Method for producing free-flowing granules

Abstract

The present invention relates to a method for producing granules comprising surface-reacted calcium carbonate, wherein the granules have a bulk density in the range of 0.25 to 0.70 g / mL, preferably 0.28 to 0.65 g / mL, more preferably 0.30 to 0.60 g / mL, and most preferably 0.35 to 0.60 g / mL, and to the use of the granules in dietary supplements, agricultural products, veterinary products, cosmetics, preferably cosmetic dry compositions and / or skin care dry compositions, household products, food products, packaging products, or personal care products, preferably oral care compositions, or as an excipient in pharmaceuticals.

Description

[Technical Field]

[0001] The present invention relates to a method for producing granules comprising surface-reacted calcium carbonate, wherein the granules have a bulk density in the range of 0.25 to 0.70 g / mL, preferably 0.28 to 0.65 g / mL, more preferably 0.30 to 0.60 g / mL, and most preferably 0.35 to 0.60 g / mL, and to the use of the granules in dietary supplements, agricultural products, veterinary products, cosmetics, preferably cosmetic dry compositions and / or skin care dry compositions, household products, food products, packaging products, or personal care products, preferably oral care compositions, or as an excipient in pharmaceuticals. [Background technology]

[0002] Granules are of considerable importance and are preferred to powders in many applications, such as pharmaceuticals, nutritional supplements, agricultural products, animal products, cosmetics, household products, foods, packaging products, and personal care products. Thus, granules resulting from powder agglomeration typically range in size from 0.2 to 4.0 mm, depending on their subsequent use, and are widely used to improve the physical properties of powders, such as wettability, flowability, bulk density, and product appearance.

[0003] Furthermore, granulation is carried out, for example, to prevent segregation of the constituents of a powder mixture, to prevent dusting, or to improve flowability.

[0004] Granulation, the process of adhering primary powder particles to form larger multi-particulate entities, is the process of holding multiple particles together by creating bonds between the particles, for example, by a binder.

[0005] One of the most important types of granulation is wet granulation, in which granules are formed by adding a granulation liquid onto a powder bed under the influence of an impeller. The agitation brought about by the system, along with the wetting of the ingredients in the formulation, leads to the aggregation of primary powder particles, producing wet granules. The granulation liquid contains a solvent, which must be volatile so that it can be removed by drying and non-toxic. Water mixed into the powder can form bonds between powder particles, which are strong enough to hold them together. However, once the water dries, the agglomerates may break apart. Therefore, the water may not be strong enough to create and maintain the bonds. In such cases, the granulation liquid contains a binder.

[0006] Granular forms of surface-reacted calcium carbonate are also commonly known. For example, European Patent Application Publication No. 2 264 108 A1 (WO 2010 / 146530 A1) mentions that the surface-reacted calcium carbonate obtained from the process described therein may be in the form of a cake, granules, or powder. Several documents also describe various uses of surface-reacted calcium carbonate, such as in water purification, as a controlled release carrier, in fast disintegrating dosage forms, or in gastroretentive drug formulations and delivery systems (EP 1 975 310 B1, EP 1 982 759 B1, EP 1 974 807 B1, EP 1 974 806 B1, EP 2 589 430 A1, WO 2010 / 037753 A1, EP 2 719 373 A1, or EP 2 719 376 A1), generally referring to granules.

[0007] However, these granules, either resulting from the basic process of producing surface-reacted calcium carbonate or obtained by (wet) granulation, have several drawbacks, such as poor bulk density, flow properties and compactability, as well as low mechanical stability. Furthermore, wet granulation requires the use of binders, which is not very beneficial.

[0008] Thus, although surface-reacted calcium carbonate can be granulated using various methods, conventional processes in the absence of a binder do not provide the desired results, i.e., high bulk density, flow properties and compressibility, as well as high mechanical stability.

[0009] It is therefore an object of the present invention to provide a method for producing granules comprising surface-reacted calcium carbonate which have high bulk density, flow properties and compactability, as well as high mechanical stability. A further object of the present invention is to improve the above-mentioned properties without the use of binders.

[0010] One or more of the above-mentioned and other objects are solved by the subject matter defined herein in the independent claims. Advantageous embodiments of the invention are defined in the corresponding dependent claims.

[0011] The present invention therefore relates to a method for producing granules comprising surface-reacted calcium carbonate, the method comprising the steps of: (a) providing an aqueous suspension comprising surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is the reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more acids, wherein the carbon dioxide is formed in situ by treatment with the acids and / or is provided from an external source; (b) homogenizing the aqueous suspension containing the surface-reacted calcium carbonate of step (a); and (c) removing the liquid from the aqueous suspension comprising surface-reacted calcium carbonate of step (b) by spray drying to obtain granules comprising surface-reacted calcium carbonate.

[0012] According to one embodiment, the natural ground calcium carbonate is selected from calcium carbonate containing minerals selected from the group comprising marble, chalk, limestone, and mixtures thereof; and the precipitated calcium carbonate is selected from the group comprising precipitated calcium carbonate having amorphous, aragonite, vaterite, or calcite mineralogical crystal forms, and mixtures thereof.

[0013] According to another embodiment, the surface-reacted calcium carbonate in the aqueous suspension of step (a) has: (a) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and particularly 1 to 10 μm 50 and / or (b) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area.

[0014] According to yet another embodiment, the aqueous suspension of step (a) has a solids content in the range of 1 to 40% by weight, preferably 5 to 35% by weight, most preferably 7 to 26% by weight, based on the total weight of the aqueous suspension.

[0015] According to one embodiment, at least one disintegrant is added before and / or during and / or after step (b), Preferably, the at least one disintegrant is selected from the group comprising croscarmellose sodium, modified cellulose gum, insoluble cross-linked polyvinylpyrrolidone, starch, modified starch, starch glycolates such as sodium starch glycolate, microcrystalline cellulose, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-, hydroxyalkyl-, carboxyalkyl-cellulose esters, alginic acid, microcrystalline cellulose and its polymorphs, ion exchange resins, gums, chitin, chitosan, clay, gellan gum, cross-linked polacrilin copolymer, agar, gelatin, dextrin, acrylic acid polymers, sodium / calcium carboxymethylcellulose, hydroxypropylmethylcellulose phthalate, shellac, effervescent mixtures such as hydrogen carbonate (bicarbonate) in combination with one or more acids such as citric acid or tartaric acid, and mixtures thereof.

[0016] According to another embodiment, at least one disintegrant is added before and / or during and / or after step (b) in an amount ranging from 0.3 to 10% by weight, preferably from 0.5 to 8% by weight, more preferably from 1 to 5% by weight, based on the total dry weight of the surface-reacted calcium carbonate.

[0017] According to yet another embodiment, the homogenization in step (b) is carried out one or more times, preferably 1 to 5 times, more preferably 1 to 3 times.

[0018] According to yet another embodiment, said homogenization in step (b) is carried out by milling.

[0019] According to one embodiment, the homogenization of step (b) is carried out with: (a) a pressure in the range of 5 to 90 MPa (50 to 900 bar), preferably 10 to 75 MPa (100 to 750 bar), most preferably 20 to 65 MPa (200 to 650 bar), and / or (b) an initial temperature in the range of 5 to 95°C, preferably 10 to 80°C, and most preferably 15 to 60°C.

[0020] According to another embodiment, the spray drying of step (c) is carried out with: (a) a pressure in the range of 0.01 to 30 MPa (0.1 to 300 bar), preferably 0.5 to 10 MPa (5 to 100 bar), more preferably 0.6 to <5 MPa (6 to <50 bar), most preferably 0.7 to 2.5 MPa (7 to 25 bar), and / or (b) A temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C.

[0021] According to a further aspect, the present invention provides granules comprising surface-reacted calcium carbonate, the surface-reacted calcium carbonate is the reaction product of natural ground or precipitated calcium carbonate with carbon dioxide and one or more acids, the carbon dioxide being formed in situ by treatment with the acids and / or supplied from an external source; The granules have a bulk density in the range of 0.25 to 0.70 g / mL, preferably 0.28 to 0.65 g / mL, more preferably 0.30 to 0.60 g / mL, and most preferably 0.35 to 0.60 g / mL.

[0022] According to one embodiment, the granules have: (a) a volume particle size d of 50 to 500 μm, preferably 60 to 400 μm, and most preferably 70 to 350 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar); 90 , (b) a volume median particle size d measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar) of 5 to 300 μm, preferably 10 to 200 μm, and most preferably 12 to 175 μm 50 , and (c) a volume particle size d of 1 to 100 μm, preferably 1 to 90 μm, and most preferably 1 to 80 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar); 10 and / or (d) Spherical.

[0023] According to another embodiment, the granules comprise particles of surface-reacted calcium carbonate having: (a) 1m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area, and / or (b) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and especially 1 to 10 μm 50 and / or (c) 0.15–1.60 cm calculated from mercury intrusion porosimetry measurements. 3 / g, preferably 0.30 to 1.50 cm 3 / g, more preferably 0.30 to 1.40 cm 3 / g, most preferably 0.30 to 1.35 cm 3 Intraparticle indented specific pore volume in the range of / g.

[0024] According to yet another embodiment, the granules comprise at least one disintegrant, Preferably, the at least one disintegrant is selected from the group comprising croscarmellose sodium, modified cellulose gum, insoluble cross-linked polyvinylpyrrolidone, starch, modified starch, starch glycolates such as sodium starch glycolate, microcrystalline cellulose, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-, hydroxyalkyl-, carboxyalkyl-cellulose esters, alginates, microcrystalline cellulose and its polymorphs, ion exchange resins, gums, chitin, chitosan, clay, gellan gum, cross-linked polacrilin copolymer, agar, gelatin, dextrin, acrylic acid polymers, sodium / calcium carboxymethylcellulose, hydroxypropylmethylcellulose phthalate, shellac, effervescent mixtures such as hydrogen carbonate (bicarbonate) in combination with one or more acids such as citric acid or tartaric acid, and mixtures thereof.

[0025] According to one embodiment, the granules comprise at least one disintegrant in an amount ranging from 0.25 to 35% by weight, preferably from 0.5 to 15% by weight, more preferably from 0.5 to 10% by weight, even more preferably from 0.7 to 10% by weight, and most preferably from 0.8 to 10% by weight, relative to the total dry weight of the granules.

[0026] According to another embodiment, the granules are obtained by the method defined herein.

[0027] According to another aspect, the present invention relates to the use of a granule as defined herein in a nutritional supplement product, an agricultural product, an animal product, a cosmetic, preferably a dry cosmetic composition and / or a dry skin care composition, a household product, a food product, a packaging product, or a personal care product, preferably an oral care composition, or as an excipient in a pharmaceutical product.

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

[0029] In the sense of this application, the term "surface reaction" refers to the reaction of a substance with HO in an aqueous environment. + It shall be used to indicate that the material has been subjected to a process which involves partially dissolving it by treatment with an ion donor (e.g., by use of a water-soluble free acid and / or acid salt), followed by a crystallization process which may occur in the absence or presence of further crystallization additives.

[0030] In the context of the present invention, "H3O + "Ion donors" are Bronsted acids and / or acid salts, ie, salts containing acidic hydrogen.

[0031] As used herein, the term "acid" refers to an acid within the meaning of the definition by Bronsted and Lowry (e.g., H2SO4, HSO4 - )

[0032] In the sense of the present invention, a "water-insoluble" substance is defined as a substance which, when mixed with deionized water and filtered at 20° C. on a filter having a pore size of 0.2 μm to recover the liquid filtrate, gives 0.1 g or less of recovered solid material after 100 g of said liquid filtrate is evaporated at 95-100° C. A "water-soluble" substance is defined as a substance which, when mixed with deionized water and filtered at 20° C. on a filter having a pore size of 0.2 μm to recover the liquid filtrate, gives 0.1 g or less of recovered solid material after 100 g of said liquid filtrate is evaporated at 95-100° C.

[0033] In the sense of the present invention, "natural ground calcium carbonate" (GCC) is calcium carbonate obtained from natural sources such as limestone, marble or chalk and processed by wet and / or dry processes such as grinding, screening and / or fractionation by means of a cyclone or classifier.

[0034] "Precipitated calcium carbonate" (PCC) in the sense of the present invention is a synthetic material obtained by precipitation following the reaction of carbon dioxide with lime in an aqueous, semi-arid, or humid environment, or by precipitation of a source of calcium and carbonate ions in water. PCC can be amorphous, vaterite, calcite, or aragonite crystalline forms.

[0035] The BET specific surface area in the sense of the present invention is defined as the surface area of ​​a particle divided by the mass of the particle. As used herein, the specific surface area is measured by adsorption using the BET isotherm (ISO 9277:2010) and is expressed as m 2 It is specified in / g.

[0036] Where the term "comprising" is used in the present specification and claims, it does not exclude other elements. For the purposes of the present invention, the term "consisting of" is considered to be a preferred embodiment of the term "comprising of". Hereinafter, when a group is defined to include at least a certain number of embodiments, this is to be understood as also disclosing a group that preferably consists only of these embodiments.

[0037] Where an indefinite or definite article is used when referring to a singular noun e.g. "a", "an" or "the", this includes a plural of that noun unless otherwise stated.

[0038] Terms such as "obtainable" or "defined" and "obtained" or "defined" are used interchangeably. For example, this does not mean that the term "obtained" indicates that, for example, an embodiment must be obtained by the sequence of steps that follows the term "obtained," unless the context clearly dictates otherwise, but that such a limited understanding is always included in the terms "obtained" or "defined," as a preferred embodiment.

[0039] According to the present invention, the method for producing granules comprising surface-reacted calcium carbonate must comprise the following steps: (a) providing an aqueous suspension comprising surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is the reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more acids, wherein the carbon dioxide is formed in situ by treatment with the acids and / or is provided from an external source; (b) homogenizing the aqueous suspension containing the surface-reacted calcium carbonate of step (a); and (c) removing the liquid from the aqueous suspension comprising surface-reacted calcium carbonate of step (b) by spray drying to obtain granules comprising surface-reacted calcium carbonate.

[0040] It has been found in particular that the process according to the invention must comprise a step of homogenizing the aqueous suspension comprising the surface-reacted calcium carbonate in order to obtain granules having high bulk density, flow properties and compactability, as well as high mechanical stability.

[0041] Reference is made below to further details of the invention and in particular to the above-described method for producing granules comprising surface-reacted calcium carbonate.

[0042] One aspect of the present invention is to provide an aqueous suspension comprising surface-reacted calcium carbonate according to step (a), wherein the surface-reacted calcium carbonate is the reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more acids, the carbon dioxide being formed in situ by acid treatment and / or supplied from an external source, preferably the carbon dioxide being formed in situ by acid treatment.

[0043] Surface-reacted calcium carbonate is a mixture of natural ground or precipitated calcium carbonate with carbon dioxide and one or more HO in an aqueous medium. + The carbon dioxide is a reaction product with an ion donor, where HO +The surface-reacted calcium carbonate is formed in situ by treatment with an ion donor and / or supplied from an external source. Preferably, the surface-reacted calcium carbonate is formed by treating natural ground or precipitated calcium carbonate with carbon dioxide and one or more HO in an aqueous medium. + The carbon dioxide is a reaction product with an ion donor, where HO + It is formed in situ by treatment with an ion donor or supplied from an external source. More preferably, the surface-reacted calcium carbonate is formed by treating natural ground or precipitated calcium carbonate with carbon dioxide and one or more HO in an aqueous medium. + The carbon dioxide is a reaction product with an ion donor, where HO + It is formed in situ by treatment with an ion donor.

[0044] HO in the context of the present invention + The ion donor is a Bronsted acid and / or an acid salt.

[0045] In a preferred embodiment of the present invention, the surface-reacted calcium carbonate is obtained by a process comprising the following steps: (a) providing a suspension of natural or precipitated calcium carbonate; (b) a pK of 0 or less at 20°C a1 or a pK value of 0 to 2.5 at 20°C a1 adding at least one acid having a value of 0.05 to the suspension of step (a); and (c) treating the suspension of step (a) with carbon dioxide before, during, or after step (b). According to another embodiment, the surface-reacted calcium carbonate is obtained by a process comprising the following steps: (A) providing natural or precipitated calcium carbonate; (B) providing at least one water-soluble acid; (C) providing CO2 gas; (D) contacting the natural or precipitated calcium carbonate of step (A) with at least one acid of step (B) and CO of step (C); wherein the method is characterized by: (i) at least one acid of step (B) has a pK, relative to the ionization of its first available hydrogen, greater than 2.5 and less than 7 at 20°C; a1 and the corresponding anion is formed upon loss of this first available hydrogen capable of producing a water-soluble calcium salt; and (ii) after contact of natural or precipitated calcium carbonate with at least one acid, the hydrogen-containing salt has a pK of greater than 7 at 20°C. a1 and if the salt anion is capable of forming a water-insoluble calcium salt, additionally providing at least one water-soluble salt.

[0046] "Natural ground calcium carbonate" (GCC) is preferably selected from calcium carbonate-containing minerals selected from the group including marble, chalk, limestone, and mixtures thereof. Natural ground calcium carbonate may contain additional naturally occurring components such as aluminosilicates.

[0047] Generally, the grinding of natural ground calcium carbonate can be a dry or wet grinding process and can be carried out in any conventional grinding equipment, for example, under conditions such that grinding is obtained primarily as a result of impact with secondary objects, i.e., in one or more of a ball mill, rod mill, vibratory mill, roll crusher, centrifugal impact mill, vertical bead mill, attrition mill, pin mill, hammer mill, crusher, shredder, declamper, knife cutter, or other such equipment known to those skilled in the art. When the calcium carbonate-containing mineral material comprises a wet-ground calcium carbonate-containing mineral material, the grinding process can be carried out under conditions such that autogenous grinding occurs and / or by horizontal and / or vertical ball mill grinding and / or by other such methods known to those skilled in the art. The wet-processed ground calcium carbonate-containing mineral material thus obtained can be washed and dewatered by known methods, for example, by flocculation, filtration, or forced evaporation, before drying. The subsequent drying step (if required) can be carried out in a one-stage process, such as spray drying, or in at least two stages. Such mineral materials also typically undergo a beneficiation process (flotation, bleaching, or magnetic separation) to remove impurities.

