of step a).

[0041] According to one embodiment, the diameter to height ratio of the cylindrical mixer, the planetary mixer, or the guedu mixer is 1:1 to 1:5.

[0042] According to another embodiment, contact step c) is performed in such a manner that the at least one surface treatment agent of step b) is sprayed onto the at least one calcium carbonate-containing filler material of step a), and / or contact step c) is performed in a continuous or batch processing mode.

[0043] According to another aspect, the present invention relates to a surface-treated filler material product comprising...

[0044] a) at least one calcium carbonate-containing filler material, said at least one calcium carbonate-containing filler material having

[0045] i) The volume median particle size d in the range of 5 μm to 100 μm 50 value,

[0046] ii) Top cutting in the range of 30 μm and 500 μm (d 98 ),

[0047] b) A treatment layer on the surface of the at least one calcium carbonate-containing filler material, the treatment layer comprising at least one surface treatment agent and / or its reaction product, wherein the surface-treated filler material product comprises, based on the total dry weight of the at least one calcium carbonate-containing filler material, an amount of 0.1 wt.% to 3 wt.% of the treatment layer.

[0048] The surface-treated filler material product, by weight of the total product, has a residue on a 45 μm sieve greater than 0.5 wt.% as measured according to ISO 787 / 7.

[0049] According to one embodiment, the surface-treated filler material product is obtained by a method for preparing a surface-treated filler material product as defined herein.

[0050] According to another aspect of the invention, an article, preferably a polymer article, is provided that comprises a surface-treated filler material product as defined herein.

[0051] It should be understood that, for the purposes of this invention, the following terms have the following meanings:

[0052] For the purposes of this invention, the term "surface-treated filler material product" refers to a calcium carbonate-containing filler material that has been contacted with a surface-treated agent to obtain a coating on at least a portion of the surface of the calcium carbonate-containing filler material.

[0053] The term "surface treatment agent" refers to a reagent suitable for making calcium carbonate-containing filler materials more hydrophobic.

[0054] In the context of this invention, the term "reaction product" for a surface treatment agent refers to a product obtained by contacting a calcium carbonate-containing filler material with the surface treatment agent. The reaction product is formed between the applied surface treatment agent and reactive molecules located on the surface of the calcium carbonate-containing filler material.

[0055] In this invention, a "treatment layer" refers to a layer of treatment agent on the surface of a surface-treated filler material product, preferably a single layer. The "treatment layer" mainly consists of a surface treatment agent and / or one or more of its reaction products.

[0056] The term "mainly" in relation to the treatment layer refers to a treatment layer containing compounds that are different from the surface treatment agent and / or one or more of its reaction products, in an amount of <5 wt.%, preferably <2 wt.%, and most preferably <1 wt.%, by total weight of the treatment layer.

[0057] In the context of this invention, the "specific surface area (SSA)" of a calcium carbonate-containing filler material is defined as the surface area of ​​the calcium carbonate-containing filler material divided by its mass. As used herein, the specific surface area is measured using a BET isotherm (ISO 9277:2010) via nitrogen adsorption and expressed in m³. 2 / g specifies.

[0058] The "particle size" of particulate materials, such as the calcium carbonate-containing filler material discussed in this paper, is defined by its particle size d. x The distribution is used to describe it.

[0059] value d x Indicates the diameter; relative to said diameter, x% of the particles have a diameter less than d. x This means d 98 The value is that 98% of all particles are smaller than its particle size. d 98 The value is also known as "top tangent". d x The value is given as a volume percentage. Therefore, d 50 The value is the volumetric median particle size, which is the total particle size of 50 vol.% of all particles smaller than this value. The volumetric median particle size d was evaluated using a Malvern Mastersizer 2000 laser diffraction system. 50 d was measured using a Malvern Mastersizer 2000 laser diffraction system. 50 or d 98The value indicates the diameter such that 50% or 98% of the particles by volume have a diameter smaller than this value. The raw data obtained through measurements were analyzed using Mietheory, with the particle refractive index at 1.57 and the absorptivity at 0.005.

[0060] In the context of this invention, the term "melt" is defined as a material in a state that transitions from a solid to a liquid state, i.e., a state that is not completely liquid at temperatures ranging from 18°C ​​to 45°C.

[0061] According to the present invention, the term "liquid" refers to a material that is completely liquid at temperatures ranging from 18°C ​​to 45°C.

[0062] When the term "comprising" is used in this specification and claims, it does not exclude other unspecified elements of primary or secondary functional importance. For the purposes of this invention, the term "consisting of" is considered a preferred embodiment of the term "comprising." If a set is defined below as comprising at least a certain number of embodiments, this should also be understood as disclosing a set that preferably consists only of those embodiments.

[0063] Whenever the terms “include” or “have” are used, they are meant to be equivalent to “include” as defined above.

[0064] When referring to a singular noun, the use of an indefinite or definite article (e.g., "a / an" or "the") includes the plural form of the noun unless otherwise specified.

[0065] As described above, the method of the present invention for preparing surface-treated filler material products includes at least method steps a), b), and c). Hereinafter, reference is made to further details of the invention, and in particular to the foregoing steps of the method of the present invention for preparing surface-treated filler material products.

[0066] Characterization of step a): Provide at least one calcium carbonate-containing filler material.

[0067] According to step a) of the method of the present invention, at least one calcium carbonate-containing filler material is provided.

[0068] The phrase "at least one" calcium carbonate-containing filler material means that one or more, such as two or three, calcium carbonate-containing filler materials can be provided. According to a preferred embodiment, only one calcium carbonate-containing filler material is provided in step a).

[0069] According to a preferred embodiment of the invention, the material comprising calcium carbonate is selected from the group consisting of: ground calcium carbonate (GCC), preferably marble, limestone, dolomite and / or chalk; precipitated calcium carbonate (PCC), preferably aragonite, calcite and / or aragonite; surface-reacted calcium carbonate (MCC) and mixtures thereof.

[0070] For example, the at least one material comprising calcium carbonate is ground calcium carbonate.

[0071] GCC is understood to be calcium carbonate in its natural form, extracted from sedimentary rocks such as limestone or chalk, or from metamorphic marble rocks, and processed in wet and / or dry forms by methods such as grinding, screening, and / or grading, using processes such as cyclone separators or classifiers. In one embodiment of the invention, GCC is selected from the group consisting of marble, chalk, dolomite, limestone, and mixtures thereof.

[0072] In contrast, PCC-type calcium carbonate comprises synthetic calcium carbonate products obtained by carbonation of calcium hydroxide slurry or by precipitation from ionic salt solutions. When derived from finely divided calcium oxide particles in water, the calcium hydroxide slurry is commonly referred to in the art as lime slurry or lime milk. PCC can be rhombohedral and / or subtriangular and / or aragonite; preferably synthetic or precipitated calcium carbonate, comprising aragonite, aragonite, or calcite mineralogical crystal forms or mixtures thereof.

[0073] In the context of this invention, "surface-reacted calcium carbonate" can be characterized as naturally ground or precipitated calcium carbonate having internal structural modification or surface-reacted products.

[0074] In a preferred embodiment, the at least one calcium carbonate-containing filler material is marble.

[0075] It should be understood that, based on the total dry weight of the at least one calcium carbonate-containing filler material, the amount of calcium carbonate in the at least one calcium carbonate-containing filler material is preferably at least 80 wt.%, for example at least 95 wt.%, more preferably between 97 wt.% and 100 wt.%, and even more preferably between 98.5 wt.% and 99.95 wt.%.

[0076] The term "dry" calcium carbonate-containing packing material should be understood as packing material containing less than 0.3% by weight of water relative to the weight of the packing material. The percentage of water (equal to the residual total moisture content) is determined according to the Coulometric Karl Fischer method, in which the water content of the packing material is determined in Coulometric units by heating the packing material to 220°C and releasing it as vapor and separating it using a nitrogen flow (100 mL / min).

[0077] A specific requirement of this invention is that the at least one calcium carbonate-containing filler material is a coarse material. That is, the volume median particle size d of the at least one calcium carbonate-containing filler material is... 50 The value ranges from 5 μm to 100 μm. For example, the volume median particle size d of the at least one calcium carbonate-containing filler material. 50 The range is 6 μm to 80 μm, preferably 7 μm to 60 μm and most preferably 7.5 μm to 50 μm.

[0078] In addition, the top cut (d) of the at least one calcium carbonate-containing filler material 98 The range of ) is from 30 μm to 500 μm. For example, the top cut (d) of the at least one calcium carbonate-containing filler material. 98 The range of ) is 40 μm and 400 μm, preferably 50 μm to 300 μm, and more preferably 50 μm to 250 μm.

[0079] The coarse material is a material with a low content of fine particles. Specifically, the coarse at least one calcium carbonate-containing filler material is characterized by a residue on a 45 μm sieve greater than 0.5 wt.% based on the total weight of the calcium carbonate-containing filler material, as measured according to ISO 787 / 7. Preferably, the at least one calcium carbonate-containing filler material has a residue on a 45 μm sieve ranging from 0.5 wt.% to 30 wt.% based on the total weight of the calcium carbonate-containing filler material, as measured according to ISO 787 / 7, and more preferably from 0.75 wt.% to 25 wt.%. For example, the at least one calcium carbonate-containing filler material has a residue on a 45 μm sieve ranging from 0.75 wt.% to 15 wt.% based on the total weight of the calcium carbonate-containing filler material, as measured according to ISO 787 / 7, or from 0.75 wt.% to 10 wt.%.

[0080] Therefore, the at least one calcium carbonate-containing filler material has

[0081] i) A volume median particle size d ranging from 5 μm to 100 μm, preferably from 6 μm to 80 μm, more preferably from 7 μm to 60 μm, and most preferably from 7.5 μm to 50 μm. 50 Value, and

[0082] ii) Top cut (d) ranging from 30 μm to 500 μm, preferably 40 μm and 400 μm, more preferably 50 μm to 300 μm, and most preferably 50 μm to 250 μm. 98 ),as well as

[0083] iii) Based on the total weight of the calcium carbonate-containing filler material, greater than 0.5 wt.%, preferably from 0.5 wt.% to 30 wt.%, and more preferably from 0.75 wt.% to 25 wt.% of the residue on a 45 μm sieve as measured according to ISO 787 / 7.

[0084] In view of the above, it should be understood that the at least one calcium carbonate-containing filler material is preferably in the form of a particulate material.

[0085] More preferably, the BET specific surface area of ​​the at least one calcium carbonate-containing filler material is 0.5 m². 2 / g to 150m 2 / g, as measured by the BET nitrogen method. For example, the specific surface area (BET) of the at least one calcium carbonate-containing filler material is 0.5 m². 2 / g to 50m 2 / g, more preferably 0.5m 2 / g to 35m 2 / g and most preferably 0.5m 2 / g to 10m 2 / g, as measured by the BET nitrogen method.

[0086] Preferably, the at least one calcium carbonate-containing filler material is a dry-milled material, a wet-milled and dried material, or a mixture of the foregoing. Typically, the grinding step can be performed using any conventional grinding apparatus, for example, under conditions where refinement is primarily achieved through impact with the secondary mass, i.e., performed using one or more of the following: ball mill, rod mill, vibratory mill, crusher, centrifugal impact mill, vertical bead mill, grinder, pin mill, hammer mill, pulverizer, paper shredder, de-lumping machine, cutter, or other such equipment known to those skilled in the art.

[0087] In the case where the at least one calcium carbonate-containing filler material is a wet-milled calcium carbonate-containing filler material, the milling step can be performed under conditions that allow autogenous milling to occur and / or by horizontal ball milling and / or other such methods known to those skilled in the art. The wet-treated calcium carbonate-containing filler material thus obtained can be washed and dehydrated by well-known methods such as flocculation, filtration, or forced evaporation prior to drying. Subsequent drying steps can be performed in a single step (such as spray drying) or in at least two steps, for example by applying a first heating step to the calcium carbonate-containing filler material to reduce the relevant moisture content to a level not exceeding about 0.5 wt.% based on the total dry weight of the at least one calcium carbonate-containing filler material. The residual total moisture content of the filler can be measured by Karl Fischer electrostatic titration, in which moisture is desorbed in an oven at 195°C and continuously injected with dry N2 at 100 mL / min into a KF coulometric titrator (Mettler Toledo KF coulometric titrator C30, combined with a Mettler oven DO 0337) for 10 minutes. The residual total moisture content can be determined by a calibration curve, and a 10-minute gas flow blind point without a sample can also be considered. The residual total moisture content can be further reduced by applying a second heating step to the at least one calcium carbonate-containing filler material. When the drying is performed by more than one drying step, the first step can be performed by heating in a hot gas flow, while the second and additional drying steps are preferably performed by indirect heating, wherein the atmosphere in the corresponding vessel includes a surface treatment agent. Also typically, the at least one calcium carbonate-containing filler material undergoes a beneficiation step (such as flotation, bleaching, or magnetic separation) to remove impurities.

[0088] In one embodiment of the invention, the at least one calcium carbonate-containing filler material comprises a filler material containing dry-milled calcium carbonate. In another preferred embodiment, the at least one calcium carbonate-containing filler material is a material that has been wet-milled in a horizontal ball mill and subsequently dried using a well-known spray drying method.

[0089] According to the at least one calcium carbonate-containing filler material, based on the total dry weight of the at least one calcium carbonate-containing filler material, the at least one calcium carbonate-containing filler material preferably has a residual total moisture content of 0.01 wt.% to 1 wt.%, preferably 0.01 wt.% to 0.2 wt.%, more preferably 0.02 wt.% to 0.2 wt.%, and most preferably 0.04 wt.% to 0.2 wt.%.

[0090] For example, when wet-milled and spray-dried marble is used as the at least one calcium carbonate-containing filler material, the residual total moisture content of the at least one calcium carbonate-containing filler material is preferably 0.01 wt.% to 0.1 wt.%, more preferably 0.02 wt.% to 0.08 wt.%, and most preferably 0.04 wt.% to 0.07 wt.%, based on the total dry weight of the at least one calcium carbonate-containing filler material. If PCC is used as the at least one calcium carbonate-containing filler material, the residual total moisture content of the at least one calcium carbonate-containing filler material is preferably 0.01 wt.% to 0.2 wt.%, more preferably 0.05 wt.% to 0.17 wt.%, and most preferably 0.05 wt.% to 0.15 wt.%, based on the total dry weight of the at least one calcium carbonate-containing filler material.

[0091] Characterization of step b): providing at least one surface treatment agent

[0092] According to step b) of the method of the present invention, at least one surface treatment agent is provided that is in a molten or liquid state at a temperature ranging from 18°C ​​to 45°C.

[0093] It should be understood that the expression "at least one" surface treatment agent means that one or more surface treatment agents can be provided in the method of the present invention.

[0094] Therefore, it should be noted that the at least one surface treatment agent can be a single surface treatment agent. Alternatively, the at least one surface treatment agent can be a mixture of two or more surface treatment agents. For example, the at least one surface treatment agent can be a mixture of two or three surface treatment agents, such as two surface treatment agents.

[0095] In one embodiment of the present invention, the at least one surface treatment agent is a surface treatment agent.

[0096] To avoid reducing particle size during the method, it should be understood that the at least one surface treatment agent must be in a molten or liquid state at a temperature ranging from 18°C ​​to 45°C. That is, the at least one calcium carbonate-containing filler material is treated with at least one surface treatment agent in a molten or liquid state.

[0097] When measured using appropriate equipment, such as the Physica MCR 300 rheometer (Paar Physica) equipped with the TEZ 150P-C measurement unit and CC 28.7 measurement system, the measurement time is 5 seconds. -1At a shear rate of 0.5°C and at +25°C (±2°C), the at least one surface treatment agent is preferably characterized by a viscosity of ≤1000, preferably ≤900 mPa·s, more preferably ≤700 mPa·s, and most preferably ≤500 mPa·s at +25°C (±2°C).

[0098] It should be noted that the at least one surface treatment agent can also be provided in an organic solvent to achieve the viscosity mentioned above. However, the organic solvent should be characterized by the lowest possible boiling point to avoid the energy-intensive drying step required to remove the organic solvent. For the same reason, the at least one surface treatment agent should be dissolved in the lowest possible amount of organic solvent. The amount of organic solvent is preferably less than 50 wt.%, more preferably less than 30 wt.%, and most preferably less than 10 wt.%, based on the total weight of the mixture comprising the at least one surface treatment agent and the organic solvent. The organic solvent can be selected from the group consisting of solvents comprising ester and / or ether functional groups, aromatic solvents, mineral oils and mixtures thereof. Examples of organic solvents include diethyl ether, petroleum ether, ethyl acetate, toluene, xylene and mixtures thereof.

[0099] However, the at least one surface treatment agent is preferably provided in undiluted form, i.e., without organic solvents.

[0100] It should be understood that the at least one surface treatment agent can be any surface treatment agent known to those skilled in the art capable of forming a hydrophobic treatment layer on at least a portion of the accessible surface area of ​​the at least one calcium carbonate-containing filler material particles.

[0101] In one embodiment of the invention, the at least one surface treatment agent in step b) is a phosphate blend of one or more monophosphate esters and / or one or more diester phosphate esters, and / or at least one monosubstituted succinic anhydride, wherein the at least one monosubstituted succinic anhydride is composed of succinic anhydride, wherein the succinic anhydride is monosubstituted by a group selected from straight-chain, branched, and aliphatic or cyclic groups, wherein the total number of carbon atoms in the substituent of the straight-chain, branched, and aliphatic groups is at least C2 to C20, and the total number of carbon atoms in the substituent of the cyclic groups is at least C3 to C20.

[0102] Preferably, the at least one surface treatment agent in step b) is a phosphate blend of one or more monophosphate esters and / or one or more diester phosphate esters, or at least one monosubstituted succinic anhydride, wherein the at least one monosubstituted succinic anhydride is composed of succinic anhydride, wherein the succinic anhydride is monosubstituted by a group selected from straight-chain, branched, and aliphatic or cyclic groups, wherein the total number of carbon atoms in the substituent of the straight-chain, branched, and aliphatic groups is at least C2 to C20, and the total number of carbon atoms in the substituent of the cyclic groups is at least C3 to C20.

[0103] In one embodiment, the at least one surface treatment agent in step b) is a phosphate blend of one or more monophosphate esters and / or one or more diester phosphate esters.

[0104] In the context of this invention, the term "phosphate monoester" refers to a phosphoric acid molecule monoesterified with an alcohol molecule selected from the following: unsaturated or saturated, branched or straight-chain, aliphatic or aromatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21, preferably C8 to C20, more preferably C8 to C18 and most preferably C8 to C16.

[0105] In the context of this invention, the term "phosphate diester" refers to a phosphoric acid molecule diesterized from two alcohol molecules selected from the following: identical or different, unsaturated or saturated, branched or straight-chain, aliphatic or aromatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21, preferably C8 to C20, more preferably C8 to C18 and most preferably C8 to C16.

[0106] 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 München, 1993).

[0107] Synthesizing alkyl esters of phosphoric acid by various methods and surface treatment of minerals with alkyl esters of phosphoric acid are well known to those skilled in the art, for example from Pesticide Formulations and Application Systems: Volume 15; Collins HM, Hall FR, Hopkinson M, STP1268; Publications: 1996, US 3,897,519A, US 4,921,990 A, US 4,350,645 A, US 6,710,199 B2, US 4,126,650A, US 5,554,781 A, EP1092000B1 and WO 2008 / 023076 A1.

[0108] It should be understood that the expression "one or more" monophosphates means that one or more monophosphates may be present in the phosphate blend.

[0109] Therefore, it should be noted that the one or more monophosphate esters can be a single monophosphate ester. Alternatively, the one or more monophosphate esters can be a mixture of two or more monophosphate esters. For example, the one or more monophosphate esters can be a mixture of two or three monophosphate esters, such as two monophosphate esters.

[0110] In one embodiment of the invention, the one or more phosphate monoesters are composed of orthophosphate molecules esterified with an alcohol selected from: unsaturated or saturated, straight-chain or branched, aliphatic or aromatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21. For example, the one or more phosphate monoesters are composed of orthophosphate molecules esterified with an alcohol selected from: unsaturated or saturated, branched or straight-chain, aliphatic or aromatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C8 to C20, more preferably C8 to C18, and most preferably C8 to C16.

[0111] In one embodiment of the invention, the one or more phosphate monoesters are composed of orthophosphate molecules esterified with an alcohol selected from: saturated and straight-chain or branched and aliphatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21. For example, the one or more phosphate monoesters are composed of orthophosphate molecules esterified with an alcohol selected from: saturated and straight-chain or branched and aliphatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C8 to C20, more preferably C8 to C18, and most preferably C8 to C16.

[0112] In one embodiment of the invention, the one or more phosphate monoesters are composed of orthophosphate molecules esterified with an alcohol selected from saturated, straight-chain, and aliphatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21, preferably C8 to C20, more preferably C8 to C18, and most preferably C8 to C16. Alternatively, the one or more phosphate monoesters are composed of orthophosphate molecules esterified with an alcohol selected from saturated, branched, and aliphatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21, preferably C8 to C20, more preferably C8 to C18, and most preferably C8 to C16.

[0113] In one embodiment of the invention, the one or more monophosphate esters are selected from the group consisting of: hexyl phosphate monoester, heptyl phosphate monoester, octyl phosphate monoester, 2-ethylhexyl phosphate monoester, nonyl phosphate monoester, decyl phosphate monoester, undecyl phosphate monoester, dodecyl phosphate monoester, tetradecyl phosphate monoester, hexadecyl phosphate monoester, and mixtures thereof.

[0114] For example, the one or more phosphate monoesters are selected from the group consisting of 2-ethylhexyl phosphate monoester, hexadecyl phosphate monoester, heptylnonyl phosphate monoester, and mixtures thereof.

[0115] It should be understood that the expression "one or more" phosphate diesters means that one or more phosphate diesters may be present in the phosphate ester blend.

[0116] Therefore, it should be noted that the one or more phosphate diesters can be a single phosphate diester. Alternatively, the one or more phosphate diesters can be a mixture of two or more phosphate diesters. For example, the one or more phosphate diesters can be a mixture of two or three phosphate diesters, such as two phosphate diesters.

[0117] In one embodiment of the invention, the one or more phosphate diesters are composed of orthophosphate molecules esterified with two alcohols selected from the group consisting of unsaturated or saturated, straight-chain or branched, aliphatic or aromatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21. For example, the one or more phosphate diesters are composed of orthophosphate molecules esterified with two fatty alcohols selected from the group consisting of unsaturated or saturated, branched or straight-chain, aliphatic or aromatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C8 to C20, more preferably C8 to C18, and most preferably C8 to C16.

[0118] It should be understood that the two alcohols used for esterifying phosphoric acid can be independently selected from the same or different, unsaturated or saturated, branched or straight-chain, aliphatic or aromatic alcohols, with a total carbon atom count of C6 to C21 in the alcohol substituents. In other words, the one or more phosphate diesters may include two substituents derived from the same alcohol, or the phosphate diester molecule may include two substituents derived from different alcohols.

[0119] In one embodiment of the invention, the one or more phosphate diesters are composed of orthophosphate molecules esterified with two alcohols selected from the group consisting of identical or different, saturated, straight-chain or branched, and aliphatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21. For example, the one or more phosphate diesters are composed of orthophosphate molecules esterified with two alcohols selected from the group consisting of identical or different, saturated, straight-chain or branched, and aliphatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C8 to C20, more preferably C8 to C18, and most preferably C8 to C16.

[0120] In one embodiment of the invention, the one or more phosphate diesters are composed of orthophosphate molecules esterified with two alcohols selected from the group consisting of identical or different, saturated, and straight-chain and aliphatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21, preferably C8 to C20, more preferably C8 to C18, and most preferably C8 to C16. Alternatively, the one or more phosphate diesters are composed of orthophosphate molecules esterified with two alcohols selected from the group consisting of identical or different, saturated, and branched and aliphatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21, preferably C8 to C20, more preferably C8 to C18, and most preferably C8 to C16.

[0121] In one embodiment of the invention, the one or more phosphate diesters are selected from the group consisting of: hexyl phosphate diester, heptyl phosphate diester, octyl phosphate diester, 2-ethylhexyl phosphate diester, nonyl phosphate diester, decyl phosphate diester, undecyl phosphate diester, dodecyl phosphate diester, tetradecyl phosphate diester, hexadecyl phosphate diester, and mixtures thereof.

[0122] For example, the one or more phosphate diesters are selected from the group consisting of 2-ethylhexyl phosphate diester, hexadecyl phosphate diester, and mixtures thereof. In one embodiment of the invention, the one or more phosphate diesters are 2-octyl-1-dodecyl phosphate diester.

[0123] In one embodiment of the invention, the one or more monophosphates are selected from the group consisting of 2-ethylhexyl phosphate, hexadecyl phosphate and mixtures thereof, and the one or more diphosphates are selected from the group consisting of 2-ethylhexyl phosphate, hexadecyl phosphate and mixtures thereof.

[0124] For example, a phosphate blend comprises a monophosphate ester and a diester phosphate ester. In this case, the monophosphate ester is selected from the group consisting of 2-ethylhexyl phosphate monoester and hexadecyl phosphate monoester, and the diester phosphate ester is selected from the group consisting of 2-ethylhexyl phosphate diester and hexadecyl phosphate diester.

[0125] If the phosphate blend comprises a monophosphate and a diester, it should be understood that the alcohol substituents of the monophosphate and the diester are preferably identical. For example, the phosphate blend comprises 2-ethylhexyl phosphate monoester and 2-ethylhexyl phosphate diester. Alternatively, the phosphate blend comprises hexadecyl phosphate monoester and hexadecyl phosphate diester.

[0126] In one embodiment of the invention, the phosphate blend comprises two or more monophosphates and two or more diesters. In this case, the two or more monophosphates are selected from the group consisting of 2-ethylhexyl phosphate and hexadecyl phosphate, and the two or more diesters are selected from the group consisting of 2-ethylhexyl phosphate and hexadecyl phosphate.

[0127] According to one embodiment of the present invention, the phosphate blend comprises one or more monophosphates and one or more diesters in a specific molar ratio. Specifically, the molar ratio of the one or more monophosphates to the one or more diesters in the phosphate blend can be from 1:1 to 1:100.

[0128] In this invention, the term "molar ratio of the one or more monophosphates to the one or more diesters" refers to the ratio of the sum of the molecular weights of monophosphate molecules to the sum of the molecular weights of diester molecules.

[0129] According to one embodiment, the molar ratio of the one or more monophosphates to the one or more diesters in the phosphate blend is 1:1 to 1:100, preferably 1:1.1 to 1:80, more preferably 1:1.1 to 1:60, even more preferably 1:1.1 to 1:40, still even more preferably 1:1.1 to 1:20, and most preferably 1:1.1 to 1:10.