[0048] In the sense of the present invention, "precipitated calcium carbonate" (PCC) is a synthetic material generally obtained by precipitation after the reaction of carbon dioxide with calcium hydroxide in an aqueous environment, or by precipitation from a solution of calcium ions and carbonate ions provided in the form of soluble salts, for example, CaCl and NaCO. Further possible methods for producing PCC are the lime-soda process or the Solvay process, in which PCC is a by-product of ammonia production. Precipitated calcium carbonate exists in three primary crystalline forms: calcite, aragonite, and vaterite, with many different polymorphs (crystal habits) for each of these crystalline forms. Calcite has a trigonal structure with typical crystal habits such as scalenohedral (S-PCC), rhombohedral (R-PCC), hexagonal prismatic, tabletop, colloidal (C-PCC), cubic, and prismatic (P-PCC). Aragonite has an orthorhombic structure with a typical crystal habit of twinned hexagonal prisms, but also a structure with a varied assortment of thin, elongated prisms, curved blades, steeply sloped pyramids, chisel-like crystals, branched tree forms, and coral- or worm-like morphologies. Vaterite belongs to the hexagonal crystal system. The resulting PCC slurry can be mechanically dewatered and dried.

[0049] According to one embodiment of the present invention, the precipitated calcium carbonate is preferably amorphous, precipitated calcium carbonate comprising the mineralogical crystal forms of aragonite, vaterite, or calcite, or mixtures thereof.

[0050] The precipitated calcium carbonate is ground with carbon dioxide and at least one HO by the same means as used to grind the natural calcium carbonate described above. + It can be milled before treatment with the ion donor.

[0051] According to one embodiment of the present invention, the natural ground calcium carbonate or precipitated calcium carbonate has a weight median particle size d of 0.05 to 10.0 μm, preferably 0.2 to 5.0 μm, more preferably 0.4 to 3.0 μm, most preferably 0.6 to 1.2 μm, in particular 0.7 μm. 50According to a further embodiment of the present invention, the natural ground calcium carbonate or precipitated calcium carbonate is in the form of particles having a top cut particle size d of 0.15 to 55 μm, preferably 1 to 40 μm, more preferably 2 to 25 μm, most preferably 3 to 15 μm, in particular 4 μm. 98 The particle is in the form of a particle having the formula:

[0052] The natural ground calcium carbonate and / or precipitated calcium carbonate can be used in the dry state or suspended in water. Preferably, the corresponding slurry has a content of natural ground calcium carbonate or precipitated calcium carbonate in the range of 1% to 90% by weight, more preferably 3% to 60% by weight, even more preferably 5% to 40% by weight, and most preferably 10% to 25% by weight, based on the weight of the slurry.

[0053] One or more H3Os used in the production of surface-reacted calcium carbonate + The ion donor is HO under manufacturing conditions. + The acid may be any strong, medium or weak acid that generates ions, or a mixture thereof. + The ion donor is HO under manufacturing conditions. + It may also be an acid salt that generates ions.

[0054] According to one embodiment, at least one HO + The ion donor has a pK of 0 or less at 20°C. a1 It is a strong acid having the formula:

[0055] According to another embodiment, at least one HO + The ion donor has a pK of 0 to 2.5 at 20°C. a1 It is a medium-strength acid with a pK at 20°C a1 When pK at 20°C is 0 or less, the acid is preferably selected from sulfuric acid, hydrochloric acid, or a mixture thereof. a1 If is between 0 and 2.5, H3O +The ion donor is preferably selected from H2SO3, H3PO4, oxalic acid, or mixtures thereof. Also, at least one H3O + The ion donor is an acid salt, e.g., Li + , Na + Or K + HSO4 that is at least partially neutralized by the corresponding cation such as - or H2PO4 - , or Li + , Na + , K. + , Mg 2+ or Ca 2+ HPO4 that has been at least partially neutralized by the corresponding cation such as 2- At least one H3O + The ion donor may be a mixture of one or more acids and one or more acid salts.

[0056] According to yet another embodiment, at least one HO + The ion donor has a pK of greater than 2.5 and less than or equal to 7 when measured at 20°C. a1 value and have a corresponding anion capable of forming a water-soluble calcium salt. Subsequently, the hydrogen-containing salt has a pK greater than 7 when measured at 20°C. a1 and if the salt anion is capable of forming a water-insoluble calcium salt, then at least one water-soluble salt is additionally provided. According to a preferred embodiment, the weak acid has a pK of greater than 2.5 to 5 at 20°C. a1Preferably, the weak acid is selected from the group consisting of acetic acid, formic acid, propanoic acid, and mixtures thereof. Exemplary cations of the water-soluble salt are selected from the group consisting of potassium, sodium, lithium, and mixtures thereof. In a more preferred embodiment, the cation is sodium or potassium. Exemplary anions of the water-soluble salt are selected from the group consisting of phosphate, dihydrogen phosphate, monohydrogen phosphate, oxalate, silicate, mixtures thereof, and hydrates thereof. In a more preferred embodiment, the anion is selected from the group consisting of phosphate, dihydrogen phosphate, monohydrogen phosphate, mixtures thereof, and hydrates thereof. In a most preferred embodiment, the anion is selected from the group consisting of dihydrogen phosphate, monohydrogen phosphate, mixtures thereof, and hydrates thereof. The addition of the water-soluble salt can be carried out dropwise or in one step. In the case of dropwise addition, the addition is preferably carried out within a period of 10 minutes. It is more preferred to add the salt in one step.

[0057] According to one embodiment of the present invention, at least one HO + The ion donor is selected from the group consisting of hydrochloric acid, sulfuric acid, sulfurous acid, phosphoric acid, citric acid, oxalic acid, acetic acid, formic acid, and mixtures thereof. Preferably, at least one HO + Ion donors are hydrochloric acid, sulfuric acid, sulfurous acid, phosphoric acid, and oxalic acid; Li + , Na + or K + H2PO4 that is at least partially neutralized by the corresponding cation, such as - ;Li + , Na + , K. + , Mg 2+ or Ca 2+ HPO4 that has been at least partially neutralized by the corresponding cation such as 2- and mixtures thereof, more preferably the at least one acid is selected from the group consisting of hydrochloric acid, sulfuric acid, sulfurous acid, phosphoric acid, oxalic acid, and mixtures thereof, and most preferably at least one HO +The ion donor is phosphoric acid.

[0058] One or more H3O + The ion donor can be added to the suspension as a concentrated solution or as a more dilute solution. Preferably, HO for natural ground calcium carbonate or precipitated calcium carbonate. + The molar ratio of the ion donor is 0.01 to 4, more preferably 0.02 to 2, even more preferably 0.05 to 1, and most preferably 0.1 to 0.58.

[0059] Alternatively, natural ground calcium carbonate or precipitated calcium carbonate may be added to the suspension in water prior to suspending. + It is also possible to add an ion donor to the water.

[0060] In a preferred embodiment, the surface-reacted calcium carbonate is a mixture of natural ground calcium carbonate and carbon dioxide and one or more HO in an aqueous medium. + The carbon dioxide is a reaction product with an ion donor, where HO + Formed in situ by treatment with an ion donor and HO + In a more preferred embodiment, the surface-reacted calcium carbonate is prepared by reacting a calcium carbonate-containing mineral selected from the group consisting of marble, chalk, limestone, and mixtures thereof with carbon dioxide and one or more HO in an aqueous medium. + The reaction product with the ion donor, where carbon dioxide is H3O + Formed in situ by treatment with an ion donor and HO + The ion donor is phosphoric acid.

[0061] In the next step, the natural ground calcium carbonate or precipitated calcium carbonate is treated with carbon dioxide. A strong acid, such as sulfuric acid or hydrochloric acid, is added to the natural ground calcium carbonate or precipitated calcium carbonate. + When used for treatment with an ion donor, carbon dioxide is generated automatically. Alternatively or additionally, carbon dioxide can be supplied from an external source.

[0062] H3O + Treatment with the ion donor and treatment with carbon dioxide can be carried out simultaneously when using a strong or medium-strength acid. For example, an acid with a pK in the range of 0 to 2.5 at 20°C can be used. a1 First, H3O is used with a medium-strength acid + Treatment with an ion donor is also possible, where carbon dioxide is formed in situ, and thus treatment with carbon dioxide can be used to convert HO + This is done automatically in conjunction with treatment with the ion donor, followed by an additional treatment with carbon dioxide supplied from an external source.

[0063] In a preferred embodiment, HO + The ion donor treatment step and / or the carbon dioxide treatment step are repeated at least once, more preferably multiple times. + The ion donor is added over a period of at least about 5 minutes, preferably at least about 10 minutes, typically from about 10 minutes to about 20 minutes, more preferably about 30 minutes, even more preferably about 45 minutes, and sometimes about 1 hour or more.

[0064] H3O + After treatment with the ion donor and treatment with carbon dioxide, the pH of the aqueous suspension, measured at 20°C, spontaneously reaches a value above 6.0, preferably above 6.5, more preferably above 7.0, even more preferably above 7.5, thereby producing the surface-reacted natural or precipitated calcium carbonate as an aqueous suspension having a pH above 6.0, preferably above 6.5, more preferably above 7.0, even more preferably above 7.5.

[0065] Further details about the production of surface-reacted natural calcium carbonate are disclosed in WO 00 / 39222 A1, WO 2004 / 083316 A1, WO 2005 / 121257 A2, WO 2009 / 074492 A1, EP 2 264 108 A1, EP 2 264 109 A1, and U.S. 2004 / 0020410 A1, the contents of these references being incorporated herein by reference.

[0066] Similarly, surface-reacted precipitated calcium carbonate is obtained. As can be seen in detail from WO 2009 / 074492 A1, surface-reacted precipitated calcium carbonate is obtained by reacting precipitated calcium carbonate with HO. + The surface-reacted precipitated calcium carbonate is obtained by contacting, in an aqueous medium, an insoluble and at least partially crystalline calcium salt of said anion formed on the surface of at least a portion of the precipitated calcium carbonate, with an anion capable of being solubilized in the aqueous medium and producing a water-insoluble calcium salt thereof, to form a slurry of surface-reacted precipitated calcium carbonate, wherein the surface-reacted precipitated calcium carbonate comprises an insoluble and at least partially crystalline calcium salt of said anion formed on the surface of at least a portion of the precipitated calcium carbonate.

[0067] The solubilized calcium ions are dissolved in HO + corresponds to the excess solubilized calcium ions compared to the solubilized calcium ions naturally produced by dissolution of precipitated calcium carbonate by HO. + The ions are provided exclusively in the form of counterions to the anions, i.e., via addition of the anions in the form of acids or non-calcium salts, and in the absence of any further calcium ions or calcium ion generating sources.

[0068] The excess solubilized calcium ions are preferably provided by the addition of a soluble neutral or acidic calcium salt, or by the addition of an acid or a neutral or acidic non-calcium salt that generates a soluble neutral or acidic calcium salt in situ.

[0069] Above H3O + The ions may be provided by the addition of an acid or acid salt of the anion, or by the addition of an acid or acid salt which simultaneously acts to provide all or a portion of the excess solubilized calcium ions.

[0070] In a further preferred embodiment of the production of surface-reacted natural ground calcium carbonate or surface-reacted precipitated calcium carbonate, the natural ground calcium carbonate or precipitated calcium carbonate is reacted with acid and / or carbon dioxide in the presence of at least one compound selected from the group consisting of silicates, silica, aluminum hydroxide, alkaline earth aluminates such as sodium or potassium aluminate, or mixtures thereof. Preferably, the at least one silicate is selected from aluminum silicate, calcium silicate, or alkaline earth metal silicates. These components can be added to the aqueous suspension comprising the natural ground calcium carbonate or precipitated calcium carbonate before the addition of the acid and / or carbon dioxide.

[0071] Alternatively, one or more components of silicate and / or silica and / or aluminium hydroxide and / or alkaline earth aluminate can be added to an aqueous suspension of natural or precipitated calcium carbonate, while the reaction of the natural or precipitated calcium carbonate with acid and carbon dioxide has already begun. Further details about the production of surface-reacted natural or precipitated calcium carbonate in the presence of at least one component of silicate and / or silica and / or aluminium hydroxide and / or alkaline earth aluminate are disclosed in WO 2004 / 083316 A1, the content of which reference is incorporated herein by reference.

[0072] The surface-reacted calcium carbonate can be kept in suspension and optionally further stabilized by a dispersing agent. Conventional dispersing agents known to those skilled in the art can be used. Preferred dispersing agents consist of polyacrylic acid and / or carboxymethylcellulose.

[0073] Alternatively, the aqueous suspension can be dried, thereby obtaining solid (i.e., dry or substantially free of water that is not in fluid form) surface-reacted natural ground calcium carbonate or surface-reacted precipitated calcium carbonate in the form of granules or powder.

[0074] In a preferred embodiment, the surface-reacted calcium carbonate has a surface-reacted viscosity of 1 m 2 as measured using nitrogen and the BET method according to ISO 9277:2010. 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area.

[0075] The surface-reacted calcium carbonate particles have a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, especially 1 to 10 μm. 50 (or d 50 It is even more preferred that the hydroxyl group has a hydroxyl group (vol)).

[0076] According to an exemplary embodiment, the surface-reacted calcium carbonate has: (a) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and particularly 1 to 10 μm 50 and / or (b) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area.

[0077] Preferably, the surface-reacted calcium carbonate has: (a) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and particularly 1 to 10 μm 50 , or (b) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area.

[0078] Preferably, the surface-reacted calcium carbonate has: (a) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and particularly 1 to 10 μm 50 , and (b) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area.

[0079] The surface-reacted calcium carbonate particles have a volume particle size d of 2 to 150 μm, preferably 4 to 100 μm, more preferably 6 to 80 μm, even more preferably 8 to 60 μm, and most preferably 10 to 30 μm. 98 (or d 98 It is even more preferred that the hydroxyl group has a hydroxyl group (vol)).

[0080] Value dx is the x% of particles x This refers to the diameter of the 98 The value indicates that 98% by weight of all particles have a particle size smaller than this value. 98 The value is also called the "top cut." x The value can be given as a volume percentage or a weight percentage. 50 The (wt) value is the weight median particle size, i.e., 50% by weight of all particles are smaller than this particle size, and d 50 The (vol) value is the volume median particle size, i.e. 50% by volume of all particles are smaller than this particle size.

[0081] The "particle size" of the surface-reacted calcium carbonate in this specification is described as a particle size distribution based on volume. The "particle size" of the granules in this specification is described as a particle size distribution based on volume. Furthermore, the "particle size" of the surface-reacted calcium carbonate in the sense of the present invention refers to the primary particle size.

[0082] Volume median particle size d 50 was evaluated using a Malvern Mastersizer 2000 or 3000 laser diffraction system. 10 , d 50 , or d 98 The values ​​indicate the diameter values ​​such that 10%, 50%, or 98% by volume of the particles have a diameter smaller than this value, respectively. The raw data obtained from the measurements are analyzed using Mie theory with a particle refractive index of 1.57 and an absorption coefficient of 0.005.

[0083] Throughout the present invention, the volumetric particle size distribution is determined by laser diffraction. For example, the volumetric particle size distribution of granules is measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar), as described in detail in the examples herein below.

[0084] Preferably, the surface-reacted calcium carbonate has a porosity of 0.15 to 1.60 cm as calculated from mercury intrusion porosimetry measurements. 3 / g, preferably 0.30 to 1.50 cm 3 / g, more preferably 0.30 to 1.40 cm 3 / g, most preferably 0.30 to 1.35 cm 3 / g.

[0085] Specific pore volume is measured using mercury intrusion porosimetry using a Micromeritics Autopore V 9620 mercury porosimeter with a maximum applied pressure of 414 MPa (60,000 psi), equivalent to a Laplace throat diameter of 0.004 μm (~nm). An equilibration time of 20 seconds is used for each pressure step. Sample material is then loaded onto a 5 cm 3 The chamber is sealed in a powder penetrometer. Data are corrected for mercury compression, penetrometer expansion, and sample material compression using the software Pore-Comp (Gane, PAC, Kettle, JP, Matthews, GP, and Ridgway, CJ, "Void Space Structure of Compressible Polymer Spheres and Consolidated Calcium Carbonate Paper-Coating Formulations", Industrial and Engineering Chemistry Research, 35(5), 1996, pp. 1753-1764).

[0086] The total pore volume seen in the integrated intrusion data can be separated into two regions with intrusion data ranging from 214 μm down to approximately 1-4 μm, indicating a strong contribution from coarse packing of the sample between any aggregate structures. Below these diameters, there is fine interparticle packing of the particles themselves. If the particles also contain intraparticle pores, this region is bimodal, and the intraparticle specific pore volume is defined as the specific pore volume of mercury intruded into pores narrower than the inflection point of the bimodal transition. The sum of these three regions gives the total pore volume of the powder, but is heavily influenced by the precipitation of powder at the coarse pore end of the original sample compaction / distribution.

[0087] Taking the first derivative of the cumulative penetration curve reveals a pore size distribution based on the equivalent Laplace diameter, which necessarily includes pore blocking. The derivative curve clearly shows the coarse aggregate pore structure region, the interparticle pore region, and, if present, the intraparticle pore region. Once the intraparticle pore size range is known, it is possible to subtract the remaining interparticle and interaggregate pore volumes from the total pore volume to obtain only the desired pore volume of the internal pores as pore volume per unit mass (specific pore volume). Of course, the same subtraction principle applies to isolating any other pore size region of interest.