[0130] According to one embodiment of the present invention,

[0131] I) The one or more phosphate monoesters are composed of orthophosphate molecules, which are monoesterified with an alcohol molecule selected from: unsaturated or saturated, branched or straight-chain, aliphatic or aromatic alcohols, wherein the total number of carbon atoms in the alcohol substituent is C6 to C21, preferably C8 to C20, more preferably C8 to C18 and most preferably C8 to C16, and / or

[0132] II) The one or more phosphate diesters are composed of orthophosphate molecules, which are diesterized with two alcohol molecules selected from the following: the same or different, unsaturated or saturated, branched or straight, aliphatic or aromatic fatty alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21, preferably C8 to C20, more preferably C8 to C18 and most preferably C8 to C16.

[0133] In one embodiment of the invention, the phosphate blend further comprises one or more triphosphates and / or phosphoric acid.

[0134] In the context of this invention, the term "triphosphate" refers to a phosphoric acid molecule triesterified with three alcohol molecules selected from the following: identical or different, unsaturated or saturated, branched or straight-chain, aliphatic or aromatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21, preferably C8 to C20, more preferably C8 to C18 and most preferably C8 to C16.

[0135] It should be understood that the expression "one or more" triphosphates means that one or more triphosphates may be present in the phosphate blend.

[0136] Therefore, it should be noted that the one or more triphosphates can be a single triphosphate. Alternatively, the one or more triphosphates can be a mixture of two or more triphosphates. For example, the one or more triphosphates can be a mixture of two or three triphosphates, such as two triphosphates.

[0137] In one embodiment of the invention, the one or more triphosphate esters are composed of orthophosphate molecules esterified with three alcohols selected from the group consisting of identical or different, unsaturated or saturated, straight-chain or branched, aliphatic or aromatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21. For example, the one or more triphosphate esters are composed of orthophosphate molecules esterified with three alcohols selected from the group consisting of identical or different, unsaturated or saturated, branched or straight-chain, aliphatic or aromatic fatty alcohols, wherein the total number of carbon atoms in the alcohol substituents is C8 to C20, more preferably C8 to C18, and most preferably C8 to C16.

[0138] It should be understood that the three alcohols used for esterifying phosphoric acid can be independently selected from unsaturated or saturated, branched or straight-chain, aliphatic or aromatic alcohols, with a total carbon atom count of C6 to C21 in the alcohol substituents. In other words, the one or more phosphate triester molecules may include three substituents derived from the same alcohol, or the phosphate triester molecule may include three substituents derived from different alcohols.

[0139] In one embodiment of the invention, the one or more triphosphate esters are composed of orthophosphate molecules esterified with three alcohols selected from the group consisting of identical or different, saturated, and straight-chain or branched and aliphatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21. For example, the one or more triphosphate esters are composed of orthophosphate molecules esterified with three alcohols selected from the group consisting of identical or different, saturated, and straight-chain or branched and aliphatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C8 to C20, more preferably C8 to C18, and most preferably C8 to C16.

[0140] In one embodiment of the invention, the one or more triphosphates are composed of orthophosphate molecules esterified with three alcohols selected from: saturated, straight-chain, and aliphatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21, preferably C8 to C20, more preferably C8 to C18, and most preferably C8 to C16. Alternatively, the one or more triphosphates are composed of orthophosphate molecules esterified with three alcohols selected from: saturated, branched, and aliphatic alcohols, wherein the total number of carbon atoms in the alcohol substituents is C6 to C21, preferably C8 to C20, more preferably C8 to C18, and most preferably C8 to C16.

[0141] In one embodiment of the invention, the one or more triphosphates are selected from the group consisting of: hexyl phosphate, heptyl phosphate, octyl phosphate, 2-ethylhexyl phosphate, nonyl phosphate, decyl phosphate, undecyl phosphate, dodecyl phosphate, tetradecyl phosphate, hexadecyl phosphate, and mixtures thereof.

[0142] For example, the one or more phosphate triesters are selected from the group consisting of 2-ethylhexyl phosphate triester and hexadecyl phosphate triester and mixtures thereof.

[0143] In one embodiment of the invention, the phosphate blend comprises one or more monophosphates, one or more diesters, and one or more triphosphates, and optionally phosphoric acid. For example, the phosphate blend comprises one or more monophosphates, one or more diesters, and one or more triphosphates, and phosphoric acid.

[0144] Alternatively, phosphate blends may include one or more monophosphates and one or more diesters and optionally phosphoric acid. For example, phosphate blends may include one or more monophosphates and one or more diesters and phosphoric acid.

[0145] If the phosphate blend comprises one or more triphosphates, it is preferred that the phosphate blend comprises ≤10 mol.% of the one or more triphosphates, based on the total molar amount of the one or more monophosphates, the one or more diphosphates, and the one or more triphosphates with phosphoric acid. For example, the phosphate blend comprises ≤8 mol.%, preferably ≤6 mol.%, and more preferably ≤4 mol.%, such as from 0.1 mol.% to 4 mol.% of the one or more triphosphates, based on the total molar amount of the one or more monophosphates, the one or more diphosphates, and the one or more triphosphates with phosphoric acid.

[0146] Alternatively or concurrently, if the phosphate blend includes phosphoric acid, it is preferred that the phosphate blend comprises ≤10 mol.% of phosphoric acid, based on the total molar amount of the one or more monophosphates, one or more diphosphates, and one or more triphosphates with phosphoric acid. For example, the phosphate blend comprises ≤8 mol.%, preferably ≤6 mol.%, and more preferably ≤4 mol.%, such as 0.1 mol.% to 4 mol.% of phosphoric acid, based on the total molar amount of the one or more monophosphates, one or more diphosphates, and one or more triphosphates with phosphoric acid.

[0147] If the phosphate blend further comprises phosphoric acid and one or more triphosphates, it is preferred that, based on the total molar ratio of said one or more monophosphates to said one or more diphosphates and said one or more triphosphates to phosphoric acid, the molar ratio of phosphoric acid to said one or more monophosphates to said one or more diphosphates to said one or more triphosphates in the phosphate blend is ≤10 mol.-% : ≤40 mol.-% : ≥40 mol.% : ≤10 mol.-%.

[0148] In the context of this invention, the term "molar ratio of phosphoric acid to one or more monophosphates to one or more diesters to one or more triphosphates" refers to the sum of the molecular weights of the phosphoric acid molecules divided by the sum of the molecular weights of the monophosphate molecules divided by the sum of the molecular weights of the diester molecules divided by the sum of the molecular weights of the triphosphate molecules.

[0149] For example, EP 2 770 017 A1 describes a method for preparing a surface-treated filler material product treated with at least one phosphate ester blend and a suitable compound for coating, which is therefore incorporated herein by reference.

[0150] Alternatively or alternatively, the at least one surface treatment agent in step b) is at least one monosubstituted succinic anhydride, which is composed of succinic anhydride and is monosubstituted by a group selected from straight-chain, branched, aliphatic and cyclic groups, wherein the total number of carbon atoms in the substituent is at least C2 to C20.

[0151] In one embodiment, at least one surface-treating agent of step b) is preferably provided in an organic solvent, and is at least one monosubstituted succinic anhydride. Alternatively, at least one surface-treating agent of step b) is provided in water as a solvent.

[0152] It should be understood that the at least one monosubstituted succinic anhydride represents a surface treatment agent and is composed of succinic anhydride, wherein the succinic anhydride is monosubstituted by a group selected from any straight-chain, branched, aliphatic, and cyclic group, and the total number of carbon atoms in the substituent is C2 to C20.

[0153] In one embodiment of the invention, the at least one monosubstituted succinic anhydride is composed of succinic anhydride, wherein the succinic anhydride is monosubstituted by a group selected from straight-chain, branched, aliphatic, and cyclic groups, and the total number of carbon atoms in the substituent is C3 to C20. For example, the at least one monosubstituted succinic anhydride is composed of succinic anhydride, wherein the succinic anhydride is monosubstituted by a group selected from straight-chain, branched, aliphatic, and cyclic groups, and the total number of carbon atoms in the substituent is C4 to C20.

[0154] In one embodiment of the invention, the at least one monosubstituted succinic anhydride is composed of succinic anhydride, wherein the succinic anhydride is monosubstituted as one of the linear and aliphatic groups, and the total number of carbon atoms in the substituent is C2 to C20, preferably C3 to C20, and most preferably C4 to C20. Alternatively or alternatively, the at least one monosubstituted succinic anhydride is composed of succinic anhydride, wherein the succinic anhydride is monosubstituted as one of the branched and aliphatic groups, and the total number of carbon atoms in the substituent is C2 to C20, preferably C3 to C20, and most preferably C4 to C20.

[0155] Therefore, preferably, the at least one monosubstituted succinic anhydride is composed of succinic anhydride, wherein the succinic anhydride is monosubstituted as a group of a straight-chain or branched alkyl group, and the total number of carbon atoms in the substituent is C2 to C20, preferably C3 to C20 and most preferably C4 to C20.

[0156] For example, the at least one monosubstituted succinic anhydride is composed of succinic anhydride, wherein the succinic anhydride is monosubstituted as a group of a straight-chain alkyl group, and the total number of carbon atoms in the substituent is C2 to C20, preferably C3 to C20, and most preferably C4 to C20. Alternatively or alternatively, the at least one monosubstituted succinic anhydride is composed of succinic anhydride, wherein the succinic anhydride is monosubstituted as a group of a branched alkyl group, and the total number of carbon atoms in the substituent is C2 to C20, preferably C3 to C20, and most preferably C4 to C20.

[0157] In the context of this invention, the term "alkyl" refers to a straight-chain or branched, saturated organic compound composed of carbon and hydrogen. In other words, "alkyl monosubstituted succinic anhydride" consists of a straight-chain or branched, saturated hydrocarbon chain containing a side-chain succinic anhydride group.

[0158] In one embodiment of the invention, the at least one monosubstituted succinic anhydride is at least one linear or branched alkyl monosubstituted succinic anhydride. For example, the at least one alkyl monosubstituted succinic anhydride is selected from the group consisting of: ethyl succinic anhydride, propyl succinic anhydride, butyl succinic anhydride, triisobutyl succinic anhydride, pentyl succinic anhydride, hexyl succinic anhydride, heptyl succinic anhydride, octyl succinic anhydride, nonyl succinic anhydride, decyl succinic anhydride, dodecyl succinic anhydride, hexadecyl succinic anhydride, octadecyl succinic anhydride, and mixtures thereof.

[0159] Therefore, it should be understood that, for example, the term "butyl succinic anhydride" includes one or more linear and branched butyl succinic anhydrides. A specific example of one or more linear butyl succinic anhydrides is n-butyl succinic anhydride. Specific examples of one or more branched butyl succinic anhydrides are isobutyl succinic anhydride, sec-butyl succinic anhydride, and / or tert-butyl succinic anhydride.

[0160] Furthermore, it should be understood that, for example, the term "hexadecyl succinic anhydride" includes one or more straight-chain and branched hexadecyl succinic anhydrides. A specific example of one or more straight-chain hexadecyl succinic anhydrides is n-hexadecyl succinic anhydride. Specific examples of one or more branched hexadecyl succinic anhydrides are 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, 5-methylpentadecanyl succinic anhydride, 4-methylpentadecanyl succinic anhydride, 3-methylpentadecanyl succinic anhydride, 2-methylpentadecanyl succinic anhydride, 1-methylpentadecanyl succinic anhydride, 13-ethyltetradecyl succinic anhydride, 12-ethyltetradecyl succinic anhydride, 11-ethyltetradecyl succinic anhydride, 10-ethyltetradecyl succinic anhydride, 9-ethyltetradecyl succinic anhydride, 8- Ethyltetradecyl succinic anhydride, 7-ethyltetradecyl succinic anhydride, 6-ethyltetradecyl succinic anhydride, 5-ethyltetradecyl succinic anhydride, 4-ethyltetradecyl succinic anhydride, 3-ethyltetradecyl succinic anhydride, 2-ethyltetradecyl succinic anhydride, 1-ethyltetradecyl succinic anhydride, 2-butyldodecyl succinic anhydride, 1-hexyldecyl succinic anhydride, 1-hexyl-2-decyl succinic anhydride, 2-hexyldecyl succinic anhydride, 6,12-dimethyltetradecyl succinic anhydride, 2,2-diethyldodecyl succinic anhydride, 4,8,12-trimethyltetrazyl succinic anhydride, 2,2,4,6,8-pentamethylundecyl succinic anhydride, 2-ethyl-4-methyl-2-(2-methylpentyl)-heptyl succinic anhydride and / or 2-ethyl-4,6-dimethyl-2-propylnonyl succinic anhydride.