[0088] Preferably, the intraparticle pore size of the surface-reacted calcium carbonate is in the range of 0.004 to 1.6 μm, more preferably 0.005 to 1.3 μm, particularly preferably 0.006 to 1.15 μm, and most preferably 0.007 to 1.0 μm, as determined by mercury porosimetry.

[0089] The surface-reacted calcium carbonate comprises a water-insoluble, at least partially crystalline calcium salt of at least one acid anion, which salt is formed on the surface of natural ground calcium carbonate or precipitated calcium carbonate. According to one embodiment, the water-insoluble, at least partially crystalline salt of at least one acid anion at least partially, preferably completely, covers the surface of the natural ground calcium carbonate or precipitated calcium carbonate. Depending on the at least one acid used, the anion may be sulfate, sulfite, phosphate, citrate, oxalate, acetate, formate, and / or chloride.

[0090] As mentioned above, the surface-reacted calcium carbonate is provided in the form of an aqueous suspension.

[0091] Preferably, the aqueous suspension of step (a) has a solids content in the range of 1 to 40% by weight, preferably 5 to 35% by weight, most preferably 7 to 26% by weight, based on the total weight of the aqueous suspension.

[0092] For the purposes of the present invention, a "suspension" or "slurry" refers to a system comprising a liquid, i.e., an aqueous solvent, and particles of surface-reacted calcium carbonate, wherein the particles of surface-reacted calcium carbonate exist as a solid in the liquid. The aqueous suspension may be more viscous and denser than the liquid from which it is formed.

[0093] The "liquid" is typically an "aqueous solvent," but does not exclude that the aqueous solvent contains a small amount of at least one water-miscible solvent. For example, the at least one water-miscible solvent is preferably selected from methanol, ethanol, acetone, acetonitrile, tetrahydrofuran, and mixtures thereof. In one embodiment of the present invention, the liquid contains water in an amount of at least 80% by weight, preferably at least 90% by weight, more preferably at least 95% by weight, and even more preferably at least 99% by weight, based on the total weight of the aqueous solvent. Preferably, the aqueous solvent consists of water, i.e., the amount of water is 100% by weight, based on the total weight of the liquid.

[0094] It is further preferred that the aqueous suspension provided in step (a) has a Brookfield viscosity at 100 rpm of 25 to 1000 mPa·s at a temperature of +23°C (±2°C), preferably 25 to 700 mPa·s at +23°C (±2°C), more preferably 25 to 500 mPa·s at +23°C (±2°C), and most preferably 50 to 300 mPa·s at +23°C (±2°C).

[0095] According to step (b) of the method of the present invention, the aqueous suspension comprising the surface-reacted calcium carbonate of step (a) is homogenized.

[0096] "Homogenization" in the sense of the present invention refers to a step which leads the particles of surface-reacted calcium carbonate in aqueous suspension of step (a) to form stronger agglomerates after drying in terms of particle stability.

[0097] Homogenization can be carried out by using a variety of methods well known in the art.

[0098] The homogenizing device can be selected from those conventionally used for homogenization purposes. Thus, the homogenizing device can be selected from the group including piston pumps, high shear devices, etc. For example, a GEA Ariete NS3055 from GEA Mechanical Equipment Italia SpA can be used for homogenization in step (b).

[0099] Alternatively, the homogenization in step (b) is carried out by milling. The homogenization in step (b) can be carried out using a milling or kneading device known in the art. Therefore, the milling or kneading device can be selected from horizontal and vertical mills conventionally used for milling purposes, or kneaders conventionally used for kneading purposes. For example, the milling device can be selected from horizontal and / or vertical stirred media mills, preferably vertical stirred media mills, horizontal and / or vertical stirred bead mills, such as Dyno-KDL bead mills, Netzsch LabStar or LMZ-type mills, or LME-type mills; sand mills, etc. For example, the kneading device can be selected from Sigma-Kneader, planetary mixers, etc.

[0100] It should be noted that depending on the method used, there may be differences as to the particle size distribution to be achieved.

[0101] The homogenization in step (b) may be carried out once or several times. It is understood that the number of times step (b) is carried out mainly depends on the pressure used and the surface-reacted calcium carbonate particles obtained in step (b). Therefore, a person skilled in the art can easily adapt the number of times for carrying out step (b) according to the equipment or conditions used during step (b). Therefore, the homogenization in step (b) may be carried out in a recirculation mode.

[0102] Preferably, the homogenization in step (b) is carried out 1 to 5 times, more preferably 1 to 3 times, i.e., 1, 2, or 3 times, even more preferably 1 or 2 times. Most preferably, the homogenization in step (b) is carried out 2 times.

[0103] It is understood that the homogenization in step (b) is preferably carried out by using a high-pressure homogenizer.

[0104] In one embodiment, the homogenization in step (b) is carried out at a pressure in the range of 5 to 90 MPa (50 to 900 bar), preferably 10 to 75 MPa (100 to 750 bar), most preferably 20 to 65 MPa (200 to 650 bar).

[0105] Additionally or alternatively, the homogenization in step (b) is carried out at an initial temperature in the range of 5 to 95°C, preferably 10 to 80°C, most preferably 15 to 60°C.

[0106] It is therefore preferred that the homogenization in step (b) is carried out with: (a) a pressure in the range of 5 to 90 MPa (50 to 900 bar), preferably 10 to 75 MPa (100 to 750 bar), most preferably 20 to 65 MPa (200 to 650 bar), or (b) an initial temperature in the range of 5 to 95°C, preferably 10 to 80°C, and most preferably 15 to 60°C.

[0107] More preferably, the homogenization in step (b) is carried out with: (a) a pressure in the range of 5 to 90 MPa (50 to 900 bar), preferably 10 to 75 MPa (100 to 750 bar), most preferably 20 to 65 MPa (200 to 650 bar), and (b) an initial temperature in the range of 5 to 95°C, preferably 10 to 80°C, and most preferably 15 to 60°C.

[0108] Preferably, the aqueous suspension in step (b) has a solids content in the range of 1 to 40% by weight, preferably 5 to 35% by weight, most preferably 7 to 26% by weight, based on the total weight of the aqueous suspension.

[0109] It is understood that homogenization in step (b) can result in an increase in the solids content of the aqueous suspension compared to the aqueous suspension subjected to step (b). For example, the aqueous suspension obtained in homogenization step (b) can have a solids content that is at least 1%, more preferably at least 2%, and most preferably at least 3%, e.g., 3-4%, higher than the solids content of the aqueous suspension subjected to step (b). This is particularly true when step (b) is carried out in a homogenizer.

[0110] When step (b) is carried out by milling, it is preferred that the aqueous suspension obtained in homogenization step (b) has a solids content that is at most 3%, more preferably at most 2%, and most preferably at most 1% higher than the solids content of the aqueous suspension subjected to step (b).

[0111] It is understood that the homogenization by milling is preferably carried out at a specific energy in the range of 25 to 125 kWh / tonne of dry product, preferably 35 to 100 kWh / tonne of dry product.

[0112] Additionally or alternatively, homogenization by milling is carried out at an initial temperature in the range of 5 to 95°C, preferably 10 to 80°C, most preferably 15 to 60°C.

[0113] It is therefore preferred that the homogenization by milling in step (b) is carried out with: (c) a specific energy in the range of 25 to 125 kWh per tonne of dry product, preferably 35 to 100 kWh per tonne of dry product; or (d) an initial temperature in the range of 5 to 95°C, preferably 10 to 80°C, and most preferably 15 to 60°C.

[0114] More preferably, the homogenization by milling in step (b) is carried out with: (c) a specific energy in the range of 25 to 125 kWh per tonne of dry product, preferably 35 to 100 kWh per tonne of dry product; and (d) an initial temperature in the range of 5 to 95°C, preferably 10 to 80°C, and most preferably 15 to 60°C.

[0115] In one embodiment, at least one disintegrant is added before, during, and / or after step (b). Preferably, at least one disintegrant is added before, during, or after step (b), more preferably before or after step (b). Most preferably, at least one disintegrant is added after step (b).

[0116] In one embodiment of the present invention, the at least one disintegrant comprises one disintegrant, preferably consists of one disintegrant. Alternatively, the at least one disintegrant comprises two or more disintegrants, preferably consists of two or more disintegrants. For example, the at least one disintegrant comprises two or three disintegrants, preferably consists of two or three disintegrants.

[0117] Preferably, the at least one disintegrant comprises, preferably consists of, one disintegrant.

[0118] It should be noted that the disintegrant(s) that can be used in the method of the present invention are generally well known in the art of granulation.

[0119] It should be noted that any compound known to be or capable of acting as a disintegrant can be used in the methods of the present invention.

[0120] In a preferred embodiment, the at least one disintegrant is selected from the group consisting of croscarmellose sodium, modified cellulose gum, insoluble cross-linked polyvinylpyrrolidone, starch, modified starch, starch glycolates such as sodium starch glycolate, microcrystalline cellulose, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-, hydroxyalkyl-, and carboxyalkyl-cellulose esters, alginic acid, microcrystalline cellulose and its polymorphs, ion exchange resins, gums, chitin, chitosan, clay, gellan gum, cross-linked polacrilin copolymer, agar, gelatin, dextrin, acrylic acid polymers, sodium / calcium carboxymethylcellulose, hydroxypropylmethylcellulose phthalate, shellac, effervescent mixtures such as bicarbonate salts in combination with one or more acids, such as citric acid or tartaric acid, and mixtures thereof. Preferably, the at least one disintegrant is croscarmellose sodium. The at least one disintegrant may also be a superdisintegrant. The superdisintegrant(s) that can be used in the methods of the present invention are generally known in the art. Exemplary superdisintegrants include, but are not limited to, croscarmellose sodium, insoluble cross-linked polyvinylpyrrolidone, sodium starch glycolate, and mixtures thereof.

[0121] When at least one disintegrant is added before and / or during and / or after step (b), the at least one disintegrant is preferably added in an amount in the range of 0.3 to 10 wt. %, preferably 0.5 to 8 wt. %, more preferably 0.8 to about 5 wt. %, and most preferably 1 to about 5 wt. %, based on the total dry weight of the surface-reacted calcium carbonate.

[0122] The at least one disintegrant can be added in dry form or in the form of an emulsion, dispersion, or solution.

[0123] Thus, in one embodiment, a method for producing granules comprising surface-reacted calcium carbonate comprises the steps of: (a) providing an aqueous suspension comprising surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is the reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more acids, wherein the carbon dioxide is formed in situ by treatment with the acid and / or is provided from an external source, preferably wherein the carbon dioxide is formed in situ by treatment with the acid; (b) homogenizing the aqueous suspension containing the surface-reacted calcium carbonate of step (a); (c) removing the liquid from the aqueous suspension comprising surface-reacted calcium carbonate of step (b) by spray drying to obtain granules comprising surface-reacted calcium carbonate; and (d) adding at least one disintegrant to the aqueous suspension before, during, and / or after step (b).

[0124] Alternatively, the method may comprise a step (d) of mechanically and / or physically disintegrating the aqueous suspension comprising the surface-reacted calcium carbonate before, during and / or after step (b).

[0125] Such mechanical and / or physical disruption can be carried out by any method known to those skilled in the art as suitable for such purposes, for example, the mechanical and / or physical disruption step (d) can be carried out by an ultrasound probe, etc.

[0126] Thus, in one embodiment, a method for producing granules comprising surface-reacted calcium carbonate comprises the steps of: (a) providing an aqueous suspension comprising surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is the reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more acids, wherein the carbon dioxide is formed in situ by treatment with the acid and / or is provided from an external source, preferably wherein the carbon dioxide is formed in situ by treatment with the acid; (b) homogenizing the aqueous suspension containing the surface-reacted calcium carbonate of step (a); (c) removing the liquid from the aqueous suspension comprising surface-reacted calcium carbonate of step (b) by spray drying to obtain granules comprising surface-reacted calcium carbonate; and (d) mechanically and / or physically disintegrating the aqueous suspension comprising the surface-reacted calcium carbonate before, during, and / or after step (b).

[0127] It is understood that further additives suitable for improving mouthfeel, palatability or controlled release, such as mannitol, carboxymethylcellulose or ground calcium carbonate (GCC), can be added before and / or during and / or after step (b), preferably before or after step (b), most preferably after step (b).

[0128] When such additives are added, they are preferably added in an amount ranging from 0.3 to 40% by weight, preferably from 0.5 to 30% by weight, more preferably from 1 to about 25% by weight, based on the total dry weight of the surface-reacted calcium carbonate.

[0129] According to step (c) of the present invention, the liquid is removed from the aqueous suspension comprising the surface-reacted calcium carbonate of step (b) by spray drying to obtain granules comprising the surface-reacted calcium carbonate.

[0130] The spray-drying device can be selected from those conventionally used for spray-drying purposes. Thus, the spray dryer can be selected from the group including a rotary atomizer, a fountain nozzle, a two-fluid nozzle, a pressure nozzle, a combi-nozzle, etc. Preferably, the spray-drying step (c) is carried out by using a rotary atomizer or a two-fluid nozzle. When the homogenization step (b) is carried out by attrition, the spray dryer can be selected from those conventionally used for spray-drying, for example, the spray dryer can be selected from the group including a rotary atomizer, a fountain nozzle, a two-fluid nozzle, a pressure nozzle, a combi-nozzle, etc. It should be noted that the fountain nozzle can also be called a pressure nozzle, which is operated in a fountain (or co-current) mode. In one embodiment, the homogenization step (b) is carried out by attrition, and the spray-drying step (c) is carried out by using a rotary atomizer. It is understood that different conditions are set for different spray-drying techniques to achieve the desired granules. However, a person skilled in the art knows how to adapt such conditions for different spray-drying techniques.

[0131] For example, when using a pressure nozzle, the spray drying in step (c) is carried out by: (a) a supply pressure in the range of 0.01 to 30 MPa (0.1 to 300 bar), preferably 0.5 to 10 MPa (5 to 100 bar), more preferably 0.6 to <5 MPa (6 to <50 bar), and most preferably 0.7 to 2.5 MPa (7 to 25 bar); and / or (b) A temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C.

[0132] In one embodiment, when a pressure nozzle is used, the spray drying in step (c) is carried out by: (a) a supply pressure in the range of 0.01 to 30 MPa (0.1 to 300 bar), preferably 0.5 to 10 MPa (5 to 100 bar), more preferably 0.6 to <5 MPa (6 to <50 bar), and most preferably 0.7 to 2.5 MPa (7 to 25 bar); or (b) A temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C.

[0133] Preferably, when using a pressure nozzle, the spray drying in step (c) is carried out by: (a) a supply pressure in the range of 0.01 to 30 MPa (0.1 to 300 bar), preferably 0.5 to 10 MPa (5 to 100 bar), more preferably 0.6 to <5 MPa (6 to <50 bar), and most preferably 0.7 to 2.5 MPa (7 to 25 bar); and (b) A temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C.

[0134] In one embodiment, when a two-fluid nozzle is used, the spray drying in step (c) is carried out with: (a) a supply pressure in the range of 0.01 to 30 MPa (0.1 to 300 bar), preferably 0.5 to 10 MPa (5 to 100 bar), more preferably 0.6 to <5 MPa (6 to <50 bar), and most preferably 0.7 to 2.5 MPa (7 to 25 bar); and / or (b) an orifice diameter in the range of 0.8 to 1.8 mm, preferably 0.9 to 1.6 mm, and most preferably 1.05 to 1.5 mm; and / or (c) a temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C; and / or (d) an air pressure to the nozzle of 0.1 to 0.7 MPa (1 to 7 bar), preferably 0.15 to 0.65 MPa (1.5 to 6.5 bar), most preferably 0.2 to 0.6 MPa (2 to 6 bar).

[0135] For example, when using a two-fluid nozzle, the spray drying in step (c) is carried out by: (a) a supply pressure in the range of 0.01 to 30 MPa (0.1 to 300 bar), preferably 0.5 to 10 MPa (5 to 100 bar), more preferably 0.6 to <5 MPa (6 to <50 bar), and most preferably 0.7 to 2.5 MPa (7 to 25 bar); or (b) an orifice diameter in the range of 0.8 to 1.8 mm, preferably 0.9 to 1.6 mm, and most preferably 1.05 to 1.5 mm; or (c) a temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C; or (d) an air pressure to the nozzle of 0.1 to 0.7 MPa (1 to 7 bar), preferably 0.15 to 0.65 MPa (1.5 to 6.5 bar), most preferably 0.2 to 0.6 MPa (2 to 6 bar).

[0136] Alternatively, when a two-fluid nozzle is used, the spray drying in step (c) is carried out by: (a) a supply pressure in the range of 0.01 to 30 MPa (0.1 to 300 bar), preferably 0.5 to 10 MPa (5 to 100 bar), more preferably 0.6 to <5 MPa (6 to <50 bar), and most preferably 0.7 to 2.5 MPa (7 to 25 bar); and (b) an orifice diameter in the range of 0.8 to 1.8 mm, preferably 0.9 to 1.6 mm, and most preferably 1.05 to 1.5 mm; and (c) a temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C; and (d) an air pressure to the nozzle of 0.1 to 0.7 MPa (1 to 7 bar), preferably 0.15 to 0.65 MPa (1.5 to 6.5 bar), most preferably 0.2 to 0.6 MPa (2 to 6 bar).

[0137] It will be understood that two-fluid nozzles are well known in the art and include, for example, the combi-nozzle from GEA-Niro of Denmark.

[0138] In one embodiment, when a rotary atomizer is used, the spray drying in step (c) is carried out by: (a) a supply pressure in the range of 0.05 to 0.8 MPa (0.5 to 8 bar), preferably 0.1 to 0.65 MPa (1 to 6.5 bar), most preferably 0.2 to 0.45 MPa (2 to 4.5 bar), and / or (b) a rotation wheel speed of ≦11000, preferably 8000-11000 rpm, more preferably 9000-10000 rpm (wheel diameter d=150 mm and / or speed 73 m / s), and / or (c) A temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C.