[0161] Furthermore, it should be understood that, for example, the term "octadecyl succinic anhydride" includes one or more straight-chain and branched octadecyl succinic anhydrides. A specific example of one or more straight-chain octadecyl succinic anhydrides is n-octadecyl succinic anhydride. Specific examples of one or more branched hexadecyl succinic anhydrides are 16-methylheptadecyl succinic anhydride, 15-methylheptadecyl succinic anhydride, 14-methylheptadecyl succinic anhydride, 13-methylheptadecyl succinic anhydride, 12-methylheptadecyl succinic anhydride, 11-methylheptadecyl succinic anhydride, 10-methylheptadecyl succinic anhydride, 9-methylheptadecyl succinic anhydride, 8-methylheptadecyl succinic anhydride, 7-methylheptadecyl succinic anhydride, 6-methylheptadecyl succinic anhydride, 5-methylheptadecyl succinic anhydride, 4-methylheptadecyl succinic anhydride, 3-methylheptadecyl succinic anhydride, 2-methylheptadecyl succinic anhydride, 1-methylheptadecyl succinic anhydride, 1 4-Ethylhexadecylsuccinic anhydride, 13-Ethylhexadecylsuccinic anhydride, 12-Ethylhexadecylsuccinic anhydride, 11-Ethylhexadecylsuccinic anhydride, 10-Ethylhexadecylsuccinic anhydride, 9-Ethylhexadecylsuccinic anhydride, 8-Ethylhexadecylsuccinic anhydride, 7-Ethylhexadecylsuccinic anhydride, 6-Ethylhexadecylsuccinic anhydride, 5-Ethylhexadecylsuccinic anhydride, 4-Ethylhexadecylsuccinic anhydride, 3-Ethylhexadecylsuccinic anhydride, 2-Ethylhexadecylsuccinic anhydride, 1-Ethylhexadecylsuccinic anhydride, 2-Hexyldodecylsuccinic anhydride, 2-Heptylundecylsuccinic anhydride, isooctadecylsuccinic anhydride and / or 1-Octyl-2-decylsuccinic anhydride.

[0162] In one embodiment of the invention, the at least one alkyl monosubstituted succinic anhydride is selected from the group consisting of butyl succinic anhydride, hexyl succinic anhydride, heptyl succinic anhydride, octyl succinic anhydride, hexadecyl succinic anhydride, octadecyl succinic anhydride, and mixtures thereof.

[0163] In one embodiment of the invention, the at least one monosubstituted succinic anhydride is an alkyl monosubstituted succinic anhydride. For example, the alkyl monosubstituted succinic anhydride is butyl succinic anhydride. Alternatively, the alkyl monosubstituted succinic anhydride is hexyl succinic anhydride. Alternatively, the alkyl monosubstituted succinic anhydride is heptyl succinic anhydride or octyl succinic anhydride. Alternatively, the alkyl monosubstituted succinic anhydride is hexadecyl succinic anhydride. For example, the alkyl monosubstituted succinic anhydride is a straight-chain hexadecyl succinic anhydride, such as n-hexadecyl succinic anhydride, or a branched-chain hexadecyl succinic anhydride, such as 1-hexyl-2-decyl succinic anhydride. Alternatively, the alkyl monosubstituted succinic anhydride is octadecyl succinic anhydride. For example, one of the alkyl monosubstituted succinic anhydrides is a straight-chain octadecyl succinic anhydride, such as n-octadecyl succinic anhydride, or a branched-chain octadecyl succinic anhydride, such as isooctadecyl succinic anhydride or 1-octyl-2-decyl succinic anhydride.

[0164] In one embodiment of the present invention, the alkyl monosubstituted succinic anhydride is butyl succinic anhydride, such as n-butyl succinic anhydride.

[0165] In one embodiment of the invention, the at least one monosubstituted succinic anhydride is a mixture of two or more alkyl monosubstituted succinic anhydrides. For example, the at least one monosubstituted succinic anhydride is a mixture of two or three alkyl monosubstituted succinic anhydrides.

[0166] In one embodiment of the invention, the at least one monosubstituted succinic anhydride is composed of succinic anhydride, wherein the succinic anhydride is monosubstituted as a group of a straight-chain or branched alkenyl group, and the total number of carbon atoms in the substituent is C2 to C20, preferably C3 to C20 and most preferably C4 to C20.

[0167] In the context of this invention, the term "alkenyl" refers to a straight-chain or branched, unsaturated organic compound composed of carbon and hydrogen. The organic compound further contains at least one double bond, preferably one double bond, in the substituents. In other words, "alkenyl monosubstituted succinic anhydride" consists of a straight-chain or branched, unsaturated hydrocarbon chain containing side-chain succinic anhydride groups. It should be understood that, in the context of this invention, the term "alkenyl" includes cis and trans isomers.

[0168] In one embodiment of the invention, the at least one monosubstituted succinic anhydride is at least one linear or branched alkenyl monosubstituted succinic anhydride. For example, the at least one alkenyl monosubstituted succinic anhydride is selected from the group consisting of: vinyl succinic anhydride, propenyl succinic anhydride, butenyl succinic anhydride, triisobutyl succinic anhydride, pentenyl succinic anhydride, hexenyl succinic anhydride, heptenyl succinic anhydride, octenyl succinic anhydride, nonenyl succinic anhydride, decenyl succinic anhydride, dodecenyl succinic anhydride, hexadecenyl succinic anhydride, octadecenyl succinic anhydride, and mixtures thereof.

[0169] Therefore, it should be understood that, for example, the term "hexadecenyl succinic anhydride" includes one or more straight-chain and branched hexadecenyl succinic anhydrides. A specific example of one or more straight-chain hexadecenyl succinic anhydrides is n-hexadecenyl succinic anhydrides such as 14-hexadecenyl succinic anhydride, 13-hexadecenyl succinic anhydride, 12-hexadecenyl succinic anhydride, 11-hexadecenyl succinic anhydride, 10-hexadecenyl succinic anhydride, 9-hexadecenyl succinic anhydride, 8-hexadecenyl succinic anhydride, 7-hexadecenyl succinic anhydride, 6-hexadecenyl succinic anhydride, 5-hexadecenyl succinic anhydride, 4-hexadecenyl succinic anhydride, 3-hexadecenyl succinic anhydride, and / or 2-hexadecenyl succinic anhydride. Specific examples of one or more branched hexadecenyl succinic anhydrides are 14-methyl-9-pentadecenyl succinic anhydride, 14-methyl-2-pentadecenyl succinic anhydride, 1-hexyl-2-decenyl succinic anhydride and / or isohexadecenyl succinic anhydride.

[0170] Furthermore, it should be understood that, for example, the term "octadecenyl succinic anhydride" includes one or more straight-chain and branched octadecenyl succinic anhydrides. A specific example of one or more straight-chain octadecenyl succinic anhydrides is n-octadecenyl succinic anhydrides such as 16-octadecenyl succinic anhydride, 15-octadecenyl succinic anhydride, 14-octadecenyl succinic anhydride, 13-octadecenyl succinic anhydride, 12-octadecenyl succinic anhydride, 11-octadecenyl succinic anhydride, 10-octadecenyl succinic anhydride, 9-octadecenyl succinic anhydride, 8-octadecenyl succinic anhydride, 7-octadecenyl succinic anhydride, 6-octadecenyl succinic anhydride, 5-octadecenyl succinic anhydride, 4-octadecenyl succinic anhydride, 3-octadecenyl succinic anhydride, and / or 2-octadecenyl succinic anhydride. Specific examples of one or more branched octadecenyl succinic anhydrides are 16-methyl-9-heptadecenyl succinic anhydride, 16-methyl-7-heptadecenyl succinic anhydride, 1-octyl-2-decenyl succinic anhydride and / or isooctadecenyl succinic anhydride.

[0171] In one embodiment of the invention, the at least one alkenyl monosubstituted succinic anhydride is selected from the group consisting of hexenyl succinic anhydride, octenyl succinic anhydride, hexadecenyl succinic anhydride, octadecenyl succinic anhydride, and mixtures thereof.

[0172] In one embodiment of the invention, the at least one monosubstituted succinic anhydride is an alkenyl monosubstituted succinic anhydride. For example, the alkenyl monosubstituted succinic anhydride is hexenyl succinic anhydride. Alternatively, the alkenyl monosubstituted succinic anhydride is octenyl succinic anhydride. Alternatively, the alkenyl monosubstituted succinic anhydride is hexadecenyl succinic anhydride. For example, the alkenyl monosubstituted succinic anhydride is a straight-chain hexadecenyl succinic anhydride, such as n-hexadecenyl succinic anhydride, or a branched-chain hexadecenyl succinic anhydride, such as 1-hexyl-2-decenyl succinic anhydride. Alternatively, the alkenyl monosubstituted succinic anhydride is octadecenyl succinic anhydride. For example, the alkyl monosubstituted succinic anhydride is a straight-chain octadecenyl succinic anhydride, such as n-octadecenyl succinic anhydride, or a branched-chain octadecenyl succinic anhydride, such as isooctadecenyl succinic anhydride or 1-octyl-2-decenyl succinic anhydride.

[0173] In one embodiment of the invention, the alkenyl monosubstituted succinic anhydride is a linear octadecenyl succinic anhydride, such as n-octadecenyl succinic anhydride. In another embodiment of the invention, the alkenyl monosubstituted succinic anhydride is a linear octenyl succinic anhydride, such as n-octenyl succinic anhydride.

[0174] If the at least one monosubstituted succinic anhydride is an alkenyl monosubstituted succinic anhydride, it should be understood that, based on the total weight of the at least one monosubstituted succinic anhydride provided in step b), the alkenyl monosubstituted succinic anhydride is present in an amount of ≥95 wt.% and preferably ≥96.5 wt.%.

[0175] In one embodiment of the invention, the at least one monosubstituted succinic anhydride is a mixture of two or more alkenyl monosubstituted succinic anhydrides. For example, the at least one monosubstituted succinic anhydride is a mixture of two or three alkenyl monosubstituted succinic anhydrides.

[0176] If the at least one monosubstituted succinic anhydride is a mixture of two or more alkenyl monosubstituted succinic anhydrides, then one alkenyl monosubstituted succinic anhydride is a straight-chain or branched octadecenyl succinic anhydride, and each additional alkenyl monosubstituted succinic anhydride is selected from vinyl succinic anhydride, propenyl succinic anhydride, butenyl succinic anhydride, pentenyl succinic anhydride, hexenyl succinic anhydride, heptenyl succinic anhydride, nonenyl succinic anhydride, hexadecenyl succinic anhydride, and mixtures thereof. For example, the at least one monosubstituted succinic anhydride is a mixture of two or more alkenyl monosubstituted succinic anhydrides, wherein one alkenyl monosubstituted succinic anhydride is a linear octadecenyl succinic anhydride, and each additional alkenyl monosubstituted succinic anhydride is selected from vinyl succinic anhydride, propenyl succinic anhydride, butenyl succinic anhydride, pentenyl succinic anhydride, hexenyl succinic anhydride, heptenyl succinic anhydride, nonenyl succinic anhydride, hexadecenyl succinic anhydride, and mixtures thereof. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of two or more alkenyl monosubstituted succinic anhydrides, wherein one of the alkenyl monosubstituted succinic anhydrides is branched octadecenyl succinic anhydride, and each additional alkenyl monosubstituted succinic anhydride is selected from vinyl succinic anhydride, propenyl succinic anhydride, butenyl succinic anhydride, pentenyl succinic anhydride, hexenyl succinic anhydride, heptenyl succinic anhydride, nonenyl succinic anhydride, hexadecenyl succinic anhydride, and mixtures thereof.

[0177] For example, the at least one monosubstituted succinic anhydride is a mixture of two or more alkenyl monosubstituted succinic anhydrides, including one or more hexadecenyl succinic anhydrides, such as one or more straight-chain or branched hexadecenyl succinic anhydrides, and one or more octadecenyl succinic anhydrides, such as one or more straight-chain or branched octadecenyl succinic anhydrides.

[0178] In one embodiment of the invention, the at least one monosubstituted succinic anhydride is a mixture of two or more alkenyl monosubstituted succinic anhydrides, comprising one or more linear hexadecenyl succinic anhydrides and one or more linear octadecenyl succinic anhydrides. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of two or more alkenyl monosubstituted succinic anhydrides, comprising one or more branched hexadecenyl succinic anhydrides and one or more branched octadecenyl succinic anhydrides. For example, the one or more hexadecenyl succinic anhydrides are linear hexadecenyl succinic anhydrides, such as n-hexadecenyl succinic anhydride and / or branched hexadecenyl succinic anhydrides, such as 1-hexyl-2-decenyl succinic anhydride. Additionally or alternatively, the one or more octadecenyl succinic anhydrides are linear octadecenyl succinic anhydrides, such as n-octadecenyl succinic anhydride and / or branched octadecenyl succinic anhydride, such as isooctadecenyl succinic anhydride and / or 1-octyl-2-decenyl succinic anhydride.

[0179] If the at least one monosubstituted succinic anhydride is a mixture of two or more alkenyl monosubstituted succinic anhydrides, it should be understood that, based on the total weight of the at least one monosubstituted succinic anhydride provided in step b), one alkenyl monosubstituted succinic anhydride is present in an amount of 20 wt.% to 60 wt.%, and preferably 30 wt.% to 50 wt.%.

[0180] For example, if the at least one monosubstituted succinic anhydride is a mixture of two or more alkenyl monosubstituted succinic anhydrides comprising one or more hexadecenyl succinic anhydrides (such as one or more linear or branched hexadecenyl succinic anhydrides) and one or more octadecenyl succinic anhydrides (such as one or more linear or branched hexadecenyl succinic anhydrides), then preferably, the one or more octadecenyl succinic anhydrides are present in an amount of 20 wt.% to 60 wt.%, and preferably 30 wt.% to 50 wt.%, based on the total weight of the at least one monosubstituted succinic anhydride provided in step b).

[0181] It should also be understood that the at least one monosubstituted succinic anhydride may be a mixture of at least one alkyl monosubstituted succinic anhydride and at least one alkenyl monosubstituted succinic anhydride.

[0182] If the at least one monosubstituted succinic anhydride is a mixture of at least one alkyl monosubstituted succinic anhydride and at least one alkenyl monosubstituted succinic anhydride, it should be understood that the alkyl substituents of the at least one alkyl monosubstituted succinic anhydride and the alkenyl substituents of the at least one alkenyl monosubstituted succinic anhydride are preferably the same. For example, the at least one monosubstituted succinic anhydride is a mixture of ethyl succinic anhydride and vinyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of propyl succinic anhydride and propenyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of butyl succinic anhydride and butenyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of triisobutyl succinic anhydride and triisobutylenyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of pentyl succinic anhydride and pentenyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of hexyl succinic anhydride and hexenyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of heptyl succinic anhydride and heptenyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of octyl succinic anhydride and octenyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of nonyl succinic anhydride and nonenyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of decyl succinic anhydride and decenyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of dodecyl succinic anhydride and dodecenyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of hexadecyl succinic anhydride and hexadecenyl succinic anhydride. For example, the at least one monosubstituted succinic anhydride is a mixture of linear hexadecyl succinic anhydride and linear hexadecenyl succinic anhydride, or a mixture of branched hexadecyl succinic anhydride and branched hexadecenyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of octadecyl succinic anhydride and octadecenyl succinic anhydride. For example, the at least one monosubstituted succinic anhydride is a mixture of linear octadecyl succinic anhydride and linear octadecenyl succinic anhydride, or a mixture of branched octadecyl succinic anhydride and branched octadecenyl succinic anhydride.

[0183] In one embodiment of the invention, the at least one monosubstituted succinic anhydride is a mixture of nonylsuccinic anhydride and nonenylsuccinic anhydride.

[0184] If the at least one monosubstituted succinic anhydride is a mixture of at least one alkyl monosubstituted succinic anhydride and at least one alkenyl monosubstituted succinic anhydride, then the weight ratio between the at least one alkyl monosubstituted succinic anhydride and the at least one alkenyl monosubstituted succinic anhydride is between 90:10 and 10:90 (wt.% / wt.%). For example, the weight ratio between the at least one alkyl monosubstituted succinic anhydride and the at least one alkenyl monosubstituted succinic anhydride is between 70:30 and 30:70 (wt.% / wt.%) or between 60:40 and 40:60.

[0185] Optionally, the at least one monosubstituted succinic anhydride described in step b) of the method of the present invention is provided in combination with at least one monosubstituted succinic acid.

[0186] It should be understood that the expression "at least one" monosubstituted succinic acid means that one or more monosubstituted succinic acids can be provided in step b) of the method of the present invention.

[0187] Therefore, it should be noted that the at least one monosubstituted succinic acid can be a single monosubstituted succinic acid. Alternatively, the at least one monosubstituted succinic acid can be a mixture of two or more monosubstituted succinic acids. For example, the at least one monosubstituted succinic acid can be a mixture of two or three monosubstituted succinic acids, such as two monosubstituted succinic acids.

[0188] In one embodiment of the invention, the at least one monosubstituted succinic acid is a monosubstituted succinic acid.

[0189] It should be understood that the at least one monosubstituted succinic acid represents a surface treatment agent and is composed of succinic acid, which is monosubstituted by a group selected from any straight-chain, branched, aliphatic and cyclic group, and the total number of carbon atoms in the substituent is C2 to C20.

[0190] In one embodiment of the invention, the at least one monosubstituted succinic acid is composed of succinic anhydride, wherein the succinic acid is monosubstituted by a group selected from straight-chain, branched, aliphatic, and cyclic groups, and the total number of carbon atoms in the substituent is C3 to C20. For example, the at least one monosubstituted succinic acid is composed of succinic acid, wherein the succinic acid is monosubstituted by a group selected from straight-chain, branched, aliphatic, and cyclic groups, and the total number of carbon atoms in the substituent is C4 to C20.

[0191] If the at least one monosubstituted succinic anhydride described in method step b) is provided together with at least one monosubstituted succinic acid, it should be understood that the at least one monosubstituted succinic anhydride and the at least one monosubstituted succinic acid may include the same or different substituents.

[0192] In one embodiment of the invention, the succinic acid molecule of the at least one monosubstituted succinic acid and the succinic anhydride molecule of the at least one monosubstituted succinic anhydride are monosubstituted by the same group selected from any straight-chain, branched, aliphatic, or cyclic group, wherein the total number of carbon atoms in the substituent of any straight-chain, branched, or aliphatic group is C2 to C20, preferably C3 to C20, and most preferably C4 to C20, and the total number of carbon atoms in the substituent of the cyclic group is C3 to C20, and most preferably C4 to C20.

[0193] If the at least one monosubstituted succinic anhydride is provided in combination with at least one monosubstituted succinic acid, the at least one monosubstituted succinic acid is present in an amount of ≤10 mol.-% based on the total molar amount of the at least one monosubstituted succinic anhydride and the at least one monosubstituted succinic acid. For example, the at least one monosubstituted succinic acid is present in an amount of ≤5 mol.-%, preferably ≤2.5 mol.-%, and most preferably ≤1 mol.-% based on the total molar amount of the at least one monosubstituted succinic anhydride and the at least one monosubstituted succinic acid.

[0194] In one embodiment of the invention, at least one monosubstituted succinic anhydride and at least one monosubstituted succinic acid are provided in method step b).

[0195] If the at least one monosubstituted succinic anhydride is provided in combination with the at least one monosubstituted succinic acid, the at least one monosubstituted succinic anhydride and the at least one monosubstituted succinic acid are preferably provided as a blend.

[0196] Preferably, the at least one surface treatment agent in step b) is provided in a total amount of 0.1 wt.% to 3 wt.% based on the total dry weight of the at least one calcium carbonate-containing filler material in step a).

[0197] For example, the at least one surface treatment agent of step b) is provided in a total amount of 0.1 wt.% to 2 wt.% and most preferably 0.1 wt.% to 1.5 wt.% based on the total dry weight of the at least one calcium carbonate-containing filler material of step a).

[0198] Alternatively or alternatively, preferably, the total weight of the surface treatment agent on the surface of the at least one calcium carbonate-containing filler material is less than 35 mg / m³. 2 The amount of the at least one calcium carbonate-containing filler material provided in step a) is provided for the at least one surface treatment agent in step b).

[0199] In one embodiment of the invention, preferably, the total weight of the surface treatment agent on the surface of the at least one calcium carbonate-containing filler material is less than 20 mg / m³. 2 Even more preferably less than 15 mg / m 2 And most preferably less than 5 mg / m 2 The amount of the at least one calcium carbonate-containing filler material provided in step a) is provided for the at least one surface treatment agent in step b).

[0200] For example, preferably, the total weight of the surface treatment agent on the surface of the at least one calcium carbonate-containing filler material is 0.1-35 mg / m³. 2 More preferably 0.2-20 mg / m 2 Even more preferably 0.5-15 mg / m 2 And the most preferred dosage is 0.1-5 mg / m². 2 The amount of the at least one calcium carbonate-containing filler material provided in step a) is provided for the at least one surface treatment agent in step b).

[0201] Characterization in step c): Contacting the at least one calcium carbonate-containing filler material with the at least one surface treatment agent.

[0202] According to step c) of the method of the present invention, in one or more steps, the surface of the at least one calcium carbonate-containing filler material of step a) is contacted with the at least one surface treatment agent of step b) in any order under mixing, such that a treatment layer comprising the at least one surface treatment agent and / or one or more reaction products thereof is formed on the surface of the at least one calcium carbonate-containing filler material of step a).

[0203] Step c) of contacting the at least one calcium carbonate-containing filler material with the at least one surface treatment agent occurs under mild conditions. It should be understood that mild conditions are required to reduce the amount of fine particles due to low abrasion, such that the surface-treated filler material product obtained by the method has a particle size distribution substantially the same as that of the at least one calcium carbonate-containing filler material of step a) (with a small amount of fine particles). This is achieved, in particular, in a way that the total energy intake is lower than that typically required by prior art methods. More precisely, preferably, contact step c) is performed in a way that the total energy intake achieved by adding the at least one surface treatment agent of step b) to the at least one calcium carbonate-containing filler material of step a) does not exceed 15 kWh / T. For example, contact step c) is performed in a way that the total energy intake achieved by adding the at least one surface treatment agent of step b) to the at least one calcium carbonate-containing filler material of step a) is in the range of 2 kWh / T to 15 kWh / T, for example, 2 kWh to 10 kWh / T or 2 kWh / T to 8 kWh / T.

[0204] In one embodiment of the invention, the method of the invention, particularly contact step c), can be performed in a continuous mode. In this case, the at least one calcium carbonate-containing filler material can be contacted with the at least one surface treatment agent at a constant flow rate, such that a constant concentration of the at least one surface treatment agent is provided during step c).

[0205] Alternatively, the at least one calcium carbonate-containing filler material may be contacted with the at least one surface treatment agent in a single step, wherein the at least one surface treatment agent is preferably added at once.

[0206] In another embodiment of the invention, the method of the invention, particularly contact step c), can be performed in batch mode, i.e., in more than one step, the at least one calcium carbonate-containing filler material is contacted with the at least one surface treatment agent, wherein preferably the at least one surface treatment agent is added in approximately equal portions. Alternatively, the at least one surface treatment agent may be added to the at least one calcium carbonate-containing filler material in unequal portions, i.e., in larger and smaller portions.

[0207] It should be understood that contact step c) can be performed by adding the at least one surface treatment agent of step b) to the at least one calcium carbonate-containing filler material of step a).

[0208] Alternatively, the at least one calcium carbonate-containing filler material of step a) may be added to the at least one surface treatment agent of step b).

[0209] It should be understood that particularly advantageous effects are obtained if the at least one surface treatment agent of step b) is added to the at least one calcium carbonate-containing filler material of step a). For example, contact step c) is performed by spraying the at least one surface treatment agent of step b) onto the at least one calcium carbonate-containing filler material of step a).

[0210] To achieve a low total energy intake, it should be understood that step c) of the method should be performed without any additional temperature intake (i.e., through heating or cooling). That is, step c) is preferably performed at the appropriate ambient temperature. Therefore, step c) is preferably performed at a temperature in the range of 18°C ​​to 45°C.

[0211] In view of this, it is required that the at least one surface treatment agent has a usable viscosity within the temperature range, that is, the at least one surface treatment agent should be in a molten or liquid state at a temperature ranging from 18°C ​​to 45°C in order to achieve sufficient surface treatment.

[0212] Therefore, it is preferable that the temperature is not adjusted before and / or during contact step c), such that the at least one surface treatment agent is in a molten or liquid state, i.e., the method has no temperature adjustment step before and / or during contact step c).

[0213] The processing time for performing contact step c) is preferably 1000 seconds or less, preferably 500 seconds or less, more preferably 250 seconds or less, and most preferably 0.1 seconds to 1000 seconds. For example, the contact step c) is performed for a period of 0.1 seconds to 20 seconds, preferably 0.5 seconds to 15 seconds, and most preferably 1 second to 10 seconds.

[0214] Furthermore, it should be understood that if step c) is performed in an Archimedes spiral device such as a screw conveyor, drum mixer, pneumatic air conveyor system, planetary mixer, or Guedu mixer, the total energy intake can be reduced.

[0215] This equipment is well-known, and technicians will adapt the equipment used to the applied conditions.

[0216] However, preferably, the diameter-to-height ratio of the drum mixer, the planetary mixer, or the Guedu mixer is 1:1 to 1:5. More preferably, the drum mixer, planetary mixer, or Guedu mixer operates at a temperature ranging from 18°C ​​to 45°C.

[0217] Regarding the Archimedes' spiral apparatus, it should be understood that if the Archimedes' spiral apparatus is operated at a specific angle, the total energy intake is particularly low.

[0218] In one embodiment, the Archimedes screw device operates at an angle ranging from 0° to 80°, and more preferably from 0° to 70°. Preferably, the Archimedes screw device operates at an angle ranging from 30° to 80°, and more preferably from 35° to 70°.

[0219] If contact step c) is performed in an Archimedes spiral device, the Archimedes spiral device operates at an angle ranging from 30° to 80°, and more preferably from 35° to 70°.

[0220] In one embodiment, contact step c) is performed in two Archimedean spiral devices. For example, the first Archimedean spiral device operates at an angle ranging from 0° to 30°, and more preferably from 0° to 20°, and the second Archimedean spiral device operates at an angle ranging from 30° to 80°, and more preferably from 35° to 70°. In this embodiment, the first Archimedean spiral device is connected to the second Archimedean spiral device via a chute. That is, the contents of the first Archimedean spiral device are preferably loaded onto the second Archimedean spiral device via the chute, i.e., the loading point on the second Archimedean spiral device is lower than the discharge point of the first Archimedean spiral device.

[0221] Furthermore, it should be understood that if step c) is performed in such a manner as adding the at least one surface treatment agent of step b) to the at least one calcium carbonate-containing filler material of step a) in the lower 1 / 3 of the Archimedes spiral device, the total energy intake can be particularly reduced.

[0222] For example, if contact step c) is performed in an Archimedes spiral device, then in the lower 1 / 3 of the Archimedes spiral device, preferably the at least one surface treatment agent of step b) is added to the at least one calcium carbonate-containing filler material of step a), the Archimedes spiral device operating at an angle ranging from 30° to 80°, and more preferably from 35° to 70°.