[0139] For example, when using a rotary atomizer, the spray drying in step (c) is carried out by: (a) a supply pressure in the range of 0.05 to 0.8 MPa (0.5 to 8 bar), preferably 0.1 to 0.65 MPa (1 to 6.5 bar), and most preferably 0.2 to 0.45 MPa (2 to 4.5 bar); or (b) a rotation wheel speed of ≦11000, preferably 8000 to 11000 rpm, more preferably 9000 to 10000 rpm (wheel diameter d=150 mm and / or speed 73 m / s), or (c) A temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C.

[0140] Alternatively, when using a rotary atomizer, the spray drying in step (c) is carried out by: (a) a supply pressure in the range of 0.05 to 0.8 MPa (0.5 to 8 bar), preferably 0.1 to 0.655 MPa (1 to 6.55 bar), and most preferably 0.2 to 0.45 MPa (2 to 4.5 bar); and (b) a rotation wheel speed of ≦11000, preferably 8000 to 11000 rpm, more preferably 9000 to 10000 rpm (wheel diameter d=150 mm and / or speed 73 m / s), and (c) A temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C.

[0141] In one embodiment, when using a fountain nozzle, the spray drying in step (c) is carried out with: (a) a supply pressure in the range of 0.8 to 6 MPa (8 to 60 bar), preferably 1.0 to 2.5 MPa (10 to 25 bar), most preferably 1.1 to 1.8 MPa (11 to 18 bar), and / or (b) A temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C.

[0142] For example, when using a fountain nozzle, the spray drying in step (c) is carried out with: (a) a supply pressure in the range of 0.8 to 6 MPa (8 to 60 bar), preferably 1.0 to 2.5 MPa (10 to 25 bar), most preferably 1.1 to 1.8 MPa (11 to 18 bar); or (b) A temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C.

[0143] Alternatively, when using a fountain nozzle, the spray drying in step (c) is carried out with: (a) a supply pressure in the range of 0.8 to 6 MPa (8 to 60 bar), preferably 1.0 to 2.5 MPa (10 to 25 bar), and most preferably 1.1 to 1.8 MPa (11 to 18 bar); and (b) A temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C.

[0144] The granules obtained in step (c) are preferably in dry form, i.e. in free-flowing form.

[0145] The term "dry" granules is understood to mean materials having less than 4% by weight of water relative to the granule weight. The percentage of water can be measured by heating the granules to 105°C in a drying chamber using a method according to ISO 787-2.

[0146] The granules obtained by the process of the present invention have a preferred bulk density. Thus, in another aspect, the present invention relates to granules comprising surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is the reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more acids, wherein the carbon dioxide is formed in situ by acid treatment and / or is provided from an external source, the granules having a bulk density in the range of 0.25 to 0.70 g / mL. Preferably, the granules comprise surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is the reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more acids, wherein the carbon dioxide is formed in situ by acid treatment, the granules having a bulk density in the range of 0.25 to 0.70 g / mL.

[0147] For example, the granules have a bulk density in the range of 0.28 to 0.65 g / mL, more preferably 0.30 to 0.60 g / mL, and most preferably 0.35 to 0.60 g / mL.

[0148] It will be appreciated that the granules preferably have a very specific particle size distribution which can be adjusted depending on the process used.

[0149] In particular, the granules have: (a) Volume particle size d of 50–500 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 90 , (b) Volume median particle size d between 5 and 300 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 50 , and (c) Volume particle size d of 1 to 100 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 10 .

[0150] Preferably, the granules have: (a) Volume particle size d of 60–400 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 90 , (b) Volume median particle size d between 10 and 200 μm measured in the dry state at a dispersion pressure of 0.01 MPa (0.1 bar) by laser diffraction 50 , and (c) Volume particle size d of 1 to 90 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 10 .

[0151] Most preferably, the granules have: (a) Volume particle size d of 70 to 350 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 90 , (b) Volume median particle size d of 12 to 175 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 50 , and (c) Volume particle size d of 1 to 80 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 10 .

[0152] In one embodiment, particularly when step (b) is carried out in a homogenizer, the granules have: (d) Volume particle size d of 50-500 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 90 , (e) Volume median particle size d between 20 and 300 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 50 , and (f) Volume particle size d of 2 to 100 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 10 .

[0153] Preferably, the granules have: (d) Volume particle size d of 60 to 400 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 90 , (e) Volume median particle size d of 30–200 μm measured in the dry state at a dispersion pressure of 0.01 MPa (0.1 bar) by laser diffraction 50 , and (f) Volume particle size d of 3 to 90 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 10 .

[0154] Most preferably, the granules have: (d) Volume particle size d of 70 to 350 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 90 , (e) Volume median particle size d of 50–175 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 50 , and (f) Volume particle size d of 10 to 80 μm measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar). 10 .

[0155] Additionally or alternatively, the granules have a spherical shape. "Spherical" in the sense of the present invention refers to granules that have approximately the same diameter on all axes in three-dimensional space.

[0156] Thus, the granules preferably have: (a) a volume particle size d of 50 to 500 μm, preferably 60 to 400 μm, and most preferably 70 to 350 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar); 90 , (b) a volume median particle size d measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar) of 5 to 300 μm, preferably 10 to 200 μm, and most preferably 12 to 175 μm 50 , and (c) a volume particle size d of 1 to 100 μm, preferably 1 to 90 μm, and most preferably 1 to 80 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar); 10 , or (d) Spherical.

[0157] Alternatively, the granules have: (a) a volume particle size d of 50 to 500 μm, preferably 60 to 400 μm, and most preferably 70 to 350 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar); 90 , (b) a volume median particle size d measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar) of 5 to 300 μm, preferably 10 to 200 μm, and most preferably 12 to 175 μm 50 , and (c) a volume particle size d of 1 to 100 μm, preferably 1 to 90 μm, and most preferably 1 to 80 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar); 10 , and (d) Spherical.

[0158] For example, if step (b) is carried out in a homogenizer, the granules will have: (a) a volume particle size d of 50 to 500 μm, preferably 60 to 400 μm, and most preferably 70 to 350 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar); 90 , (b) a volume median particle size d measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar) of 20 to 300 μm, preferably 30 to 200 μm, and most preferably 50 to 175 μm 50 , and (c) a volume particle size d of 2 to 100 μm, preferably 3 to 90 μm, and most preferably 10 to 80 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar); 10 , or (d) Spherical.

[0159] Alternatively, the granules have: (a) a volume particle size d of 50 to 500 μm, preferably 60 to 400 μm, and most preferably 70 to 350 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar); 90 , (b) a volume median particle size d measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar) of 20 to 300 μm, preferably 30 to 200 μm, and most preferably 50 to 175 μm 50 , and (c) a volume particle size d of 2 to 100 μm, preferably 3 to 90 μm, and most preferably 10 to 80 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa (0.1 bar); 10 , and (d) Spherical.

[0160] It should further be noted that the granules exhibit favorable stability. In particular, the granules exhibit higher stability compared to granules obtained by the same method but lacking the step of homogenizing the aqueous suspension containing surface-reacted calcium carbonate. For example, the granules exhibit a d (0.5 bar) vs. (0.1 bar) of ≧40, more preferably ≧50, even more preferably ≧60, and most preferably ≧70, such as in the range of 70-120 or 70-110. 50 Additionally or alternatively, the granules have a stability determined by the ratio of d (1.5 bar) to (0.1 bar) of ≧10, more preferably ≧20, even more preferably ≧30, and most preferably ≧35, such as in the range of 35-90 or 35-80. 50 The stability is determined by the ratio of

[0161] In one embodiment, the granules have a d (0.5 bar) to (0.1 bar) of ≧40, more preferably ≧50, even more preferably ≧60, most preferably ≧70, such as in the range of 70-120 or 70-110. 50and d (1.5 bar) to (0.1 bar) ratio of ≧10, more preferably ≧20, even more preferably ≧30, most preferably ≧35, such as in the range of 35-90 or 35-80. 50 The stability is determined by the ratio of

[0162] Additionally, the granules preferably have a particle size of ≧15.0 m as measured by the BET nitrogen method. 2 For example, the granules have a specific surface area of ​​15.0 to 200.0 m / g, measured using nitrogen and the BET method according to ISO 9277:2010. 2 / g specific surface area.

[0163] Furthermore, the granules were measured using mercury intrusion porosimetry to determine the particle size, which was 0.15 to 2.75 cm 3 / g, preferably 0.30 to 2.50 cm 3 / g, most preferably 0.40 to 2.00 cm 3 / g.

[0164] The granules were measured using nitrogen and the BET method according to ISO 9277:2010. 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 The surface-reacted calcium carbonate particles preferably have a BET specific surface area of ​​1 / g.

[0165] The granules have a volume median particle size d measured by using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, especially 1 to 10 μm. 50 It is further preferred that the surface-reacted calcium carbonate particles have:

[0166] According to an exemplary embodiment, the granules comprise particles of surface-reacted calcium carbonate having: (a) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and particularly 1 to 10 μm 50 and / or (b) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area.

[0167] Preferably, the granules comprise particles of surface-reacted calcium carbonate having: (a) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and particularly 1 to 10 μm 50 , or (b) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area.

[0168] Alternatively, the granules comprise particles of surface-reacted calcium carbonate having: (a) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and particularly 1 to 10 μm 50 , and (b) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area.

[0169] Furthermore, the granules have a volume particle size d of 2 to 150 μm, preferably 4 to 100 μm, more preferably 6 to 80 μm, even more preferably 8 to 60 μm, and most preferably 10 to 30 μm. 98 (or d 98 It may be preferred to include particles of surface-reacted calcium carbonate having a surface-reacted calcium carbonate content of 1000 ppm (vol) or less.

[0170] The granules have a diameter of 0.15 to 1.60 cm, calculated from mercury intrusion porosimetry measurements. 3 / g, preferably 0.30 to 1.50 cm 3 / g, more preferably 0.30 to 1.40 cm 3 / g, most preferably 0.30 to 1.35 cm 3 It is further preferred that the surface-reacted calcium carbonate particles have an intra-particle indented specific pore volume in the range of 0.15 to 0.15 / g.

[0171] According to an exemplary embodiment, the granules comprise particles of surface-reacted calcium carbonate having: (a) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and particularly 1 to 10 μm 50 and / or (b) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area, and / or (c) 0.15–1.60 cm calculated from mercury intrusion porosimetry measurements. 3 / g, preferably 0.30 to 1.50 cm 3 / g, more preferably 0.30 to 1.40 cm 3 / g, most preferably 0.30 to 1.35 cm 3 / g, most preferably 0.30 to 0.90 cm 3 Intraparticle indented specific pore volume in the range of / g.

[0172] Preferably, the granules comprise particles of surface-reacted calcium carbonate having: (a) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and particularly 1 to 10 μm 50 , or (b) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area, or (c) 0.15–1.60 cm calculated from mercury intrusion porosimetry measurements. 3 / g, preferably 0.30 to 1.50 cm 3 / g, more preferably 0.30 to 1.40 cm 3 / g, most preferably 0.30 to 1.35 cm 3 / g, most preferably 0.30 to 0.90 cm 3 Intraparticle indented specific pore volume in the range of / g.

[0173] Alternatively, the granules comprise particles of surface-reacted calcium carbonate having: (a) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and particularly 1 to 10 μm 50 , and (b) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area, and (c) 0.15–1.60 cm calculated from mercury intrusion porosimetry measurements. 3 / g, preferably 0.30 to 1.50 cm 3 / g, more preferably 0.30 to 1.40 cm 3 / g, most preferably 0.30 to 1.35 cm 3 Intraparticle indented specific pore volume in the range of / g.

[0174] In one embodiment, the granules contain at least one disintegrant or any compound that can act as a disintegrant. For example, the at least one disintegrant is selected from the group consisting of croscarmellose sodium, modified cellulose gum, insoluble cross-linked polyvinylpyrrolidone, starch, modified starch, starch glycolates such as sodium starch glycolate, microcrystalline cellulose, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-, hydroxyalkyl-, carboxyalkyl-cellulose esters, alginic acid, microcrystalline cellulose and its polymorphs, ion exchange resins, gums, chitin, chitosan, clay, gellan gum, cross-linked polacrilin copolymer, agar, gelatin, dextrin, acrylic acid polymers, sodium / calcium carboxymethylcellulose, hydroxypropylmethylcellulose phthalate, shellac, effervescent mixtures such as bicarbonate in combination with one or more acids, such as citric acid or tartaric acid, and mixtures thereof.

[0175] When present, the granules comprise at least one disintegrant (or any compound that can act as a disintegrant) in an amount ranging from 0.25 to 35% by weight, preferably from 0.5 to 15% by weight, more preferably from 0.5 to 10% by weight, even more preferably from 0.7 to 10% by weight, and most preferably from 0.8 to 10% by weight, based on the total dry weight of the granule. In one embodiment, the granules comprise at least one disintegrant (or any compound that can act as a disintegrant) in an amount ranging from 0.25 to 35% by weight, preferably from 0.5 to 15% by weight, more preferably from 0.5 to 10% by weight, even more preferably from 1.0 to 10% by weight, and most preferably from 1.5 to 10% by weight, based on the total dry weight of the granule. It is particularly preferred that the granules comprise at least one disintegrant (or any compound that can act as a disintegrant) in an amount ranging from 0.8 to 8% by weight, preferably from 0.8 to 6% by weight, more preferably from 0.8 to 5% by weight, and most preferably from 0.8 to 4% by weight, based on the total dry weight of the granule.

[0176] It is understood that the granules are preferably obtained by the process defined herein.

[0177] Thus, the granules are preferably obtained by a process comprising the following steps: (a) providing an aqueous suspension comprising surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is the reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more acids, wherein the carbon dioxide is formed in situ by treatment with the acid and / or is provided from an external source, preferably wherein the carbon dioxide is formed in situ by treatment with the acid; (b) homogenizing the aqueous suspension containing the surface-reacted calcium carbonate of step (a); and (c) removing the liquid from the aqueous suspension comprising surface-reacted calcium carbonate of step (b) by spray drying to obtain granules comprising surface-reacted calcium carbonate.

[0178] If the granules comprise at least one disintegrant (or any compound capable of acting as a disintegrant), the granules are preferably obtained by a process comprising the following steps: (a) providing an aqueous suspension comprising surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is the reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more acids, wherein the carbon dioxide is formed in situ by treatment with the acid and / or is provided from an external source, preferably wherein the carbon dioxide is formed in situ by treatment with the acid; (b) homogenizing the aqueous suspension containing the surface-reacted calcium carbonate of step (a); (c) removing the liquid from the aqueous suspension comprising surface-reacted calcium carbonate of step (b) by spray drying to obtain granules comprising surface-reacted calcium carbonate; and (d) adding at least one disintegrant (or any compound that can act as a disintegrant) to the aqueous suspension before, during, and / or after step (b).

[0179] Additionally or alternatively, the granules are subjected to a treatment with at least one active ingredient and / or an inert precursor thereof, whereby the at least one active ingredient and / or an inert precursor thereof is present substantially only on the outer surface of the granules.

[0180] The term "active ingredient" in the sense of the present invention refers to a substance that has a specific effect on an organism and that causes a specific reaction in humans, animals, microorganisms and / or plants.

[0181] Preferably, the at least one active ingredient and / or its inactive precursor is provided in liquid form.

[0182] The term "liquid" in the sense of the present invention refers to a non-gaseous, fluid composition comprising or consisting of at least one active ingredient and / or its inert precursors, which fluid composition is readily flowable under the pressure conditions and temperatures used, i.e., at the pressures and temperatures at which the granules are mixed with the at least one active ingredient and / or its inert precursors.

[0183] It is therefore understood that the at least one active ingredient and / or its inactive precursor may be liquid in a temperature range of 5 to 200° C., preferably 10 to 120° C., and most preferably 10 to 100° C. For example, the at least one active ingredient and / or its inactive precursor may be liquid under ambient pressure conditions, i.e., atmospheric pressure, in a temperature range of 5 to 200° C., preferably 10 to 120° C., and most preferably 10 to 100° C. Alternatively, the at least one active ingredient and / or its inactive precursor may be liquid under reduced pressure conditions, for example, at a pressure of 100 to 700 mbar, in a temperature range of 5 to 200° C., preferably 10 to 120° C., and most preferably 10 to 100° C.

[0184] In one embodiment, the at least one active ingredient and / or its inactive precursor is liquid at ambient temperature and pressure conditions, e.g., room temperature, e.g., about 5-35°C, preferably 10-30°C, most preferably 15-25°C, and atmospheric pressure.

[0185] Alternatively, the at least one active ingredient and / or its inactive precursor are molten at the temperature of use, for example about 35-200°C, preferably 45-120°C, most preferably 55-100°C, and at ambient pressure conditions, i.e. atmospheric pressure, or at reduced pressure conditions, for example at a pressure of 100-700 mbar.

[0186] Alternatively, the at least one active ingredient and / or its inert precursors are dissolved in the solvent, i.e., the at least one active ingredient and / or its inert precursors and the solvent form a system in which no discrete solid particles are observed in the solvent, thus forming a "solution."

[0187] In one embodiment of the present invention, the solvent is selected from the group comprising water, methanol, ethanol, n-butanol, isopropanol, n-propanol, acetone, dimethyl sulfoxide, dimethylformamide, tetrahydrofuran, vegetable oils and derivatives thereof, animal oils and derivatives thereof, molten fats and waxes, and mixtures thereof. Preferably, the solvent is water, ethanol, and / or acetone. More preferably, the solvent is water.

[0188] For example, at least one active ingredient and / or its inactive precursor may be a chiral compound, and thus, at least one active ingredient and / or its inactive precursor may include the (R)-enantiomer, the (S)-enantiomer, and mixtures thereof, e.g., racemic mixtures.

[0189] Additionally or alternatively, the at least one active ingredient and / or its inactive precursor may be an isomeric compound. Thus, the at least one active ingredient and / or its inactive precursor may include (Z)-isomers, (E)-isomers, and mixtures thereof. For example, if the active ingredient is described as cinnamaldehyde, the cinnamaldehyde may exist as (Z)-cinnamaldehyde and / or (E)-cinnamaldehyde.

[0190] For example, the at least one active ingredient and / or its inactive precursors are selected from the group comprising fragrances, flavorings, herbal extracts and oils, fruit extracts and oils, nutrients, trace minerals, repellents, food, cosmetic, flame retardants, enzymes, polymers, pesticides, fertilizers, preservatives, antioxidants, reactive chemicals, pharmaceutical and / or nutraceutical and / or veterinary active agents of synthetic, semi-synthetic, natural origin, or their pharmaceutical and / or nutraceutical and / or veterinary inactive precursors, and mixtures thereof.

[0191] The fragrance is preferably an alcohol, aldehyde, and / or ketone having a molecular weight of at least about 100 g / mol and is useful alone or in combination with other fragrances to impart an odor, fragrance, perfume, or scent. For example, fragrances include 2,4-dimethyl-3-cyclohexene-1-methanol (Floralol), 2,4-dimethylcyclohexanemethanol (Dihydrofloralol), 5,6-dimethyl-1-methylethenylbicyclo[2.2.1]hept-5-ene-2-methanol (Arbozol), α,α-4-trimethyl-3-cyclohexene-1-methanol (α-terpineol), 2,4,6-trimethyl-3-cyclohexene-1-methanol (isocyclogeraniol), 4-(1-methylethyl) ... Cenmethanol (mayol), α-3,3-trimethyl-2-norboranemethanol, 1,1-dimethyl-1-(4-methylcyclohex-3-enyl)methanol, 2-phenylethanol, 2-cyclohexylethanol, 2-(o-methylphenyl)ethanol, 2-(m-methylphenyl)ethanol, 2-(p-methylphenyl)ethanol, 6,6-dimethylbicyclo-[3.1.1]hept-2-ene-2-ethanol (nopol), 2-(4-methylphenoxy)ethanol, 3,3-dimethyl-Δ 2-β-Norborneneethanol (Pacho Mint), 2-Methyl-2-cyclohexylethanol, 1-(4-Isopropylcyclohexyl)ethanol, 1-Phenylethanol, 1,1-Dimethyl-2-Phenylethanol, 1,1-Dimethyl-2-(4-Methyl-phenyl)ethanol, 1-Phenylpropanol, 3-Phenylpropanol, 2-Phenylpropanol (Hydrotropic Alcohol), 2-(Cyclododecyl)propan-1-ol (Hydroxy-Ambran), 2,2-Dimethyl- 3-(3-methylphenyl)-propan-1-ol (Majantol), 2-methyl-3-phenylpropanol, 3-phenyl-2-propen-1-ol (cinnamyl alcohol), 2-methyl-3-phenyl-2-propen-1-ol (methyl cinnamyl alcohol), α-n-pentyl-3-phenyl-2-propen-1-ol (α-amyl cinnamyl alcohol), ethyl 3-hydroxy-3-phenylpropionate, 2-(4-methylphenyl)-2-propanol, 3-(4-methylcinnamyl alcohol) cyclohex-3-ene)butanol, 2-methyl-4-(2,2,3-trimethyl-3-cyclopenten-1-yl)butanol, 2-ethyl-4-(2,2,3-trimethyl-cyclopent-3-enyl)-2-buten-1-ol, 3-methyl-2-buten-1-ol (prenol), 2-methyl-4-(2,2,3-trimethyl-3-cyclopenten-1-yl)-2-buten-1-ol, ethyl 3-hydroxybutyrate, 4-phenyl-3-buten-2-ol, 2-methyl-4-phenylbutan-2-ol ol, 4-(4-hydroxyphenyl)butan-2-one, 4-(4-hydroxy-3-methoxyphenyl)-butan-2-one, 3-methyl-pentanol, 3-methyl-3-penten-1-ol, 1-(2-propenyl)cyclopentan-1-ol (purinol), 2-methyl-4-phenylpentanol (pamplefleur), 3-methyl-5-phenylpentanol (phenoxanol), 2-methyl-5-phenylpentanol, 2-methyl-5-(2,3-dimethyltricyclo[2.2.1.0. 2,6]hept-3-yl)-2-penten-1-ol (Santalol), 4-methyl-1-phenyl-2-pentanol, 5-(2,2,3-trimethyl-3-cyclopentenyl)-3-methylpentan-2-ol (Sandalol), (1-methyl-bicyclo[2.1.1]hepten-2-yl)-2-methylpent-1-en-3-ol, 3-methyl-1-phenylpentan-3-ol, 1,2-dimethyl-3-(1-methylethenyl)cyclopentan-1-ol, 2-isopropyl-5-methyl-2-hexenol, cis-3-hexen-1- ol, trans-2-hexen-1-ol, 2-isopropenyl-4-methyl-4-hexen-1-ol (lavandulol), 2-ethyl-2-prenyl-3-hexenol, 1-hydroxymethyl-4-isopropenyl-1-cyclohexene (dihydrocuminyl alcohol), 1-methyl-4-isopropenylcyclohex-6-en-2-ol (carbenol), 6-methyl-3-isopropenylcyclohexan-1-ol (dihydrocarveol), 1-methyl-4-isopropenylcyclohexan-3-ol, 4-isopropyl- 1-Methylcyclohexan-3-ol, 4-tert-butylcyclohexanol, 2-tert-butylcyclohexanol, 2-tert-butyl-4-methylcyclohexanol (rutanol), 4-isopropylcyclohexanol, 4-methyl-1-(1-methylethyl)-3-cyclohexen-1-ol, 2-(5,6,6-trimethyl-2-norbornyl)cyclohexanol, isobornylcyclohexanol, 3,3,5-trimethylcyclohexanol, 1-methyl-4-isopropylcyclohexan-3-ol, 1-methyl 4-isopropyl-2,4-heptadiene-1-ol, 6-heptyl-5-hepten-2-ol (isolinalool), 2,4-dimethyl-2,6-heptanedienol, 6,6-dimethyl-2-oxymethyl-bicyclo[3.1.1]hept-2-ene (myrtenol), 4-methyl-2,4-heptadien-1-ol, 3,4,5,6,6-pentamethyl-2-heptanol, 3,6-Dimethyl-3-vinyl-5-hepten-2-ol, 6,6-dimethyl-3-hydroxy-2-methylenebicyclo[3.1.1]heptane, 1,7,7-trimethylbicyclo[2.2.1]heptan-2-ol, 2,6-dimethylheptan-2-ol (dimetol), 2,6,6-trimethylbicyclo[1.3.3]heptan-2-ol, octanol, 2-octenol, 2-methyloctan-2-ol, 2-methyl-6-methylene-7-octen-2-ol (myrcenol), 7-methyloctan-1-ol, 3,7-dimethyl 3,7-dimethyl-6-octenol, 3,7-dimethyl-7-octenol, 3,7-dimethyl-6-octen-1-ol (citronellol), 3,7-dimethyl-2,6-octadien-1-ol (geraniol), 3,7-dimethyl-2,6-octadien-1-ol (nerol), 3,7-dimethyl-7-methoxyoctan-2-ol (oscilol), 3,7-dimethyl-1,6-octadien-3-ol (linalool), 3,7-dimethyloctan-1-ol (pelargol), 3,7-dimethyloctan-3-ol (tetrahydrolinol) Dihydrolinalool), 2,4-octadien-1-ol, 3,7-dimethyl-6-octen-3-ol (dihydrolinalool), 2,6-dimethyl-7-octen-2-ol (dihydromyrcenol), 2,6-dimethyl-5,7-octadien-2-ol, 4,7-dimethyl-4-vinyl-6-octen-3-ol, 3-methyloctan-3-ol, 2,6-dimethyloctan-2-ol, 2,6-dimethyloctan-3-ol, 3,6-dimethyloctan-3-ol, 2,6-dimethyl-7-octen-2-ol, 2,6-dimethyl Muguol, 3-methyl-1-octen-3-ol, 7-hydroxy-3,7-dimethyloctanal, 3-nonanol, 2,6-nonadien-1-ol, cis-6-nonen-1-ol, 6,8-dimethylnonan-2-ol, 3-(hydroxymethyl)-2-nonanone, 2-nonen-1-ol, 2,4-nonadien-1-ol, 3,7-dimethyl-1,6-nonadien-3-ol, decanol, 9-decenol, 2-benzyl-M-diox-5-ol, 2-decen-1-ol, 2,4-Decadien-1-ol, 4-methyl-3-decen-5-ol, 3,7,9-trimethyl-1,6-decadien-3-ol (isobutyllinalool), undecanol, 2-undecen-1-ol, 10-undecen-1-ol, 2-dodecen-1-ol, 2,4-dodecadien-1-ol, 2,7,11-trimethyl-2,6,10-dodecatrien-1-ol (Famesol), 3,7,11-trimethyl-1,6,10-dodecatrien-3-ol (Nerolidol), 3,7,11,15-tetramethylhexadec-2-ene -1-ol (phytol), 3,7,11,15-tetramethylhexadec-1-en-3-ol (isophytol), benzyl alcohol, p-methoxybenzyl alcohol (anisyl alcohol), para-cymen-7-ol (cuminyl alcohol), 4-methylbenzyl alcohol, 3,4-methylenedioxybenzyl alcohol, methyl salicylate, benzyl salicylate, cis-3-hexenyl salicylate, n-pentyl salicylate, 2-phenylethyl salicylate, n-hexyl salicylate, 2-methyl-5-isopropylphenol, 4- Ethyl-2-methoxyphenol, 4-allyl-2-methoxyphenol (eugenol), 2-methoxy-4-(1-propenyl)phenol (isoeugenol), 4-allyl-2,6-dimethoxy-phenol, 4-tert-butylphenol, 2-ethoxy-4-methylphenol, 2-methyl-4-vinylphenol, 2-isopropyl-5-methylphenol (thymol), pentyl ortho-hydroxybenzoate, ethyl 2-hydroxybenzoate, methyl 2,4-dihydroxy-3,6-dimethylbenzoate, 3-hydroxy-5-methoxy- 1-Methylbenzene, 2-tert-butyl-4-methyl-1-hydroxybenzene, 1-ethoxy-2-hydroxy-4-propenylbenzene, 4-hydroxytoluene, 4-hydroxy-3-methoxybenzaldehyde, 2-ethoxy-4-hydroxybenzaldehyde, decahydro-2-naphthol, 2,5,5-trimethyl-octahydro-2-naphthol, 1,3,3-trimethyl-2-norbornanol (fenchol), 3a,4,5,6,7,7a-hexahydro-2,4-dimethyl-4,7-methano-1H-inden-5-ol, 3a,4,5,6,7,7a-Hexahydro-3,4-dimethyl-4,7-methano-1H-inden-5-ol, 2-methyl-2-vinyl-5-(1-hydroxy-1-methylethyl)tetrahydrofuran, β-caryophyllene alcohol, vanillin, ethyl vanillin, cinnamaldehyde, benzaldehyde, phenylacetaldehyde, heptylaldehyde, octylaldehyde, decylaldehyde, undecylaldehyde, undecylenic aldehyde, dodecylaldehyde, tridecylaldehyde, methylnonylaldehyde, dide The citric acid is selected from the group consisting of cinnamaldehyde, anisaldehyde, citronellal, citronellyloxyaldehyde, cyclamen aldehyde, α-hexyl cinnamaldehyde, hydroxycitronellal, α-methyl cinnamaldehyde, methyl nonyl acetaldehyde, propyl phenyl aldehyde, citral, perillaldehyde, tolyl aldehyde, tolyl acetaldehyde, cumin aldehyde, LILIAL®, salicylic aldehyde, α-amyl cinnamaldehyde, and heliotropin, and mixtures thereof.

[0192] Various essential oils, herb extracts, and / or fruit extracts can also be used, preferably those with various medicinal or nutraceutical properties.Essential oils, herb extracts, and / or fruit extracts are generally extracts or aromatic plants, plant parts, fruits, or fruit parts that can be used medicinally or for flavoring.Suitable herb extracts and / or fruit extracts can be used alone or in various mixtures. Commonly used essential oils, herbal extracts, and / or fruit extracts include Echinacea, Goldenseal, Calendula, Rosemary, Thyme, Kava Kava, Aloe, Blood Root, Grapefruit Seed Extract, Black Cohosh, Ginseng, Guarana, Cranberry, Ginkgo Biloba, St. John's Wort, Evening Primrose Oil, Yohimbe Bark, Green Tea, Ephedra, Maca, Bilberry, Lutein, Ginger, Eugenol-containing oils, and combinations thereof.

[0193] A variety of nutrients can be used, including virtually any vitamin, mineral, and / or phytochemical, such as vitamin A, vitamin B1, vitamin B6, vitamin B12, vitamin B6, vitamin D, vitamin E, i.e., tocopherols, vitamin K, thiamine, riboflavin, biotin, folic acid, niacin, pantothenic acid, Q10, alpha-lipoic acid, dihydrolipoic acid, curcumin, xanthophylls, beta-cryptoxanthin, lycopene, lutein, zeaxanthin, astaxanthin, beta-carotene, carotenes, mixed carotenoids, polyphenols, flavonoids, sodium, potassium, calcium, magnesium, sulfur, chlorine, choline, and / or phytochemicals, such as carotenoids, chlorophyll, chlorophyllin, fiber, fiber, and the like. Vanoids, anthocyanins, cyanidin, delphinidin, malvidin, pelargonidin, peonidin, petunidin, flavanols, catechin, epicatechin, epigallocatechin, epigallocatechin gallate, theaflavin, thearubigin, proanthocyanins, flavonols, quercetin, kaempferol, myricetin, isorhamnetin, flavonones hesperetin, naringenin, eriodictyol, tangeretin, flavones, apigenin, luteolin, lignans, phytoestrogens, resveratrol, isoflavones, daidzein, genistein, glycitein, soy isoflavones, and combinations thereof may also be used. Examples of nutrients that can be used as the active ingredient(s) are described in U.S. Patent Application Publication Nos. 2003 / 0157213 A1, 2003 / 0206993 A1, and 2003 / 0099741 A1, which are incorporated herein by reference in their entireties for all purposes.

[0194] In one embodiment, trace minerals such as manganese, zinc, copper, fluorine, molybdenum, iodine, cobalt, chromium, selenium, phosphorus, and combinations thereof may be used.

[0195] Enzymes can include, but are not limited to, coenzyme Q10, pepsin, phytase, trypsin, lipase, protease, cellulase, lactase, and combinations thereof.

[0196] The pesticide is preferably any known herbicide, insecticide, insect growth regulator, nematicide, termiticide, molluscicide, piscicide, birdcide, rodenticide, predator repellent, bactericide, insect repellent, animal repellent, antibacterial agent, fungicide, disinfectant (antimicrobial agent), and bactericide known to those skilled in the art.

[0197] It should be noted that the preservative may be any such compound known to those skilled in the art. For example, the preservative may include, but is not limited to, phenoxyethanol, ethylhexylglycerin, parabens such as methylparaben, ethylparaben, propylparaben, butylparaben, and mixtures thereof, benzalkonium chloride, chlorbutanol, benzyl alcohol, cetylpyridinium chloride, tartaric acid, lactic acid, malic acid, acetic acid, benzoic acid, sodium benzoate, sorbic acid, potassium sorbate, and mixtures thereof.

[0198] The antioxidant is preferably selected from the group comprising: butylhydroxyanisole (BHA), butylhydroxytoluene (BHT), gallates, carotenoids, polyphenols such as resveratrol, flavonoids and mixtures thereof, polyphenol derivatives, tocopherol and its salts, beta-carotene, ubiquinone, tocotrienols, dihydroquercetin, antioxidants of natural origin, and mixtures thereof. If the antioxidant is of natural origin, it may be, for example, a coniferous tree extract, such as a bark extract of Pinus pinastar, such as Pycnogenol® from Hofhaag, Switzerland, and / or a fruit extract of Emblica officinalis, such as Saberry® from Sabinsa, Germany.

[0199] The pharmaceutically active agent or its pharmaceutically inactive precursor is preferably selected from the group comprising pharmaceutically active agents or its pharmaceutically inactive precursors of synthetic origin, semi-synthetic origin, natural origin, and combinations thereof.

[0200] Thus, a pharmaceutically active agent refers to a pharmaceutically active agent of synthetic origin, semi-synthetic origin, natural origin, and combinations thereof. Additionally, a pharmaceutically inactive precursor of a pharmaceutically active agent refers to a pharmaceutically inactive precursor of synthetic origin, semi-synthetic origin, natural origin, and combinations thereof, which is activated at a later stage to the respective pharmaceutically active agent.

[0201] Activation of such pharmaceutically inactive precursors is known to those skilled in the art and is commonly used, e.g., activation in the stomach and / or gastro-intestinal pathway, e.g., acid activation or trypsin- or chymotrypsin cleavage.

[0202] It is within the understanding of one skilled in the art that the activation methods mentioned are merely exemplary features and are not intended to be limiting features.

[0203] It is noted that the pharmaceutically active agent or its pharmaceutically inactive precursor can be any such compound known to those skilled in the art.

[0204] Thus, a pharmaceutically active agent includes any compound that provides prophylactic and / or therapeutic properties when administered to humans and / or animals. Examples include, but are not limited to, pharmaceutical actives, therapeutic actives, veterinary actives, nutritional supplements, and growth regulators.