[0223] If contact step c) is performed in both Archimedean spiral devices, then in the lower 1 / 3 of the first Archimedean spiral device and / or the lower 1 / 3 of the second Archimedean spiral device, preferably, the at least one surface treatment agent of step b) is added to the at least one calcium carbonate-containing filler material of step a), wherein the first Archimedean spiral device operates at an angle ranging from 0° to 30°, and more preferably from 0° to 20°, and the second Archimedean spiral device operates at an angle ranging from 30° to 80°, and more preferably from 35° to 70°. For example, in the lower 1 / 3 of the first Archimedean spiral device or the lower 1 / 3 of the second Archimedean spiral device, preferably, the at least one surface treatment agent of step b) is added to the at least one calcium carbonate-containing filler material of step a), wherein the first Archimedean spiral device operates at an angle ranging from 0° to 30°, and more preferably from 0° to 20°, and the second Archimedean spiral device operates at an angle ranging from 30° to 80°, and more preferably from 35° to 70°. Alternatively, in the lower 1 / 3 of the first Archimedes' screw device and the lower 1 / 3 of the second Archimedes' screw device, preferably, the at least one surface treatment agent of step b) is added to the at least one calcium carbonate-containing filler material of step a), the first Archimedes' screw device operating at an angle ranging from 0° to 30°, and more preferably from 0° to 20°, and the second Archimedes' screw device operating at an angle ranging from 30° to 80°, and more preferably from 35° to 70°. Therefore, in this embodiment, the at least one surface treatment agent of step b) is divided into equal or unequal portions (e.g., two portions) of the at least one surface treatment agent of step b).

[0224] Further preferably, the Archimedes screw device operates at a temperature ranging from 18°C ​​to 45°C.

[0225] In view of this, it is preferred that the at least one surface treatment agent of step b) be added to the at least one calcium carbonate-containing filler material of step a), wherein the at least one calcium carbonate-containing filler material is loaded into the Archimedes screw device such as a screw conveyor, the drum mixer, the pneumatic air conveyor system, the planetary mixer or the Guedu mixer.

[0226] It should be understood that the at least one surface treatment agent is added in contact step c) in an amount of 0.1 wt.% to 3 wt.% of the total dry weight of the at least one calcium carbonate-containing filler material of step a). For example, the at least one surface treatment agent is added in contact step d) in an amount of 0.1 wt.% to 2 wt.% or 0.1 wt.% to 1.5 wt.% of the total dry weight of the at least one calcium carbonate-containing filler material of step a).

[0227] The obtained surface-treated filler material product, by weight of the total weight of the surface-treated filler material product, has a residue on a 45 μm sieve greater than 0.5 wt.% as measured according to ISO 787 / 7. Preferably, the obtained surface-treated filler material product has a residue on a 45 μm sieve ranging from 0.5 wt.% to 30 wt.%, and more preferably from 0.75 wt.% to 25 wt.%, as measured according to ISO 787 / 7. For example, the obtained surface-treated filler material product has a residue on a 45 μm sieve ranging from 0.75 wt.% to 15 wt.%, or from 0.75 wt.% to 10 wt.%, as measured according to ISO 787 / 7.

[0228] As mentioned above, the method is characterized by the fact that due to the low energy intake and almost no wear, the obtained surface-treated filler material product has a particle size distribution that is almost identical to that of the at least one calcium carbonate-containing filler material of step a).

[0229] In view of this, preferably, the amount of residue on a 45 μm sieve of the at least one calcium carbonate-containing filler material in step a) as measured according to ISO 787 / 7 differs from the amount of residue on a 45 μm sieve of the surface-treated filler material product as measured according to ISO 787 / 7 by less than 20 wt.%. Preferably, the amount of residue on a 45 μm sieve of the at least one calcium carbonate-containing filler material in step a) as measured according to ISO 787 / 7 differs from the amount of residue on a 45 μm sieve of the surface-treated filler material product as measured according to ISO 787 / 7 by less than 15 wt.%, more preferably less than 10 wt.%, and even more preferably less than 5 wt.%.

[0230] It should be noted that the residue on a 45 μm sieve of the surface-treated filler material product, as measured according to ISO 787 / 7, may be greater than or less than the amount of residue on a 45 μm sieve of the at least one calcium carbonate-containing filler material in step a) as measured according to ISO 787 / 7.

[0231] It should be understood that the treated layer formed on the surface of the at least one calcium carbonate-containing filler material includes the at least one surface treatment agent provided in step b) and / or one or more reaction products as reaction products obtained by contacting the calcium carbonate-containing filler material with the at least one surface treatment agent in step b). In this case, the treated layer of the surface-treated filler material product preferably further includes one or more reaction products of the at least one surface treatment agent formed on the surface of the at least one calcium carbonate-containing filler material in step c). For example, one or more reaction products such as one or more calcium salts and / or magnesium salts of the at least one surface treatment agent.

[0232] The treatment layer is preferably characterized in that the total weight of the at least one surface treatment agent and / or one or more reaction products thereof on the surface of the surface-treated filler material is 0.1-35 mg / m³. 2 More preferably 0.2-20 mg / m 2 And the most preferred dosage is 0.5-15 mg / m². 2 and 0.1-5 mg / m 2 The at least one of the filler materials includes calcium carbonate.

[0233] The treatment layer is preferably characterized in that the total weight of the at least one surface treatment agent and / or one or more reaction products thereof on the surface of the surface-treated filler material is 0.1-2 wt.% / m. 2 More preferably 0.2-1 wt.% / m 2 And most preferably 0.3-0.5 wt.% / m 2 The at least one of the filler materials includes calcium carbonate.

[0234] It should be further understood that, based on the total dry weight of the at least one filler material comprising calcium carbonate, the amount of the treated layer in the obtained surface-treated filler material is 0.1 wt.% to 3 wt.%, preferably 0.1 wt.% to 2 wt.%, more preferably 0.2 wt.% to 4 wt.%, and most preferably 0.1 wt.% to 1.5 wt.%.

[0235] Therefore, it should be understood that the at least one calcium carbonate-containing filler material product obtained in step c) comprises, preferably consists of, the following: at least one calcium carbonate-containing filler material and a treatment layer comprising the at least one surface treatment agent and / or one or more reaction products thereof. The treatment layer is formed on the surface of the at least one calcium carbonate-containing filler material obtained in step a).

[0236] Alternatively or concurrently, the treated layer of the surface-treated filler material product comprises at least one surface-treatment agent and / or one or more of its reaction products in a specific molar ratio. For example, the molar ratio of the at least one surface-treatment agent to one or more of its reaction products is from 99.9:0.1 to 0.1:99.9, preferably from 70:30 to 90:10.

[0237] In the context of this invention, the term "molar ratio of the at least one surface treatment agent to one or more reaction products" means the sum of the molecular weights of the at least one surface treatment agent to the sum of the molecular weights of the surface treatment agent molecules in its reaction products.

[0238] It should be understood that the at least one calcium carbonate-containing filler material may include water or an organic solvent. In one embodiment, the resulting surface-treated filler material product may be dried. This optional step is preferably performed to reduce the water or organic solvent content of the resulting surface-treated filler material product. Therefore, the moisture content of the resulting dried surface-treated filler material product is lower than the moisture content of the surface-treated filler material product obtained before the drying step, i.e., after step c).

[0239] According to one embodiment of the invention, the method therefore includes an additional step d): drying the surface-treated filler material product obtained in step c).

[0240] For example, under ambient pressure or reduced pressure, at a temperature ranging from 60°C to 180°C, preferably from 50°C to 150°C, more preferably from 60°C to 120°C, and most preferably from 80°C to 120°C, an optional drying step d) is performed until the water or organic solvent content in the obtained surface-treated filler material product is reduced.

[0241] In one embodiment, an optional drying step d) is performed, based on the total weight of the at least one calcium carbonate-containing filler material, until the water or organic solvent content of the obtained surface-treated filler material product ranges from 0.001 wt.% to 20 wt.%, preferably from 0.005 wt.% to 15 wt.%, more preferably from 0.01 wt.% to 10 wt.%, and most preferably from 0.05 wt.% to 5 wt.%.

[0242] It should be understood that optional drying step d) can be performed under ambient pressure or reduced pressure. Preferably, drying is performed under ambient pressure.

[0243] Therefore, optional drying step d) is preferably performed at ambient pressure and at a temperature of 60°C to 180°C. For example, optional drying step d) is performed at ambient pressure and at a temperature in the range of 50°C to 150°C, preferably 60°C to 120°C, and more preferably 80°C to 120°C.

[0244] Preferably, steps a) to c) are performed in the absence of water or organic solvents, therefore the method of the present invention does not have step d).

[0245] The surface-treated filler material product obtained according to the present invention is a coarse material.

[0246] Specifically, the surface-treated filler material product includes

[0247] a) at least one calcium carbonate-containing filler material, said at least one calcium carbonate-containing filler material having

[0248] i) The volume median particle size d in the range of 5 μm to 100 μm 50 value,

[0249] ii) Top cuts ranging from 30 μm to 500 μm (d 98 ),

[0250] b) A treatment layer on the surface of the at least one calcium carbonate-containing filler material, the treatment layer comprising at least one surface treatment agent and / or its reaction product, wherein the surface-treated filler material product comprises, based on the total dry weight of the at least one calcium carbonate-containing filler material, an amount of 0.1 wt.% to 3 wt.% of the treatment layer.

[0251] The surface-treated filler material product has a residue on a 45 μm sieve of greater than 0.5 wt.% based on the total weight of the surface-treated filler material product, as measured according to ISO 787 / 7.

[0252] For the definitions of the at least one calcium carbonate-containing filler material, the at least one surface treatment agent, and their preferred embodiments, refer to the notes provided above when discussing method steps a), b), and c).

[0253] Preferably, the surface-treated filler material product is in powder form.

[0254] In one embodiment of the invention, a surface-treated filler material product can be obtained (or obtained) by the method of the invention.

[0255] Therefore, the surface-treated filler material product includes

[0256] a) at least one calcium carbonate-containing filler material, said at least one calcium carbonate-containing filler material having

[0257] i) The volume median particle size d in the range of 5 μm to 100 μm 50 value,

[0258] ii) Top cuts ranging from 30 μm to 500 μm (d 98 ).

[0259] b) A treatment layer on the surface of the at least one calcium carbonate-containing filler material, the treatment layer comprising at least one surface treatment agent and / or its reaction product, wherein the surface-treated filler material product comprises, based on the total dry weight of the at least one calcium carbonate-containing filler material, an amount of 0.1 wt.% to 3 wt.% of the treatment layer.

[0260] The surface-treated filler material product has a residue on a 45 μm sieve greater than 0.5 wt.% based on the total weight of the surface-treated filler material product, as measured according to ISO 787 / 7.

[0261] The surface-treated filler material product can be obtained (or acquired) by a method for preparing the surface-treated filler material product, the method comprising at least the following steps:

[0262] a) Provide at least one calcium carbonate-containing filler material, said at least one calcium carbonate-containing filler material having

[0263] i) The volume median particle size d in the range of 5 μm to 100 μm 50 value,

[0264] ii) Top cuts ranging from 30 μm to 500 μm (d 98 ),as well as

[0265] iii) Based on the total weight of the calcium carbonate-containing filler material, the residue on a 45 μm sieve greater than 0.5 wt.% as measured according to ISO 787 / 7,

[0266] b) Provide at least one surface treatment agent that is in a molten or liquid state at a temperature ranging from 18°C ​​to 45°C.

[0267] c) In one or more steps, the surface of the at least one calcium carbonate-containing filler material of step a) is brought into contact with the at least one surface treatment agent of step b) under mixing, such that a treatment layer comprising the at least one surface treatment agent and / or one or more reaction products thereof is formed on the surface of the at least one calcium carbonate-containing filler material of step a).

[0268] The obtained surface-treated filler material product, based on the total weight of the surface-treated filler material product, has a residue on a 45 μm sieve greater than 0.5 wt.% as measured according to ISO 787 / 7.

[0269] The surface-treated filler material product thus obtained is advantageously incorporated into articles, preferably polymer articles, which comprise at least one polymer resin and 1 wt.% to 95 wt.% of the surface-treated filler material product.

[0270] Therefore, in another aspect, the present invention relates to an article, preferably a polymeric article, comprising the surface-treated filler material product. In one embodiment, the article, preferably a polymeric article, comprises at least one polymeric resin and, by weight of the total polymeric composition, 1 wt.% to 95 wt.% of the surface-treated filler material product. For example, by weight of the article, the article, preferably a polymeric article, comprises 5 wt.% to 95 wt.% and preferably 10 wt.% to 85 wt.% of the surface-treated filler material product. For example, by weight of the article, the article, preferably a polymeric article, comprises 15 wt.% to 80 wt.% of the surface-treated filler material product.

[0271] Therefore, the polymer composition comprises at least one polymer resin. The polymer resin represents the skeleton of the composition and, preferably, provides strength, flexibility, toughness, and durability to the final article.

[0272] It should be understood that at least one polymer resin according to the present invention is not limited to a specific resin material, as long as the polymer composition is suitable for the preparation of articles, preferably polymer articles.

[0273] In one embodiment of the invention, the at least one polymer resin is at least one thermoplastic polymer. Therefore, it is preferred that the at least one polymer resin is a thermoplastic polymer selected from the group consisting of polyolefins, polyamides, halogen-containing polymers, polyesters, polyurethanes, and homopolymers and / or copolymers of thermosetting materials.