[0205] The pharmaceutically active agent or its pharmaceutically inactive precursor can be an anti-inflammatory agent.Such agents can include, but are not limited to, nonsteroidal anti-inflammatory agents or NSAIDs, such as propionic acid derivatives; acetic acid derivatives; fenamic acid derivatives; biphenylcarboxylic acid derivatives; and oxicams.All of these NSAIDs are fully described in U.S. Patent No. 4,985,459 to Sunshine et al., the entirety of which is incorporated herein by reference for the description of such NSAIDs.Examples of useful NSAIDs include acetylsalicylic acid, ibuprofen, naproxen, benoxaprofen, flurbiprofen, fenoprofen, fenbufen, ketoprofen, indoprofen, pirprofen, carprofen, oxaprozin, pranoprofen, microprofen, tioxaprofen, suprofen, alminoprofen, tiaprofenic acid, fluprofen, bucloxic acid, and mixtures thereof. Also useful are steroidal anti-inflammatory agents, such as hydrocortisone, and COX-2 inhibitors, such as meloxicam, celecoxib, rofecoxib, valdecoxib, etoricoxib, or mixtures thereof. Mixtures of any of the above anti-inflammatory agents can be used.

[0206] Other materials that can be used as pharmaceutically active agents or their inactive precursors include commonly known mouth and throat products, including, but not limited to, upper respiratory tract agents such as phenylephrine, diphenhydramine, dextromethorphan, bromhexine, and chlorpheniramine, gastrointestinal agents such as famotidine, loperamide, and simethicone, antifungals such as miconazole nitrate, antibiotics, and analgesics such as ketoprofen and flurivprofen.

[0207] The pharmaceutically active agent or its pharmaceutically inactive precursor may also be selected from sodium pyrosulfite, butylated hydroxytoluene, butylated hydroxyanisole.

[0208] Pharmaceutically active agents or their pharmaceutically inactive precursors may also be used, for example, ephedrine, magaldrate, pseudoephedrine, sildenafil, xylocaine, benzalkonium chloride, caffeine, phenylephrine, amfepramone, orlistat, sibutramine, acetaminophen, aspirin, glitazones, metformin, chlorpromazine, dimenhydrinate, domperidone, meclozine, metoclopramide, odansetron, prednisolone, promethazine, acrivastine, cetirizine, cinarizine, clemastine, cyclizine, deslo Latadine, dexchlorpheniramine, dimenhydrinate, ebastine, fexofenadine, ibuprofen, levorevoloricin, loratadine, meclozine, mizolastine, promethazine, miconazole, chlorhexidine diacetate, fluoride, decapeptide KSL, aluminum fluoride, calcium amino chelate, ammonium fluoride, ammonium fluorosilicate, ammonium monofluorophosphate, calcium fluoride, calcium gluconate, calcium glycerophosphate, calcium lactate, calcium monofluorophosphate, Calcium carbonate, carbamide, cetylpyridinium chloride, chlorhexidine, chlorhexidine digluconate, chlorhexidine chloride, chlorhexidine diacetate, CPP casein phosphopeptide, hexetidine, octadecenylammonium fluoride, potassium fluorosilicate, potassium chloride, potassium monofluorophosphate, sodium bicarbonate, sodium carbonate, sodium fluoride, sodium fluorosilicate, sodium monofluorophosphate, sodium tri-polyphosphate, tin fluoride, stearyl trihydroxyethyl propyl Diamine dihydrofluoride, strontium chloride, tetrapotassium pyrophosphate, tetrasodium pyrophosphate, tripotassium orthophosphate, trisodium orthophosphate, alginic acid, aluminum hydroxide, sodium bicarbonate, sildenafil, tadalafil, vardenafil, yohimbine, cimetidine, nizatidine, ranitidine, acetylsalicylic acid, clopidogrel, acetylcysteine, bromhexine, codeine, dextromethorphan, diphenhydramine, noscapine, phenylpropanolamine, vitamin D, simvastatin, bisacodyl,Lactitol, lactulose, magnesium oxide, sodium picosulfate, senna glycoside, benzocaine, lidocaine, tetracaine, almotriptan, eletriptan, naratriptan, rizatriptan, sumatriptan, zolmitriptan, calcium, chromium, copper, iodine, magnesium, manganese, molybdenum, phosphorus, selenium, zinc, chloramine, hydrogen peroxide, metronidazole, triamcinolone acetonide, benzethonium chloride, cetylpyridine chloride, chlorhexidine, fluoride, lidocaine, amphotericin, miconazole, nitric acid, Statins, fish oil, ginkgo biloba, ginseng, ginger, purple cornflower, saw palmetto, cetirizine, levocetirizine, loratadine, diclofenac, flurbiprofen, acrivastine pseudoephedrine, loratadine pseudoephedrine, glucosamine, hyaluronic acid, decapeptide KSL-W, decapeptide KSL, resveratrol, misoprostol, bupropion, ondansetron HCl, esomeprazole, lansoprazole, omeprazole, pantoprazole, rabeprazole, bacteria, etc., reperamide, simethicone, acrivastine, pseudoephedrine, loratadine, pseudoephedrine, glucosamine, hyaluronic acid, decapeptide KSL-W, decapeptide KSL, resveratrol, misoprostol, bupropion, ondansetron HCl, esomeprazole, lansoprazole, omeprazole, pantoprazole, rabeprazole, bacteria, etc. Cetyl salicylate and others, sucralfate, clotrimazole, fluconazole, itraconazole, ketoconazole, terbinafine, allopurinol, probenecid, atorvastatin, fluvastatin, lovastatin, nicotinic acid, pravastatin, rosuvastatin, simvastatin, pilocarpine, naproxen, alendronate, etidronate, raloxifene, risedronate, benzodiazepines, disulfiram, naltrexone, buprenorphine, codeine, dextropoxyphene, fentanyl, hydromorphone, Tobemidone, ketoprofen, methadone, morphine, naproxen, nicomorphine, oxycodone, pethidine, tramadol, amoxicillin, ampicillin, azithromycin, ciprofloxacin, clarithromycin, doxycycline, erythromycin, fusidic acid, lymecycline, metronidazole, moxifloxacin, ofloxacin, oxytetracycline, phenoxymethylpenicillin, rifamycin, roxithromycin, sulfamethizole, tetracycline, trimethoprim, vancomycin, acarbose,Glibenclamide, gliclazide, glimepiride, glipizide, insulin, repaglinide, tolbutamide, oseltamivir, acyclovir, famciclovir, penciclovir, valganciclovir, amlopidine, diltiazem, felodipine, nifedipine, verapamil, finasteride, minoxidil, cocaine, buprenorphine, clonidine, methadone, naltrexone, calcium channel blockers, clonidine, ergotamine, beta-blockers, aceclofenac, celecoxib, dexprofen, etodolac, indomethacin, ketoprofen, ketorolac, lornoxicam, meloxicam, nabumetone, euloroxicam, parecoxib, phenylbutazone, piroxicam, tiaprofenic acid, tolfenamic acid, aripiprazole, chlorpromazine, chlorprothixene, clozapine, The antihistamine may be selected from lupenthixol, fluphenazine, haloperidol, lithium carbonate, lithium citrate, melperone, penfluridol, pericyazine, perphenazine, pimozide, pipamperone, prochlorperazine, risperidone, thiorizidine, fluconazole, itraconazole, ketoconazole, voriconazole, opium, benzodiazepines, hydroxylase, meprobamate, phenothiazines, aluminum aminoacetic acid, esomeprazole, famotidine, magnesium oxide, nizatide, omeprazole, pantoprazole, fluconazole, itraconazole, ketoconazole, metronidazole, amphetamine, atenolol, bisoprolol fumarate, metoprolol, metroprolol, pindolol, propranolol, auranofin, and bendazac.

[0209] Further examples of useful pharmaceutically active agents or pharmaceutically inactive precursors thereof can include an active ingredient selected from therapeutic agents including analgesics, anesthetics, antipyretics, antiallergics, antiarrhythmics, appetite suppressants, antifungals, anti-inflammatory agents, bronchodilators, cardiovasodilators, coronary vasodilators, cerebrovasodilators, peripheral vasodilators, anti-infectives, psychotropic agents, antimanic agents, stimulants, antihistamines, laxatives, decongestants, gastrointestinal sedatives, sexual dysfunction agents, antiseptics, antidiarrheal agents, antianginal drugs, vasodilators, antihypertensives, vasoconstrictors, antimigraine medications, antibiotics, tranquilizers, antipsychotics, antineoplastic agents, anticoagulants, antithrombotic agents, hypnotics, sedatives, antiemetics, antivomiting agents, anticonvulsants, neuromuscular agents, hyperglycemic agents, hypoglycemic agents, thyroid agents, antithrombotic agents, antithrombotic agents, anticoagulants, antithrombotic agents, antithrombotic agents, antispasmodic ... glandulars, diuretics, antispasmodics, uterine relaxants, antiobesity agents, appetite suppressants, antispasmodics, anabolic agents, erythropoietic agents, antiasthmatic agents, expectorants, antitussives, mucolytics, antiuricemic agents, dental excipients, breath fresheners, antacids, antidiuretics, intestinal regulators, beta blockers, tooth whitening agents, enzymes, coenzymes, proteins, energy boosters, fiber, probiotics, prebiotics, NSAIDs, cough suppressants, decongestants, antihistamines, expectorants, antidiarrheals, hydrogen antagonists, proton pump inhibitors, general nonselective central nervous system depressants, general nonselective central nervous system stimulants, selective central nervous system enhancers, antiparkinsonian agents, narcotic analgesics, analgesic-antipyretics, psychopharmacological agents, and sexual dysfunction agents.

[0210] Examples of useful pharmaceutically active agents or their pharmaceutically inactive precursors can also include: casein glyco-macro-peptide (CGMP), triclosan, cetylpyridinium chloride, domiphen bromide, quaternary ammonium salts, zinc compounds, sanguinarine, fluoride, alexidine, octonidine, EDTA, aspirin, acetaminophen, ibuprofen, ketoprofen, diflunisal, fenoprofen calcium, naproxen, tolmetin sodium, indomethacin, benzonatate, caramiphen edisylate, menthol, Dextromethorphan hydrobromide, theobromine hydrochloride, clophenedianol hydrochloride, pseudoephedrine hydrochloride, phenylephrine, phenylpropanolamine, pseudoephedrine sulfate, brompheniramine maleate, chlorpheniramine maleate, carbinoxamine maleate, clemastine fumarate, dexchlorpheniramine maleate, diphenhydramine hydrochloride, difenpyralid hydrochloride, azatadine maleate, diphenhydramine citrate, doxylamine succinate, promethazine hydrochloride, pyrilamine maleate, tripehle citrate amine, triprolidine hydrochloride, acrivastine, loratadine, brompheniramine, dexbromopheniramine, guaifenesin, ipecac, potassium iodide, terpine hydrate, loperamide, famotidine, ranitidine, omeprazole, lansoprazole, aliphatic alcohols, barbiturates, caffeine, strychnine, picrotoxin, pentylenetetrazole, phenylhydantoin, phenobarbital, primidone, carbamazapine, ethoxuximide, methsuximide, phensuximide, trimethadione, diazepam, benzodiazepam Azepines, phenacemide, pheneturide, acetazolamide, sulthiame, bromide, levodopa, amantadine, morphine, heroin, hydromorphone, metopon, oxymorphone, levophanol, codeine, hydrocodone, xycodone, nalorphine, naloxone, naltrexone, salicylate, phenylbutazone, indomethacin, phenacetin, chlorpromazine, methotrimeprazine, haloperidol, clozapine, reserpine, imipramine, tranylcypromine, phenelzine, lithium, sildenafil citrate, tadalafil,and vardenafil CL. For example, eugenol can be used as an anesthetic,

[0211] Examples of useful pharmaceutically active agents or their pharmaceutically inactive precursors include ACE inhibitors, antianginals, antiarrhythmics, antiasthmatics, anticholesterols, analgesics, anesthetics, anticonvulsants, antidepressants, antidiabetics, antidiarrheal preparations, antidotes, antihistamines, antihypertensives, anti-inflammatory agents, antilipids, antimanic agents, antiemetics, antistroke agents, antithyroid preparations, antineoplastics, antivirals, acne medications, alkaloids, amino acid preparations, antitussives, antiuricemics, antivirals, anabolic preparations, systemic and non-systemic Anti-infectives, antineoplastics, anti-Parkinson's agents, anti-rheumatics, appetite stimulants, biological response improvers, hematological improvers, bone metabolism regulators, cardiovascular dilators, central nervous system stimulants, cholinesterase inhibitors, contraceptives, decongestants, dietary supplements, dopamine receptor agonists, endometriosis medications, enzymes, erectile dysfunction medications such as sildenafil citrate currently marketed as Viagra®, infertility medications, gastrointestinal medications, homeopathic remedies, hormones, hypercalcemia and hypocalcemia Calcium-deficiency drugs, immunomodulators, immunosuppressants, migraine drugs, motion sickness drugs, muscle relaxants, obesity drugs, osteoporosis drugs, oxytocin preparations, parasympatholytics, parasympathomimetics, prostaglandins, psychiatric drugs, respiratory disease drugs, sedatives, smoking cessation aids such as bromocriptine, sympatholytics, tremor preparations, urinary tract drugs, vasodilators, laxatives, antacids, ion exchange resins, antipyretics, appetite suppressants, expectorants, antianxiety drugs, antiulcer drugs, anti-inflammatory drugs, coronary artery dilating drugs, cerebral hemorrhage drugs The active ingredient may be selected from the group consisting of vasodilators, peripheral vasodilators, psychotropics, stimulants, antihypertensives, vasoconstrictors, antimigraine medications, antibiotics, tranquilizers, antipsychotics, antineoplastics, anticoagulants, antithrombotic agents, hypnotics, antiemetics, antivomiting agents, anticonvulsants, neuromuscular agents, hyperglycemic and hypoglycemic agents, thyroid medications, antithyroid agents, diuretics, anticonvulsants, uterine relaxants, antiobesity agents, erythropoietic agents, antiasthmatic agents, cough suppressants, mucolytics, DNA and gene modifiers, and combinations thereof.

[0212] Examples of useful contemplated pharmaceutically active agents or their pharmaceutically inactive precursors also include antacids, H2-antagonists, and analgesics. For example, antacid formulations can be prepared using calcium carbonate alone or in combination with magnesium hydroxide and / or aluminum hydroxide. Additionally, antacids can be used in combination with H2-antagonists.

[0213] Analgesics include opiates and opiate derivatives such as Oxycontin®, ibuprofen, aspirin, acetaminophen, and combinations thereof, and can optionally include caffeine.

[0214] Other useful pharmaceutically active agents or their pharmaceutically inactive precursors can include antidiarrheals, such as Immodium® AD, antihistamines, antitussives, decongestants, vitamins, and breath fresheners. Also contemplated for use in the present invention are tranquilizers, such as Xanax®; antipsychotics, such as Clozaril® and Haldol®; nonsteroidal anti-inflammatory drugs (NSAIDs), such as ibuprofen, naproxen sodium, Voltaren®, and Lodine®; antihistamines, such as Claritin®, Hismanal®, Relafen®, and Tavist®; and antihistamines, such as Kytril® and Cesamet®. antiemetics; bronchodilators such as Bentolin® and Proventil®; antidepressants such as Prozac®, Zoloft®, and Paxil®; antimigraine medications such as Imigra®, ACE inhibitors such as Vasotec®, Capoten®, and Zestril®; anti-Alzheimer's medications such as Nicergoline®; and CaH-antagonists such as Procardia®, Adalat®, and Calan®.

[0215] Common H2-antagonists contemplated for use in the present invention include cimetidine, ranitidine hydrochloride, famotidine, nizatidine, ebrotidine, mifentidine, roxatidine, pisatidine, and aceroxatidine.

[0216] Active antacid ingredients include, but are not limited to, aluminum hydroxide, dihydroxyaluminum aminoacetate, aminoacetic acid, aluminum phosphate, dihydroxyaluminum sodium carbonate, bicarbonate, bismuth aluminate, bismuth carbonate, bismuth subcarbonate, bismuth subgallate, bismuth subnitrate, bismuth subsalicylate, calcium phosphate, citrate ion (acid or salt), aminoacetic acid, magnesium aluminate sulfate hydrate, magaldrate, magnesium aluminosilicate, magnesium carbonate, magnesium glycinate, magnesium hydroxide, magnesium oxide, magnesium trisilicate, milk solids, aluminum phosphate, monobasic or dibasic calcium phosphate, tricalcium phosphate, potassium bicarbonate, sodium tartrate, sodium bicarbonate, magnesium aluminosilicate, tartaric acid, and salts.

[0217] In certain embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor can be selected from analgesics / anesthetics such as menthol, phenol, hexylresorcinol, benzocaine, dyclonine hydrochloride, benzyl alcohol, salicylic alcohol, and combinations thereof. In certain embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor can be selected from demulcents (mucosal protectants) such as slippery elm bark, pectin, gelatin, and combinations thereof. In some embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor can be selected from antiseptic ingredients such as cetylpyridinium chloride, domiphen bromide, dequalinium chloride, eugenol, and combinations thereof.

[0218] In some embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor can be selected from antitussive ingredients, such as chlophedianol hydrochloride, codeine, codeine phosphate, codeine sulfate, dextromethorphan, dextromethorphan hydrobromide, diphenhydramine citrate, and diphenhydramine hydrochloride, and combinations thereof.

[0219] In some embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor can be selected from throat soothing agents such as honey, propolis, aloe vera, glycerin, menthol, and combinations thereof. In yet other embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor can be selected from cough suppressants. Such cough suppressants are divided into two groups: agents that alter phlegm texture or production, such as mucolytics and expectorants; and agents that suppress the cough reflex, such as codeine (a narcotic cough suppressant), antihistamines, dextromethorphan, and isoproterenol (a non-narcotic cough suppressant).