[0274] Alternatively or concurrently, the at least one polymeric resin is a homopolymer and / or copolymer of a polyolefin. For example, the at least one polymeric resin is a homopolymer and copolymer of a polyolefin. Alternatively, the at least one polymeric resin is a homopolymer or copolymer of a polyolefin.

[0275] It should be understood that the at least one polymer resin is preferably a homopolymer of a polyolefin.

[0276] For example, the polyolefin can be polyethylene and / or polypropylene and / or polybutene. Therefore, if the polyolefin is polyethylene, it is selected from the group consisting of homopolymers and / or copolymers of polyethylene, such as high-density polyethylene (HDPE), medium-density polyethylene (MDPE), low-density polyethylene (LDPE), very low-density polyethylene (VLDPE), and linear low-density polyethylene (LLDPE).

[0277] For example, polyolefins are homopolymers and / or copolymers of polyethylene.

[0278] Based on the total weight of polyethylene, the homopolymer of polyethylene used in this invention refers to polyethylene comprising substantially (i.e., greater than 99.7 wt.%, but still more preferably at least 99.8 wt.%) polyethylene units. For example, only ethylene units are detectable in the homopolymer of polyethylene.

[0279] In the case where the at least one polymer resin in the polymer composition comprises a copolymer of polyethylene, it should be understood that the polyethylene contains units that are ethylene-derived as a major component. Therefore, by weight of the total polyethylene, the copolymer of polyethylene comprises at least 55 wt.% ethylene-derived units, more preferably at least 60 wt.% ethylene-derived units. For example, by weight of the total polyethylene, the copolymer of polyethylene comprises 60 wt.% to 99.5 wt.% ethylene-derived units, more preferably 90 wt.% to 99 wt.% ethylene-derived units. The comonomers present in such copolymers of polyethylene are C3 to C10 α-olefins, preferably 1-butene, 1-hexene, and 1-octene, with the latter being particularly preferred.

[0280] Alternatively or alternatively, polyolefins are homopolymers and / or copolymers of polypropylene.

[0281] Based on the total weight of polypropylene, the homopolymer of polypropylene, as used throughout this invention, refers to polypropylene that is substantially (i.e., greater than 99 wt.%, but still more preferably at least 99.5 wt.%, such as at least 99.8 wt.%) composed of propylene units. In a preferred embodiment, only propylene units are detectable in the homopolymer of polypropylene.

[0282] In the case where the at least one polymer resin in the polymer composition comprises a copolymer of polypropylene, the polypropylene preferably contains units derived from propylene as a major component. The copolymer of polypropylene preferably comprises, and is preferably composed of, units derived from propylene and C2 and / or at least one C4 to C10 α-olefin. In one embodiment of the invention, the copolymer of polypropylene comprises, and is preferably composed of, units derived from propylene and at least one α-olefin selected from the group consisting of ethylene, 1-butene, 1-pentene, 1-hexene, and 1-octene. For example, the copolymer of polypropylene comprises, and is preferably composed of, units derived from propylene and ethylene. In one embodiment of the invention, by weight of the total polypropylene, units derived from propylene constitute the major portion of the polypropylene, i.e., at least 60 wt.%, preferably at least 70 wt.%, more preferably at least 80 wt.%, still more preferably 60 wt.% to 99 wt.%, even more preferably 70 wt.% to 99 wt.%, and most preferably 80 wt.% to 99 wt.%. The amount of units derived from C2 and / or at least one C4 to C10 α-olefin in the copolymer of polypropylene, based on the total weight of the copolymer, ranges from 1 wt.% to 40 wt.%, more preferably from 1 wt.% to 30 wt.%, and most preferably from 1 wt.% to 20 wt.%.

[0283] If the copolymer of polypropylene comprises only units derived from propylene and ethylene, then the amount of ethylene, by weight of the total copolymer of polypropylene, preferably ranges from 1 wt.% to 20 wt.%, more preferably from 1 wt.% to 15 wt.%, and most preferably from 1 wt.% to 10 wt.%. Therefore, the amount of propylene, by weight of the total copolymer of polypropylene, preferably ranges from 80 wt.% to 99 wt.%, more preferably from 85 wt.% to 99 wt.%, and most preferably from 90 wt.% to 99 wt.%.

[0284] Alternatively or alternatively, polyolefins are homopolymers and / or copolymers of polybutene.

[0285] Based on the total weight of polybutene, the homopolymer of polybutene used throughout this invention refers to polypropylene that is substantially (i.e., greater than 99 wt.%, but more preferably at least 99.5 wt.%, such as at least 99.8 wt.%) composed of butene units. In a preferred embodiment, only butene units are detectable in the homopolymer of polybutene.

[0286] In the case where the at least one polymer resin in the polymer composition comprises a copolymer of polybutene, the polybutene preferably contains units that are derived from butene as a major component. The copolymer of polybutene preferably comprises, and is preferably composed of, units derived from butene and C2 and / or C3 and / or at least one C5 to C10 α-olefin. In one embodiment of the invention, the copolymer of polybutene comprises, and is preferably composed of, units derived from butene and at least one α-olefin selected from the group consisting of ethylene, 1-propylene, 1-pentene, 1-hexene, and 1-octene. For example, the copolymer of polybutene comprises, and is preferably composed of, units derived from butene and ethylene. In one embodiment of the invention, based on the total weight of the polybutene, units derived from butene constitute the major portion of the polybutene, i.e., at least 60 wt.%, preferably at least 70 wt.%, more preferably at least 80 wt.%, still more preferably 60 wt.% to 99 wt.%, even more preferably 70 wt.% to 99 wt.%, and most preferably 80 wt.% to 99 wt.%. Based on the total weight of the polybutene copolymer, the amount of units derived from C2 and / or C3 and / or at least one C5 to C10 α-olefin in the polybutene copolymer ranges from 1 wt.% to 40 wt.%, more preferably from 1 wt.% to 30 wt.%, and most preferably from 1 wt.% to 20 wt.%.

[0287] If the at least one polymer resin is a homopolymer and / or copolymer of a halogen-containing polymer, then the at least one polymer resin is preferably selected from polyvinyl chloride (PVC), polyvinylidene chloride (PVDC), polyvinylidene fluoride (PVDF), polytetrafluoroethylene (PTFE), and copolymers of PVC-polyvinyl acetate and plasticized PVC and their copolymers.

[0288] If the at least one polymer resin is a homopolymer and / or copolymer of polyester, then the at least one polymer resin is preferably selected from polyethylene terephthalate (PET), polypropylene terephthalate (PTT), polybutylene terephthalate (PBT), polyethylene naphthalate (PEN), and biodegradable polyesters such as polylactic acid (PLA).

[0289] In one embodiment of the invention, the at least one polymer resin is a homopolymer of polyethylene and / or polypropylene and / or polybutene. For example, the at least one polymer resin is a homopolymer of polyethylene and polypropylene. Alternatively, the at least one polymer resin is a homopolymer of polyethylene or polypropylene. In one embodiment of the invention, the at least one polymer resin is a homopolymer of polypropylene.

[0290] The phrase "at least one" polymer resin means that one or more polymer resins may be present in the polymer composition of the present invention.

[0291] Therefore, it should be understood that the at least one polymer resin may be a mixture of two or more polymer resins. For example, if the at least one polymer resin is a mixture of two or more polymer resins, one polymer resin is a homopolymer or copolymer of polypropylene, and the second or additional polymer resin is selected from the group consisting of homopolymers and / or copolymers of polyethylene, polybutene, polyamide, polyester, halogen-containing polymers and mixtures thereof.

[0292] In one embodiment of the invention, the at least one polymer resin is a polymer resin. Preferably, the at least one polymer resin is a homopolymer of polyethylene or polypropylene.

[0293] In one embodiment of the invention, the melt temperature Tm of the at least one polymer resin is higher than 100°C, more preferably higher than 150°C, such as higher than 200°C. For example, the melt temperature range of the at least one polymer resin is 100°C to 350°C, more preferably 150°C to 325°C, still more preferably 180°C to 260°C, and most preferably 200°C to 300°C.

[0294] Furthermore, it should be understood that the at least one polymer resin may be selected from polyolefins having a broad melt flow rate spectrum. Generally, it is preferred that the melt flow rate (MFR) (190°C) of the polyolefin is 0.1 to 3000 g / 10 min, more preferably 0.2 to 2500 g / 10 min. For example, the melt flow rate (MFR) (190°C) of the polyolefin is 0.3 to 2000 g / 10 min or 0.3 to 1600 g / 10 min. Alternatively or additionally, the melt flow rate (MFR) (230°C) of the at least one polymer resin is 0.1 to 3000 g / 10 min, more preferably 0.2 to 2500 g / 10 min. For example, the melt flow rate (MFR) (230°C) of the polyolefin is 0.3 to 2000 g / 10 min or 0.3 to 1600 g / 10 min.

[0295] For example, if the at least one polymer resin is a polyolefin that is a homopolymer and / or copolymer of polypropylene, it is preferred that the melt flow rate (MFR) of the at least one polymer resin (190°C, 2.16 kg) is 1 to 3000 g / 10 min, more preferably 3 to 2500 g / 10 min. For example, the melt flow rate (MFR) of the at least one polymer resin that is a homopolymer and / or copolymer of polypropylene is 5 to 2000 g / 10 min or 10 to 1600 g / 10 min. Preferably, the melt flow rate (MFR) of the at least one polymer resin that is a homopolymer and / or copolymer of polypropylene is 1 to 3000 g / 10 min, more preferably 3 to 2500 g / 10 min. For example, the melt flow rate (MFR) of the at least one polymer resin, which is a homopolymer and / or copolymer of polypropylene, is 5 to 2000 g / 10 min or 10 to 1600 g / 10 min.

[0296] If the at least one polymer resin is a polyolefin that is a homopolymer and / or copolymer of polyethylene, it should be understood that the at least one polymer resin has a relatively low melt flow rate. Therefore, it is preferred that the melt flow rate (MFR) (190°C) of the at least one polymer resin as a homopolymer and / or copolymer of polyethylene is 0.5 to 20 g / 10 min, more preferably 0.7 to 15 g / 10 min. For example, the melt flow rate (MFR) (190°C) of the at least one polymer resin is 0.9 to 10 g / 10 min or 0.9 to 5 g / 10 min. Alternatively or additionally, the melt flow rate (MFR) (230°C) of the at least one polymer resin as a homopolymer and / or copolymer of polyethylene is 0.1 to 3000 g / 10 min, more preferably 0.2 to 2500 g / 10 min. For example, the melt flow rate (MFR) of the at least one polymer resin, which is a homopolymer and / or copolymer of polyethylene, is 0.3 to 2000 g / 10 min or 0.3 to 1600 g / 10 min.

[0297] In one embodiment of the invention, the polymer composition comprises, by weight of the total polymer composition, 5 wt.% to 95 wt.% and preferably 10 wt.% to 85 wt.% of the surface-treated filler material product. For example, the polymer composition comprises, by weight of the total polymer composition, 15 wt.% to 80 wt.% of the surface-treated filler material product. Attached Figure Description

[0298] Figure 1 The viscosity comparison of ASA-treated CaCO3 in PVC-plasticized sol-gel flooring is shown. Detailed implementation mode

[0299] The following examples can additionally demonstrate the present invention, but do not mean to limit the present invention to the exemplary embodiments.

[0300] Example

[0301] A) Measurement method

[0302] The following measurement methods are used to evaluate the parameters given in the examples and claims.

[0303] Particle size distribution of particulate materials (mass % of particles with diameter < X) and weight median diameter (d 50 )

[0304] The Malvern Mastersizer 2000 laser diffraction system (Malvern Instruments Plc., Great Britain) is used to evaluate the volume-determined median particle size d 50 (vol) and the volume-determined top cut particle size d 98 (vol). The d 50 (vol) or d 98 (vol) value indicates the diameter value such that 50% or 98% of the particles by volume have a diameter less than this value. The raw data obtained by measurement is analyzed using Mie theory, where the particle refractive index is 1.57 and the absorption index is 0.005. The method and instrument are known to those skilled in the art and are commonly used to determine the particle size distribution of fillers and pigments.

[0305] BET specific surface area of the material

[0306] Throughout this document, the BET method well-known to those skilled in the art (using nitrogen as the adsorption gas) (ISO 9277:2010) is used to determine the specific surface area of mineral fillers (in m 2 / g). Then, the total surface area of the mineral filler (in m 2 ) is obtained by multiplying this specific surface area by the mass of the mineral filler (in g) before treatment.

[0307] Amount of surface treatment layer

[0308] Theoretically, the amount of treatment layer on the calcium carbonate-containing filler material is calculated from the BET value of the untreated calcium carbonate-containing filler material and the amount of the mixture of monosubstituted succinic anhydride and aliphatic linear or branched carboxylic acids including stearic acid used for surface treatment. It is assumed that 100% of the mixture of monosubstituted succinic anhydride and aliphatic linear or branched carboxylic acids including stearic acid added to the calcium carbonate-containing filler material exists as a surface treatment layer on the surface of the calcium carbonate-containing filler material.

[0309] Tensile test

[0310] The samples were tested according to ISO 3167 Type 1B and tensile tests were performed on 15 cm “dog bone shaped samples” according to ISO 527. The E modulus, tensile strength, and elongation at break tests were performed on a Zwick Roell Z020 machine according to ISO 527-3.

[0311] Melt Flow Index

[0312] The melt flow index was determined according to ISO 1133 (ASTM D1238) at 190°C and under loads of 5 kg or 10 kg respectively on a Ceast machine (IT), on a "melt flow modular line" type.

[0313] B) Example

[0314] a) Example 1

[0315] This embodiment relates to the preparation of a surface-treated filler material product according to the present invention.

[0316] To prepare a surface-treated filler material, Urgaon limestone was dry-milled in a horizontal ball mill. The resulting calcium carbonate-containing filler had d... 50 It is approximately 6.6 μm, with a top cut of d. 98 The residue on a 49.3 μm and 45 μm sieve was 1.4 wt.%, and the specific surface area (BET) was 1.1 m². 2 / g and the residual moisture content is 0.2wt.%.

[0317] The obtained spray-dried calcium carbonate-containing filler material was further processed as described in the following tests.

[0318] Test 1 (Reference Process)

[0319] Spray-dried calcium carbonate-containing filler minerals were continuously fed into a needle mill at a rate of 200 kg / h and subjected to a process at 100°C using materials manufactured by Hosokawa Alpine. TM (HOSOKAWA ALPINE TMA Contraplex 250 CW needle mill (250 mm disc diameter, 3000 rpm gate speed and 6000 rpm housing speed, with 120 needles in the gate and 120 needles in the housing, three rows) manufactured in Augsburg, Germany, was used to process a feed of liquid alkenyl succinic anhydride (“ASA”, Hydrores AS 1000, CAS No. 68784-12-3, commercially available from Kemira Oyj, Vaasa, Finnland) at a rate of 6 kg / h to achieve a surface finish of 0.3 wt.%.

[0320] Test 2 (based on the process according to the invention)

[0321] Spray-dried calcium carbonate-containing filler minerals are continuously fed at a rate of 750 kg / h through a 2.8 m long horizontal conveyor screw with a 4 m long screw and a 30° inclination angle. Liquid alkenyl succinic anhydride (“ASA”, Hydrores AS 1000, CAS No. 68784-12-3, commercially available from Kemira Chemicals AB, Vasa, Finland) is fed onto the horizontal conveyor screw at a rate of 22.5 kg / h at an ambient temperature of approximately 25°C. At the end of the inclined conveyor screw, a surface-treated calcium carbonate-containing filler material product with 0.3 wt.% surface treatment is allowed to fall into a hopper.

[0322] Before and after the reference treatment using a needle mill and the treatment according to the present invention, the particle size distribution of the feeds for Test 1 and Test 2 was analyzed using a Mastersizer 2000 from Malvern Instruments (UK) to determine the average particle size distribution d. 50 and top cut d 98 The residue on a 45 μm sieve, as measured according to ISO 787 / 7, is shown in Table 1.

[0323] Table 1

[0324]

[0325] As can be readily seen from Table 1, the particle size distribution of the calcium carbonate-containing mineral filler feed was significantly affected during surface treatment in the pin mill (Test 1). (Top shear value d) 98 The median particle size d is almost half of its initial value. 50 It increased by approximately 20%, and there was almost no residue at 45 μm. Compared to the surface-treated material according to the invention (Test 2), where the median particle size d 50It increased by only about 5%, and the top shear value increased slightly, possibly due to some small aggregates, while the residue was close to the value of the untreated feed material.

[0326] These results show that the surface treatment method according to the invention not only consumes less energy for its preparation, but also does not cause any significant changes in the physical properties of the feed material. Therefore, the surface-treated calcium carbonate mineral filler material product is almost identical to the feed material, except that it is surface-treated.

[0327] b) Example 2

[0328] The surface-treated calcium carbonate-containing filler material products used in Test 1 of Example 1 (i.e., Sample 1 was prepared according to the reference treatment) and Test 2 of Example 1 (i.e., Sample 2 was prepared according to the method of the present invention) were used.

[0329] Samples 1 and 2 were incorporated into the PVC-plasticized sol-gel flooring composition, and viscosity measurements were performed. Additionally, untreated calcium carbonate-containing filler material (feed) without a surface treatment agent (Sample 3) and untreated calcium carbonate-containing filler material (feed) with a separately added surface treatment agent (Sample 4) were added to the PVC-plasticized sol-gel flooring composition. Viscosity was measured using an Anton Paar (CH) MCR 300 rheometer according to the CC27 method system, with the following parameters: cylindrical system and spindle diameter 27 mm, spindle-cylinder clearance 1 mm, at 23°C, through 10 seconds... -1 At a shear rate of 1.) 120 seconds within 0-30 seconds -1 The upslope, 2.) 30 seconds -1 The duration is 60 seconds and 3.) within 120 seconds, 30-0 seconds. -1 The paste was pre-tempered for 5 minutes at a downward slope. Data analysis was based on the measured downward slope values ​​of part 3. Table 2 illustrates the composition of the PVC-plasticized sol-gel flooring.

[0330] Table 2

[0331]

[0332] *Diisononyl phthalate, CAS 68515-48-0, added as a plasticizer.

[0333] Figure 1The effects of particle size and surface treatment agent on the viscosity of PVC plastisol flooring compositions are shown. The surface-treated filler material product obtained by pin mill coating (reference) shows an increase in viscosity compared to untreated CaCO3. Viscosity is improved when alkenyl succinic anhydride is added directly to the PVC plastisol flooring composition. Optimal viscosity results are obtained when the surface-treated filler material product prepared according to the present invention is added to the PVC plastisol flooring composition.

[0334] c) Example 3

[0335] According to Example 1 of the present invention, test 2 prepared a surface-treated calcium carbonate-containing filler material product, wherein the surface treatment with ASA was 0.5 wt.%. Table 3 below describes the preparation of the sample in S-PVC.

[0336] Table 3

[0337]

[0338] *Diisononyl phthalate, CAS 68515-48-0, added as a plasticizer.

[0339] E1 is a reference material prepared using an uncoated calcium carbonate-containing filler material. E2 to E4 are materials of the present invention prepared using a surface-coated calcium carbonate-containing filler material product according to the present invention, wherein the surface-coated calcium carbonate-containing filler material product is added in different amounts.

[0340] The sample material was dry-mixed in a hot mixer (from Fa. Vorwerk, Germany) at 120°C and 6000-7000 rpm for 120 seconds, followed by two-roll milling at 170°C. Samples were cut from a pressing plate on a Collin hydraulic press (P300P model) for tensile testing. Hydraulic milling was performed on a 2mm thick metal frame (17cm × 17cm) using 200g of milling material. Pressing was carried out at 170°C and 200 bar for 2 minutes. The hydraulic press was then cooled at 15°C (water-cooled) while maintaining the pressure at 200 bar. Table 4 below presents the test results for the samples in S-PVC.

[0341] Table 4

[0342]

[0343] Cut specimens for tensile testing were prepared using a cutting apparatus from Fa. Hans Naef AG (CH). The specimens were of type 1B according to ISO 3167, and tensile tests were performed on 15 cm “dog bone shaped specimens” according to ISO 527. E modulus, tensile strength, and elongation at break tests were performed on a Zwick Roell Z020 model apparatus according to ISO 527-3.

[0344] Compared to the reference sample, embodiments E2 to E4 of the present invention show an overall increase in elongation at break, while in embodiment E3 of the present invention, the E modulus and tensile strength show maximum values.

[0345] d) Example 4

[0346] According to Test 2 of Example 1 of the present invention, a surface-treated calcium carbonate-containing filler material product was prepared, wherein the surface treatment with ASA was 0.5 wt.%. Table 5 below describes the preparation of samples in polyolefins.

[0347] Table 5

[0348]

[0349] *LLDPE (ExxonMobil, LLDPE LL 6101, MFI=20), **Elastomer (Dow, Engage 7270, MFI=0.8), #Mineral oil (paraffin oil, VWR Chemicals, viscosity: 69cSt); (1) PE compounding applications, (2) PE heavy lamination applications

[0350] The sample materials were composited, and the melt flow index was determined according to ISO 1133 (ASTM D1238) at 190°C and under loads of 5 kg or 10 kg on a Ceast machine (IT), a "melt flow modular line" type. Table 6 below presents the test results of the samples in polyolefins.

[0351] Table 6

[0352]

[0353] Surface-treated calcium carbonate mineral filler products exhibit improved or nearly similar melt flow indices at the same or increased filler levels.

[0354] e) Example 5

[0355] According to Test 2 of Example 1 of the present invention, a surface-treated calcium carbonate-containing filler material product was prepared, wherein the surface treatment with ASA was 0.5 wt.%. Table 7 below describes the preparation of the sample in S-PVC.

[0356] Table 7

[0357]

[0358] The sample material was dry-mixed in a hot mixer (from Vorwerk, Germany) at 120°C and 6000-7000 rpm for 120 seconds, followed by two-roll milling at 170°C. The dry mixture was then processed in a Haake mill. TM Further processing was performed on a Rheomix OS twin-helix kneader (Thermo Fisher Scientific) to evaluate the gelling behavior of the dry mix. Kneading conditions were 170°C and 30 rpm on two counter-rotating delta rotors. The dry mix volume in the kneading chamber was 85 g. Gelation, sometimes referred to as plasticizing, is generally understood as a process in which a lubricant, typically contained in a stabilizer, diffuses into the PVC resin particles during processing.

[0359] sample gelation time E10 (Reference) 96 seconds E11 (This invention) 66 seconds

[0360] ASA treatment showed a significant reduction in gelation time. This means that the output of the extrusion production line can be increased by using ASA-treated CaCO3.

Claims

1. A method for preparing a surface-treated filler material product, the method comprising at least the following steps: a) Provide at least one calcium carbonate-containing filler material, said at least one calcium carbonate-containing filler material having i) Bulk median particle size ranging from 5 µm to 100 µm d 50 value, ii) Top cuts ranging from 40 µm to 500 µm d 98 ,as well as iii) Based on the total weight of the calcium carbonate-containing packing material, the residue on a 45 µm sieve exceeding 0.5 wt.% as measured according to ISO 787 / 7. b) Provide at least one surface treatment agent that is in a molten or liquid state at a temperature ranging from 18°C ​​to 45°C. c) In one or more steps, the surface of the at least one calcium carbonate-containing filler material of step a) is brought into contact with the at least one surface treatment agent of step b) under mixing, such that a treatment layer comprising the at least one surface treatment agent and / or one or more reaction products thereof is formed on the surface of the at least one calcium carbonate-containing filler material of step a). The obtained surface-treated filler material product, based on the total weight of the surface-treated filler material product, has a residue on a 45 µm sieve greater than 0.5 wt.% as measured according to ISO 787 / 7. Contact step c) is performed in such a manner that the total energy intake does not exceed 15 kWh / T by adding at least one surface treatment agent from step b) to at least one calcium carbonate-containing filler material from step a). Contact step c) is carried out at a temperature between 18°C ​​and 45°C. Contact step c) is performed in an Archimedes screw device or a pneumatic air conveyor system, and In step b), the at least one surface treatment agent is a blend of one or more monophosphate esters and / or one or more diester phosphate esters, and / or at least one monosubstituted succinic anhydride, wherein the at least one monosubstituted succinic anhydride is composed of succinic anhydride, wherein the succinic anhydride is monosubstituted by a group selected from straight-chain, branched, and aliphatic or cyclic groups, wherein the total number of carbon atoms in the substituent of the straight-chain, branched, and aliphatic groups is at least C2 to C20, and the total number of carbon atoms in the substituent of the cyclic groups is at least C3 to C20.

2. The method according to claim 1, wherein the calcium carbonate-containing filler material in step a) is selected from the group consisting of: ground calcium carbonate, precipitated calcium carbonate (PCC), surface-reacted calcium carbonate (MCC), and mixtures thereof.

3. The method according to claim 1 or 2, wherein the at least one calcium carbonate-containing filler material in step a) has a) Bulk median particle size ranging from 6 µm to 80 µm d 50 value, b) Top cuts in the ranges of 40 µm and 400 µm d 98 ,as well as c) Residue on a 45 µm sieve, ranging from 0.5 wt.% to 30 wt.% based on the total weight of the calcium carbonate-containing filler material, as measured according to ISO 787 / 7.

4. The method according to claim 1 or 2, wherein the amount of residue on a 45 µm sieve of the at least one calcium carbonate-containing filler material in step a) as measured according to ISO 787 / 7 differs from the amount of residue on a 45 µm sieve of the surface-treated filler material product as measured according to ISO 787 / 7 by less than 20 wt.

5. The method according to claim 1 or 2, wherein the Brookfield viscosity of the at least one surface treatment agent in step b) is ≤1000 mPa at 25°C. s.

6. The method according to claim 1 or 2, wherein the at least one surface treatment agent in step b) is added to the contact step c) in a total amount of 0.1 wt.% to 3 wt.% based on the total dry weight of the at least one calcium carbonate-containing filler material in step a).

7. The method according to claim 1 or 2, wherein the contact step c) is performed in such a manner that the total energy intake is in the range of 2 kWh / T to 15 kWh / T by adding the at least one surface treatment agent of step b) to the at least one calcium carbonate-containing filler material of step a).

8. The method according to claim 1 or 2, wherein the Archimedes screw device is a screw conveyor.

9. The method of claim 8, wherein the Archimedes spiral device operates at an angle ranging from 30° to 80°.

10. The method of claim 8, wherein in the lower third of the Archimedes spiral device, the at least one surface treatment agent of step b) is added to the at least one calcium carbonate-containing filler material of step a).

11. The method according to claim 1 or 2, wherein the contact step c) is performed in such a manner that the at least one surface treatment agent of step b) is sprayed onto the at least one calcium carbonate-containing filler material of step a), and / or the contact step c) is performed in a continuous or batch processing mode.

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