[0220] In yet other embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor may be an antitussive selected from the group including codeine, dextromethorphan, dextrorphan, diphenhydramine, hydrocodone, noscapine, oxycodone, pentoxyverine, and combinations thereof. In some embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor may be selected from antihistamines such as acrivastine, azatadine, brompheniramine, chlorpheniramine, clemastine, cyproheptadine, dexbrompheniramine, dimehydrinate, diphenhydramine, doxylamine, hydroxyzine, meclizine, phenindamine, phenyltoloxamine, promethazine, pyrilamine, tripelennamine, triprolidine, and combinations thereof. In certain embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor can be selected from non-sedating antihistamines, such as astemizole, cetirizine, ebastine, fexofenadine, loratidine, terfenadine, and combinations thereof.

[0221] For example, the one or more active ingredients are selected from fragrances, flavorings, essential oils, insecticides, fungicides, pharmaceutically active agents or pharmaceutically inactive precursors thereof, such as bactericides and / or anesthetics, and mixtures thereof.

[0222] When the granules contain at least one active ingredient and / or an inactive precursor thereof, the at least one active ingredient and / or inactive precursor is preferably present in the granules in an amount of 0.5 to 80% by weight, preferably 10.0 to 70% by weight, most preferably 20 to 60% by weight, based on the total dry weight of the granules.

[0223] Furthermore, it is noted that the granules of the present invention have improved flowability, compactability, and mechanical stability compared to granules produced by a process lacking the homogenization step (b).

[0224] Additionally, the granules of the present invention are ready-to-use granules in further processes for producing dispersible dosage forms, such as tablets, minitablets, pellets, capsules, jelly beans, or chewing gum, that contain these granules.

[0225] Additionally, the granules of the present invention and the dosage forms described above can be used in dietary supplements, agricultural products, animal products, cosmetics, household products, food, packaging products, or personal care products, or as excipients in pharmaceuticals.

[0226] It is understood that the cosmetic product is preferably a dry cosmetic composition and / or a dry skin care composition, more preferably a dry cosmetic composition. For example, the dry cosmetic composition is a cosmetic powder including eye shadow, powder makeup, lip powder, face powder, body powder, or blusher. According to another embodiment, the cosmetic product is a dry skin care composition. For example, the dry skin care composition may be a skin care powder including shaving powder, body powder, baby powder, foot powder, and deodorant powder. According to yet another embodiment, the dry cosmetic composition and / or dry skin care composition is a dry cosmetic and skin care composition.

[0227] The personal care product is preferably an oral care composition. In one embodiment, the oral care composition is a toothpaste, a tooth gel, a tooth powder, a cement, a composition implemented on a mouth strip or oral adhesive patch, a (chewable) tooth tablet, a chewable lozenge, or a chewable gum, preferably a toothpaste, a tooth powder, or a (chewable) tooth tablet.

[0228] Such minitablets or tablets are well known in the art and are of a particle size typically used for the product being prepared.

[0229] For example, the minitablets or tablets have a weight median particle size d of 0.1 to 20.0 mm, preferably 0.2 to 15.0 mm, more preferably 0.3 to 10.0 mm, as measured according to a mechanical sieving method. 50 It has.

[0230] The following examples and tests illustrate the present invention but are not intended to limit it in any way. [Brief explanation of the drawings]

[0231] [Figure 1] FIG. 1 shows the SEM (scanning electron microscope) results for the granules obtained for SRCC1 by using a homogenizer for homogenization and a fountain nozzle for spray drying. [Figure 2] FIG. 2 shows the SEM results for the granules obtained for SRCC2 by using a homogenizer for homogenization and a fountain nozzle for spray drying. [Figure 3] FIG. 3 shows the SEM results for the granules obtained for SRCC3 by using a homogenizer for homogenization and a fountain nozzle for spray drying. [Figure 4] FIG. 4 shows the SEM results for the granules obtained for SRCC4 by using a homogenizer for homogenization and a fountain nozzle for spray drying. [Figure 5] Figure 5 further shows the SEM results for the cross section of the granules obtained for SRCC2 by spray drying with a fountain nozzle. [Figure 6] FIG. 6 shows the SEM results for the granules obtained for SRCC5 by using a mill for homogenization and a rotary atomizer for spray drying. [Figure 7] FIG. 7 shows the SEM results for the granules obtained for SRCC6 by using a mill for homogenization and a rotary atomizer for spray drying. [Figure 8]Figure 8 shows the results for tablet hardness [N] as a function of main compression force [kN] for tablets prepared from granules prepared according to the invention by spray drying in a rotary atomizer, compared with two commercially available filler samples. [Figure 9] Figure 9 shows the results for disintegration time [sec] as a function of tablet hardness [N] for tablets prepared from granules prepared according to the invention by spray drying in a rotary atomizer, compared with two commercially available filler samples. [Example]

[0232] 1.Measurement method The measurement methods used in the examples are described below.

[0233] Particle size distribution The median particle size d was determined by volume in wet units using a Malvern Mastersizer 2000 or 3000 laser diffraction system (Malvern Instruments Plc., UK). 50 (vol) and the top cut particle size determined by volume, d 98 (vol), and volume particle size d 90 (vol) and d 10 The value of (vol) was calculated. 50 (vol) or d 98 The values ​​in vol indicate the diameter value at which 50% or 98% of the particles by volume have a diameter smaller than this value, respectively. The raw data obtained from the measurements were analyzed using Mie theory with a particle refractive index of 1.57 and an absorption coefficient of 0.005. This 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. The samples were measured in the dry state without any pretreatment.

[0234] Median particle size d determined by weight 50The particle size distribution (wt) was measured by the sedimentation method, which is an analysis of sedimentation behavior in a gravimetric field. Measurements were performed using a Sedigraph® 5120 from Micromeritics Instrument Corporation, USA. This method and instrument are known to those skilled in the art and are commonly used to determine particle size distribution of fillers and pigments. Measurements were performed in a 0.1 wt% Na4P2O7 aqueous solution. The sample was dispersed using a high-speed stirrer and sonicated.

[0235] This method and equipment is known to those skilled in the art and is commonly used to determine particle size distribution of fillers and pigments.

[0236] Unless otherwise indicated in the Examples section below, volume particle size was determined in wet units using a Malvern Mastersizer 2000 laser diffraction system (Malvern Instruments Plc., UK).

[0237] Specific surface area (SSA) The specific surface area was measured by the BET method according to ISO 9277:2010 using nitrogen following conditioning of the sample by heating for 30 minutes at 110°C if one or more disintegrants were used, or at 250°C if the sample did not contain a disintegrant. If the sample was in the form of an aqueous suspension, it was filtered in a Buchner funnel, rinsed with deionized water and dried in an oven at 110°C for at least 12 hours before such measurement.

[0238] Intra-particle specific pore volume (cm 3 / g) Specific pore volumes were measured using mercury intrusion porosimetry using a Micromeritics Autopore V 9620 mercury porosimeter with a maximum applied mercury pressure of 414 MPa (60,000 psi), equivalent to a Laplace throat diameter of 0.004 μm (~nm). The equilibration time used for each pressure step was 20 seconds. Sample materials were loaded into 5 cm 3The powder was sealed in a chamber powder penetrometer. Data were corrected for mercury compression, penetrometer expansion, and sample material compression using the software Pore-Comp (Gane, PAC, Kettle, JP, Matthews, GP, and Ridgway, CJ, "Void Space Structure of Compressible Polymer Spheres and Consolidated Calcium Carbonate Paper-Coating Formulations", Industrial and Engineering Chemistry Research, 35(5), 1996, pp. 1753-1764).

[0239] The total pore volume seen in the integrated intrusion data can be separated into two regions with intrusion data ranging from 214 μm down to approximately 1-4 μm, indicating a strong contribution from coarse packing of the sample between any aggregate structures. Below these diameters, there is fine interparticle packing of the particles themselves. If the particles also contain intraparticle pores, this region is bimodal, and the intraparticle specific pore volume is defined as the specific pore volume of mercury intruded into pores narrower than the inflection point of the bimodal transition. The sum of these three regions gives the total pore volume of the powder, but is heavily influenced by the precipitation of powder at the coarse pore end of the original sample compaction / distribution.

[0240] Taking the first derivative of the cumulative penetration curve reveals a pore size distribution based on the equivalent Laplace diameter, which necessarily includes pore blocking. The derivative curve clearly shows the coarse aggregate pore structure region, the interparticle pore region, and, if present, the intraparticle pore region. Once the intraparticle pore size range is known, it is possible to subtract the remaining interparticle and interaggregate pore volumes from the total pore volume to obtain only the desired pore volume of the internal pores as pore volume per unit mass (specific pore volume). Of course, the same subtraction principle applies to isolating any other pore size region of interest.

[0241] Bulk density 100±0.5 g of each material was carefully filled into a 250 mL graduated cylinder through a powder funnel and the volume was read to the nearest 1 mL. The loose bulk density was calculated according to the following formula and the result was recorded to the nearest 0.01 g / mL: Loose bulk density [g / mL] = weight of weighed sample [g] / bulk volume [mL]

[0242] Brookfield Viscosity Brookfield viscosity is measured with a Brookfield (Type RVT) viscometer at 25°C ± 1°C using a suitable spindle at 100 rpm after 30 seconds and is specified in mPa·s.

[0243] Solid weight of material in suspension (wt%) The weight of the solids was determined by dividing the weight of the solid material by the total weight of the aqueous suspension, which is measured by weighing the solid material obtained by evaporating the aqueous phase of the slurry and drying the resulting material to a constant weight.

[0244] Granule stability and particle size distribution A Malvern Mastersizer 3000 (Malvern Instruments Plc., UK) combined with a Malvern Aero S dry dispersion device and a dry cell was used to measure the d of 5–300 μm by laser diffraction. 50 The particle size distribution of the granules was measured within the fineness range of 0.1 bar, 0.5 bar, and 1.5 bar. The method used is described in the Mastersizer 3000 Basic Guide, Mastersizer 3000 Manual, and Manual for Aero Series Dry dispersion unit, available from Malvern Instruments Ltd. Approximately 10 ml of sample was loaded into the Aero S through the corresponding sieve. The sample was measured in the dry state. The results are expressed in V.-% (volume %). The feed rates were 0.1 bar, 0.5 bar, and 1.5 bar to demonstrate the stability of the granules.

[0245] A feed rate of 0.1 bar was used to determine the particle size distribution of the granules.

[0246] Scanning electron microscope (SEM) Samples were prepared by diluting 50–150 μl of slurry sample with 5 ml of water. The amount of slurry sample depended on the solid content, average particle size, and particle size distribution. The diluted sample was filtered using a 0.8 μm membrane filter. If the filtrate was cloudy, a finer filter was used. Double-sided conductive adhesive tape was attached to an SEM stub. The SEM stub was then lightly pressed against the still-wet filter cake on the filter. The SEM stub was then sputtered with 8 nm of Au. Observations were then performed under a FESEM (Zeiss Sigma VP) at 5 kV (Au). The samples were then analyzed using a Sigma VP field emission scanning electron microscope (Carl Zeiss AG, Germany) and high vacuum (<10 -2 The prepared samples were observed by using a secondary electron detector (SE2) at 1000 kJ / cm² (Pa).

[0247] Mechanical sieves Mechanical sieving was carried out in a vibrating sieve shaker RETSCH AS200 equipped with Easy Sieve Software, a sieve according to ISO 3310 including a sieving pan, and a balance (0.1 g). 120 g was used for sieving. This ensured homogeneity of the test sample and maximum sieving reproducibility. The test sample material was placed in the upper test sieve. Sieving was carried out in the following manner: sieving time: 3 min / amplitude: 1.0 mm / spacing: 10 s.

[0248] 2. Materials used Surface-reacted calcium carbonate (SRCC1) To obtain SRCC, a weight-based median particle size d of 1.3 μm was measured by sedimentation. 50350 litres of an aqueous suspension of ground calcium carbonate was prepared in a mixing vessel by adjusting the solids content of ground limestone calcium carbonate from Omya SAS, Orgon, having (wt) to obtain a solids content of 10 wt. % based on the total weight of the aqueous suspension.

[0249] While the slurry was mixed at a speed of 6.2 m / s, 11.2 kg of phosphoric acid in the form of an aqueous solution containing 30% by weight of phosphoric acid was added to the suspension over a period of 20 minutes at a temperature of 70° C. After the acid addition, the slurry was stirred for a further 5 minutes and then removed from the vessel.

[0250] The solid content of the obtained slurry (SRCC1) was 25.7 wt % relative to the total mass of the slurry, and the Brookfield viscosity was 554 mPa·s.

[0251] The properties of the surface-reacted calcium carbonate are summarized in Table 1 below.

[0252] [Table 1]

[0253] Other ingredients Croscarmellose Sodium-Ac-di-sol from JRS

[0254] 3. Drying of SRCC by Homogenization and Spray Drying A. Homogenization SRCC2 The surface-reacted calcium carbonate (SRCC1) slurry was then diluted to a solids content of approximately 20.1 wt. % based on the total weight of the slurry. 500 L of the slurry was then pumped twice using a GEA Ariete NS3055 homogenizer from GEA Mechanical Equipment Italia SpA at a pressure of 500 bar, a temperature of 50-70 °C, and a feed rate of 400 L / h, with a closed screw position and a small nozzle.

[0255] The solid content of the resulting slurry (SRCC2) was 23.4 wt % based on the total weight of the slurry.

[0256] After two passes through the homogenizer, the surface-reacted calcium carbonate had the properties shown in Table 2 below.

[0257] [Table 2]

[0258] SRCC3 The surface-reacted calcium carbonate (SRCC1) slurry was diluted to a solids content of approximately 18.9 wt. % based on the total weight of the slurry. Five hundred liters of the slurry were then pumped three times using a GEA Ariete NS3055 homogenizer from GEA Mechanical Equipment Italia SpA at a pressure of 500 bar, a temperature of 50-70 °C, and a feed rate of 400 L / h, with a closed screw position and a small nozzle.

[0259] The solid content of the resulting slurry (SRCC3) was 18.9 wt % based on the total weight of the slurry.

[0260] After three passes through the homogenizer, the surface-reacted calcium carbonate had the properties shown in Table 3 below.

[0261] [Table 3]

[0262] SRCC4 The surface-reacted calcium carbonate (SRCC1) slurry was mixed with croscarmellose sodium in an amount of 3 wt. % based on the total weight of the surface-reacted calcium carbonate (SRCC1) and then diluted to a solids content of approximately 20.5 wt. % based on the total weight of the slurry. Subsequently, 500 L of the slurry was pumped twice using a GEA Ariete NS3055 homogenizer from GEA Mechanical Equipment Italia SpA, with a closed screw position and a small nozzle, at a pressure of 500 bar, a temperature of 50-70°C, and a feed flow rate of 400 L / h.

[0263] The solid content of the resulting slurry (SRCC4) was 20.5 wt % based on the total weight of the slurry.

[0264] After two passes through the homogenizer, the surface-reacted calcium carbonate had the properties shown in Table 4 below.

[0265] [Table 4]

[0266] SRCC5 The surface-reacted calcium carbonate (SRCC1) slurry was diluted to a solids content of about 20.1 wt. % based on the total weight of the slurry and then milled in a Siegmund Linder 25 L vertical stirred media mill containing 33 kg of Silibeads ZY-E 0.4 / 0.6 mm at a feed flow rate of 82 L / h, a tip speed of 5.0 m / s, and a specific energy of about 55 kWh / t.

[0267] The solid content of the resulting slurry (SRCC5) was 20.2 wt % based on the total weight of the slurry.

[0268] After milling, the surface-reacted calcium carbonate had the properties shown in Table 5 below.

[0269] [Table 5]

[0270] SRCC6 The surface-reacted calcium carbonate (SRCC1) slurry was diluted to a solids content of about 22.6 wt. % based on the total weight of the slurry and then milled in a Siegmund Linder 25 L vertical stirred media mill containing 33 kg of Silibeads ZY-E 0.4 / 0.6 mm at a feed flow rate of 82 L / h, a tip speed of 5.0 m / s, and a specific energy of about 55 kWh / t.

[0271] The solid content of the resulting slurry (SRCC6) was 22.9 wt % based on the total weight of the slurry.

[0272] After milling, the surface-reacted calcium carbonate had the properties shown in Table 6 below.

[0273] [Table 6]

[0274] SRCC7 To obtain SRCC7, a weight-based median particle size d of 1.3 μm was measured by sedimentation. 50 350 litres of an aqueous suspension of ground calcium carbonate was prepared in a mixing vessel by adjusting the solids content of ground limestone calcium carbonate from Omya SAS, Orgon, having (wt) to obtain a solids content of 10 wt. % based on the total weight of the aqueous suspension.

[0275] While the slurry was mixed at a speed of 6.2 m / s, 11.2 kg of phosphoric acid in the form of an aqueous solution containing 30% by weight of phosphoric acid was added to the suspension over a period of 20 minutes at a temperature of 70° C. After the acid addition, the slurry was stirred for a further 5 minutes and then removed from the vessel.

[0276] The solid content of the obtained slurry (SRCC7) was 25.2 wt % relative to the total mass of the slurry, and the Brookfield viscosity was 365 mPa·s.

[0277] The properties of the surface-reacted calcium carbonate are summarized in Table 7 below.

[0278] [Table 7]

[0279] SRCC8 A slurry of surface-reacted calcium carbonate (SRCC7) was milled in a Siegmund Linder 200 L vertical stirred media mill containing 250 kg of Silibeads ZY-E 0.4 / 0.6 mm at a feed flow rate of 1775 L / h, a tip speed of 10.0 m / s, and a specific energy of approximately 65.8 kWh / t.

[0280] The solid content of the resulting slurry (SRCC8) was 21.7 wt % based on the total weight of the slurry.

[0281] After milling, the surface-reacted calcium carbonate had the properties shown in Table 8 below.

[0282] [Table 8]

[0283] SRCC9 A slurry of surface-reacted calcium carbonate (SRCC7) was milled in a Siegmund Linder 200 L vertical stirred media mill containing 250 kg of Silibeads ZY-E 0.4 / 0.6 mm at a feed flow rate of 2010 L / h, a tip speed of 10.0 m / s, and a specific energy of approximately 58.1 kWh / t.

[0284] The solid content of the resulting slurry (SRCC9) was 20.1 wt % based on the total weight of the slurry.

[0285] After milling, the surface-reacted calcium carbonate had the properties shown in Table 9 below.

[0286] [Table 9]

[0287] B.Drying The slurries obtained by removing the liquid from the slurries comprising surface-reacted calcium carbonate, namely SRCC1, SRCC2, SRCC3, SRCC4, SRCC5, SRCC6, SRCC8 and SRCC9, were then dried by spray drying using a rotary atomizer, a two-fluid nozzle or a fountain nozzle from GEA-Niro, Denmark.

[0288] The settings used for spray drying are shown in Table 10 below.

[0289] [Table 10]

[0290] The results for the resulting granules are shown in Table 11 below.

[0291] [Table 11]

[0292] Table 12 below shows the relationship between d for (0.5 bar) vs. (0.1 bar) and for (1.5 bar) vs. (0.1 bar). 50 and d 10The table summarizes the granule stability, as determined by the ratio of SRCC1 to SRCC2. From Table 12, it can be seen that the granules prepared by the method including the step of homogenizing an aqueous suspension containing surface-reacted calcium carbonate, i.e., Granules SRCC2, SRCC3, SRCC4, SRCC5, SRCC6, SRCC8, and SRCC9, are more stable than the granules obtained by the same method but without the step of homogenizing an aqueous suspension containing surface-reacted calcium carbonate, i.e., Granule SRCC1. Furthermore, Figures 1-4 show a comparison of SEM results of granules obtained by homogenizing with a homogenizer and spray-drying with a fountain nozzle, i.e., Granules SRCC1, SRCC2, SRCC3, and SRCC4. It should be noted that the SEM results for granules obtained by spray-drying with a rotary atomizer or a two-fluid nozzle are similar. Figure 5 also shows a cross-section of granules obtained by spray drying with a fountain nozzle, i.e., granule SRCC2. Figures 6 and 7 show a comparison of SEM results for granules obtained by homogenization in a mill and spray drying with a rotary atomizer, i.e., granules SRCC5 and SRCC6. Note that the SEM results for granules obtained by spray drying with a fountain nozzle or a two-fluid nozzle are similar. Furthermore, note that the granules prepared by the homogenization process performed on an industrial scale, i.e., granules SRCC8 and SRCC9, show the same granule stability as the granules prepared by the homogenization process performed on a laboratory scale, i.e., granules SRCC2, SRCC3, SRCC4, SRCC5, and SRCC6. Note that although the physical data (friability / bulk density) of the samples after milling may be slightly inferior, their performance is comparable.

[0293] [Table 12]

[0294] The granules prepared according to the present invention were further analyzed for their compactability. For testing, tablets were prepared as follows: First, the resulting granules of SRCC2, SRCC3, SRCC5, and SRCC6 were mixed with croscarmellose in a Turbula Mixer (Willy A., Bachofen, Turbula T10B) for 5 minutes. Subsequently, a lubricant (magnesium stearate, Ligamed MF-2-V, Cas# 557-04-0, Peter Greven) was added, and the resulting mixture was mixed again in a Turbula Mixer (Willy A., Bachofen, Turbula T10B) for 5 minutes. Tablets from two comparative filler samples, one based on tribasic calcium phosphate (tricalcium phosphate) and the other based on dibasic calcium phosphate (calcium hydrogen phosphate), were prepared in the same manner. In contrast, SRCC4 granules were mixed for 5 minutes in a Turbula Mixer (Willy A., Bachofen, Turbula T10B) with lubricant (magnesium stearate, Ligamed MF-2-V, Cas# 557-04-0, Peter Greven). These mixtures were then used to prepare tablets in a Fette 1200i using EU1" tooling with a 10 mm filling cam, eight standard convex round 10 mm punches, and a tableting speed of 10,000 tablets / hour. The filling depth was adjusted to obtain a compression force of 2 kN to 20 kN, and the tablet weight was fixed at 160 mg. Tablets were prepared in the same way from two comparative filler samples: one based on tribasic calcium phosphate (tricalcium phosphate) and the other based on dibasic calcium phosphate (dibasic calcium phosphate).

[0295] Table 13 below shows the amount (by weight) of each ingredient in the tablets prepared.

[0296] [Table 13]

[0297] The tablet hardness [N] of the tablets as a function of the main compression force [kN] is shown in Figure 8. Figure 8 shows the results of tablets prepared from granules prepared according to the present invention by spray drying in a rotary atomizer compared with two commercially available filler samples, one based on tribasic calcium phosphate (tricalcium phosphate) and the other based on dibasic calcium phosphate (calcium hydrogen phosphate). It can be seen that the tablets prepared from the granules prepared according to the present invention show a better relationship between hardness and main compression force and therefore better compressibility compared to the commercially available filler samples. It should be noted that the compressibility results for the granules obtained by spray drying with a fountain nozzle or a two-fluid nozzle are similar to those obtained by spray drying with a rotary atomizer.

[0298] The granules prepared according to the present invention were further analyzed with respect to their disintegration properties.

[0299] Disintegration time was determined using a Pharmatron DisiTest 50 automatic tablet disintegration tester. For the test, a beaker was filled with 700 mL of tap water. The water was heated to 37.0°C, and then six tablets of each sample prepared as described above were placed in a sturdy basket. The device automatically detected and recorded the disintegration time. In addition, the disintegration time was also visually observed.

[0300] Figure 9 shows the disintegration time (seconds) as a function of tablet hardness (N) for tablets prepared from granules prepared according to the invention by spray drying in a rotary atomizer compared with two commercially available filler samples, one based on tribasic calcium phosphate (tricalcium phosphate) and the other based on dibasic calcium phosphate (calcium hydrogen phosphate). It can be seen that tablets prepared from granules prepared according to the invention show a favorable relationship between disintegration time and hardness. It should be noted that the results of the disintegration time vs. hardness relationship for granules obtained by spray drying in a fountain nozzle or a two-fluid nozzle are similar to those obtained by spray drying in a rotary atomizer. The invention disclosed herein includes the following aspects: [1] A method for producing granules containing surface-reacted calcium carbonate, comprising the steps of: (a) providing an aqueous suspension comprising surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is a reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more acids, wherein the carbon dioxide is formed in situ by treatment with the acids and / or is supplied from an external source; (b) homogenizing the aqueous suspension containing the surface-reacted calcium carbonate of step (a); and (c) removing liquid from the aqueous suspension comprising surface-reacted calcium carbonate of step (b) by spray drying to obtain granules comprising surface-reacted calcium carbonate. [2] The method according to [1] above, wherein the natural ground calcium carbonate is selected from calcium carbonate-containing minerals selected from the group consisting of marble, chalk, limestone, and mixtures thereof; and the precipitated calcium carbonate is selected from the group consisting of precipitated calcium carbonate having amorphous, aragonite, vaterite, or calcite mineralogical crystal forms, and mixtures thereof. [3] The method according to [1] or [2] above, wherein the surface-reacted calcium carbonate in the aqueous suspension of step (a) comprises: (a) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and particularly 1 to 10 μm 50 and / or (b) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area. [4] The method according to any one of the above [1] to [3], wherein the aqueous suspension in step (a) has a solids content in the range of 1 to 40 wt %, preferably 5 to 35 wt %, and most preferably 7 to 26 wt %, based on the total weight of the aqueous suspension. [5] adding at least one disintegrant before step (b), and / or during step (b), and / or after step (b); Preferably, the at least one disintegrant is selected from the group comprising croscarmellose sodium, modified cellulose gum, insoluble cross-linked polyvinylpyrrolidone, starch, modified starch, starch glycolates such as sodium starch glycolate, microcrystalline cellulose, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-, hydroxyalkyl-, carboxyalkyl-cellulose esters, alginic acid, microcrystalline cellulose and its polymorphs, ion exchange resins, gums, chitin, chitosan, clay, gellan gum, cross-linked polacrilin copolymer, agar, gelatin, dextrin, acrylic acid polymers, sodium / calcium carboxymethylcellulose, hydroxypropylmethylcellulose phthalate, shellac, effervescent mixtures such as bicarbonate in combination with one or more acids such as citric acid or tartaric acid, and mixtures thereof. The method according to any one of [1] to [4] above. [6] The method according to the above-mentioned [5], wherein the at least one disintegrant is added before step (b), during step (b), and / or after step (b) in an amount ranging from 0.3 to 10 wt%, preferably from 0.5 to 8 wt%, more preferably from 1 to 5 wt%, based on the total dry weight of the surface-reacted calcium carbonate. [7] The method according to any one of the above [1] to [6], wherein the homogenization in step (b) is carried out once or multiple times, preferably 1 to 5 times, more preferably 1 to 3 times. [8] The method according to any one of the above [1] to [7], wherein the homogenization in step (b) is carried out by grinding. [9] The method according to any one of [1] to [7] above, wherein the homogenization in step (b) is carried out by: (a) a pressure in the range of 5 to 90 MPa, preferably 10 to 75 MPa, and most preferably 20 to 65 MPa; and / or (b) an initial temperature in the range of 5 to 95°C, preferably 10 to 80°C, and most preferably 15 to 60°C.

[10] The method according to any one of [1] to [9] above, wherein the spray drying in step (c) is carried out by: (a) a pressure in the range of 0.01 to 30 MPa, preferably 0.5 to 10 MPa, more preferably 0.6 to <5 MPa, and most preferably 0.7 to 2.5 MPa; and / or (b) A temperature measured as an inlet temperature in the range of 150 to 950°C, preferably 175 to 700°C, and most preferably 180 to 550°C.

[11] Granules comprising surface-reacted calcium carbonate, the surface-reacted calcium carbonate is the reaction product of natural ground or precipitated calcium carbonate with carbon dioxide and one or more acids, the carbon dioxide being formed in situ by treatment with the acid and / or supplied from an external source; The granules have a bulk density in the range of 0.25 to 0.70 g / mL, preferably 0.28 to 0.65 g / mL, more preferably 0.30 to 0.60 g / mL, and most preferably 0.35 to 0.60 g / mL. Granules containing surface-reacted calcium carbonate.

[12] The granules according to

[11] above, having: (a) a volume particle size d of 50 to 500 μm, preferably 60 to 400 μm, and most preferably 70 to 350 μm, measured in a dry state by laser diffraction at a dispersion pressure of 0.01 MPa 90 、 (b) a volume median particle size d measured in a dry state by laser diffraction at a dispersion pressure of 0.01 MPa, of 5 to 300 μm, preferably 10 to 200 μm, and most preferably 12 to 175 μm 50 , and (c) a volume particle size d of 1 to 100 μm, preferably 1 to 90 μm, and most preferably 1 to 80 μm, measured in a dry state by laser diffraction at a dispersion pressure of 0.01 MPa 10 and / or (d) Spherical.

[13] Granules according to

[11] or

[12] above, comprising particles of surface-reacted calcium carbonate having: (a) 1m measured using nitrogen and the BET method according to ISO 9277:2010 2 / g~200m 2 / g, preferably 2m 2 / g~150m 2 / g, more preferably 20m 2 / g~140m 2 / g, most preferably 40m 2 / g~70m 2 / g BET specific surface area, and / or (b) a volume median particle size d measured using laser diffraction of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, and especially 1 to 10 μm 50 and / or (c) 0.15–1.60 cm calculated from mercury intrusion porosimetry measurements. 3 / g, preferably 0.30 to 1.50 cm 3 / g, more preferably 0.30 to 1.40 cm 3 / g, most preferably 0.30 to 1.35 cm 3 Intraparticle indented specific pore volume in the range of / g.

[14] The granules comprise at least one disintegrant; Preferably, the at least one disintegrant is selected from the group comprising croscarmellose sodium, modified cellulose gum, insoluble cross-linked polyvinylpyrrolidone, starch, modified starch, starch glycolates such as sodium starch glycolate, microcrystalline cellulose, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-, hydroxyalkyl-, carboxyalkyl-cellulose esters, alginic acid, microcrystalline cellulose and its polymorphs, ion exchange resins, gums, chitin, chitosan, clay, gellan gum, cross-linked polacrilin copolymer, agar, gelatin, dextrin, acrylic acid polymers, sodium / calcium carboxymethylcellulose, hydroxypropylmethylcellulose phthalate, shellac, effervescent mixtures such as bicarbonate in combination with one or more acids such as citric acid or tartaric acid, and mixtures thereof. The granules according to any one of

[11] to

[13] above.

[15] The granules according to

[14] above, wherein the granules contain the at least one disintegrant in an amount ranging from 0.25 to 35% by weight, preferably from 0.5 to 15% by weight, more preferably from 0.5 to 10% by weight, even more preferably from 0.7 to 10% by weight, and most preferably from 0.8 to 10% by weight, based on the total dry weight of the granules.

[16] Granules according to any one of

[11] to

[15] above, obtained by the method according to any one of [1] to [9] above.

[17] Use of the granules according to any one of the above

[11] to

[16] as an excipient in a nutritional supplement product, an agricultural product, an animal product, a cosmetic, preferably a dry cosmetic composition and / or a dry skin care composition, a household product, a food product, a packaging product, or a personal care product, preferably an oral care composition, or in a pharmaceutical product.

Claims

1. A method for producing granules comprising surface-reacted calcium carbonate, comprising the steps of: (a) providing an aqueous suspension comprising surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is a reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more acids, wherein the carbon dioxide is formed in situ by treatment with the acids and / or is supplied from an external source; (b) homogenizing the aqueous suspension containing the surface-reacted calcium carbonate of step (a); and (c) removing liquid from the aqueous suspension comprising surface-reacted calcium carbonate of step (b) by spray drying to obtain granules comprising surface-reacted calcium carbonate.

2. 2. The method of claim 1, wherein the natural ground calcium carbonate is selected from calcium carbonate-containing minerals selected from the group consisting of marble, chalk, limestone, and mixtures thereof; and the precipitated calcium carbonate is selected from the group consisting of precipitated calcium carbonate having amorphous, aragonite, vaterite, or calcite mineralogical crystal forms, and mixtures thereof.

3. 3. The method of claim 1 or 2, wherein the surface-reacted calcium carbonate in the aqueous suspension of step (a) comprises: (a) A volume median particle size d of 0.5 to 50 μm, measured using laser diffraction ５０ and / or (b) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 ２ / g to 200m ２ / g BET specific surface area.

4. 4. The method according to any one of claims 1 to 3, wherein the aqueous suspension of step (a) has a solids content in the range of 1 to 40% by weight, based on the total weight of the aqueous suspension.

5. The method according to any one of claims 1 to 4, wherein at least one disintegrant is added before step (b) and / or during step (b) and / or after step (b).

6. 6. The method according to claim 5, wherein the at least one disintegrant is added before step (b) and / or during step (b) and / or after step (b) in an amount ranging from 0.3 to 10 wt.%, based on the total dry weight of the surface-reacted calcium carbonate.

7. 7. The method according to any one of claims 1 to 6, wherein the homogenization in step (b) is carried out one or more times.

8. The method according to any one of claims 1 to 7, wherein the homogenization in step (b) is carried out by milling.

9. The method according to any one of claims 1 to 7, wherein the homogenization in step (b) is carried out by: (a) a pressure in the range of 5 to 90 MPa, and / or (b) an initial temperature in the range of 5 to 95°C;

10. The method according to any one of claims 1 to 9, wherein the spray drying of step (c) is carried out by: (a) a pressure in the range of 0.01 to 30 MPa, and / or (b) Temperature measured as inlet temperature in the range of 150 to 950°C.

11. 1. Granules comprising surface-reacted calcium carbonate, the surface-reacted calcium carbonate is the reaction product of natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more acids, the carbon dioxide being formed in situ by treatment with the acid and / or supplied from an external source; the granules have a bulk density in the range of 0.25 to 0.70 g / mL; The granules have a volume particle size d 90 of 50 to 500 μm, a volume median particle size d 50 of 5 to 300 μm, and a volume particle size d 10 of 1 to 100 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa. Granules containing surface-reacted calcium carbonate.

12. 12. The granules of claim 11, comprising: (a) A volume particle size d of 60 to 400 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa ９０ , (b) a volume median particle size d of 10 to 200 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa ５０ , and (c) a volume particle size d of 1 to 90 μm, measured in the dry state by laser diffraction at a dispersion pressure of 0.01 MPa １０ and / or (d) Spherical.

13. 13. Granules according to claim 11 or 12, comprising particles of surface-reacted calcium carbonate having: (a) 1 m measured using nitrogen and the BET method according to ISO 9277:2010 ２ / g to 200m ２ / g BET specific surface area, and / or (b) a volume median particle size d of 0.5 to 50 μm, measured using laser diffraction ５０ and / or (c) 0.15 to 1.60 cm calculated from mercury intrusion porosimetry measurements ３ / g range of indented specific pore volume.

14. Granules according to any one of claims 11 to 13, wherein the granules comprise at least one disintegrant.

15. 15. The granules according to claim 14, wherein the granules comprise the at least one disintegrant in an amount ranging from 0.25 to 35% by weight, based on the total dry weight of the granules.

16. Use of the granules of any one of claims 11 to 15 as an excipient in a nutraceutical product, an agricultural product, an animal product, a cosmetic, a household product, a food product, a packaging product or a personal care product, or in a pharmaceutical product.

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