Method for producing free-flowing granules

Abstract

The present invention relates to a process for producing granules comprising surface-reacted calcium carbonate having a bulk density 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 said granules in nutritional products, agricultural products, veterinary products, cosmetic products, preferably dry cosmetic and / or dry skin care compositions, household products, foods, packaged products, or personal care products, preferably oral care compositions, or as an excipient in pharmaceutical products.

Description

[0001] The present invention relates to a process for producing granules comprising surface-reacted calcium carbonate having a bulk density 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 said granules in nutritional products, agricultural products, veterinary products, cosmetic products, preferably dry cosmetic and / or dry skin care compositions, household products, foods, packaged products, or personal care products, preferably oral care compositions, or as an excipient in pharmaceutical products.

[0002] Granules are of considerable importance and are preferred over powders in many applications such as pharmaceutical products, nutritional products, agricultural products, veterinary products, cosmetic products, household products, foods, packaged products, and personal care products. Therefore, powder agglomeration to produce granules typically having a size range of 0.2 mm to 4.0 mm is widely used to improve the physical properties of powders such as wettability, flowability, bulk density, and product appearance, depending on the subsequent use of the granules.

[0003] Furthermore, granulation is carried out, for example, to prevent segregation of the components of a powder mixture, to prevent dust or to improve flow properties.

[0004] Granulation, the process in which primary powder particles are caused to adhere to form a larger multi-particulate entity, is the process of aggregating particles together by creating bonds between the particles, for example via a binder.

[0005] One of the most important types of granulation is wet granulation, in which granules are formed by adding a granulating liquid to a powder bed affected by an impeller. The agitation created within the system together with the wetting of the components within the formulation leads to agglomeration of the primary powder particles to produce a wet granulate. The granulating liquid contains a solvent that must be volatile so that it can be removed by drying and is non-toxic. The water mixed into the powder can form a bond between the powder particles that is strong enough to lock them together. However, once the water dries up, the agglomerates may fall apart. Therefore, the water may not be strong enough to create and maintain a bond. In such a case, the granulating liquid contains a binder.

[0006] About surface-reacted calcium carbonate, also generally known is granular. For example, in EP2264108 A1 (WO2010146530 A1), it is mentioned that the surface-reacted calcium carbonate obtained by the method described therein can be in the form of blocks, granular or powder, and in several documents (EP1975310B1, EP1982759 B1, EP1974807 B1, EP1974806 B1, EP2589430 A1, WO2010037753 A1, EP2719373 A1 or EP2719376 A1) describing different uses of surface-reacted calcium carbonate (e.g. in water purification; as a controlled release carrier; in fast disintegrating dosage forms or gastric retention drug preparations and delivery systems), granular is generally mentioned.

[0007] However, these granules obtained as a result of the basic process for producing surface-reacted calcium carbonate or by (wet) granulation have several disadvantages, such as poor bulk density, flow properties and compactability and low mechanical stability. In addition, wet granulation requires the use of less favorable binders.

[0008] Thus, surface-reacted calcium carbonate can be granulated using various methods, but in the absence of a binder, conventional methods do not provide the desired results, namely high bulk density, flow properties and compactability and high mechanical stability.

[0009] Therefore, one object of the present invention is to provide a method for producing granules comprising surface-reacted calcium carbonate having high bulk density, flow properties and compactability and high mechanical stability. Another object of the present invention is to improve the aforementioned properties without the use of binders.

[0010] One or more of the foregoing and other objects are solved by the subject matter as defined herein in the independent claims. Advantageous embodiments of the invention are defined in the respective dependent claims.

[0011] The present invention therefore relates to a process for producing granules comprising surface-reacted calcium carbonate, said process comprising the following steps:

[0012] 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 acid treatment and / or is supplied from an external source;

[0013] b) homogenizing the aqueous suspension comprising the surface-reacted calcium carbonate of step a), and

[0014] 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.

[0015] 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 an amorphous, aragonite, vaterite or calcite mineralogical crystal form or a mixture thereof.

[0016] According to another embodiment, the surface-reacted calcium carbonate in the aqueous suspension of step a) has a) a volume median particle size d of 0.5 to 50 μm, preferably 0.7 to 25 μm, more preferably 0.8 to 20 μm, in particular 1 to 10 μm, measured by using laser diffraction 50 , and / or b) 1 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m 2 / g to 70m 2 / g BET specific surface area.

[0017] According to yet another embodiment, the solids content of the aqueous suspension of step a) is 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.

[0018] According to one embodiment, at least one disintegrant is added before and / or during and / or after step b), preferably, at least one disintegrant is selected from the group comprising crosslinked sodium carboxymethylcellulose, modified cellulose gum, insoluble crosslinked polyvinyl pyrrolidone, starch, modified starch, starch glycolate such as sodium starch glycolate, microcrystalline cellulose, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-cellulose esters, hydroxyalkyl-cellulose esters, carboxyalkyl-cellulose esters, alginic acid, microcrystalline cellulose and its polymorphs, ion exchange resins, gums, chitin, chitosan, clay, gellan gum, crosslinked polacrilin copolymers, agar, gelatin, dextrin, acrylic acid polymers, sodium carboxymethylcellulose / calcium carboxymethylcellulose, hydroxypropyl methylcellulose phthalate, shellac, effervescent mixtures such as bicarbonate in combination with one or more acids such as citric acid or tartaric acid, or mixtures thereof.

[0019] According to another embodiment, at least one disintegrant is added before and / or during and / or after step b) in an amount of 0.3 to 10 wt.-%, preferably 0.5 to 8 wt.-%, more preferably 1 to about 5 wt.-%, based on the total dry weight of the surface-reacted calcium carbonate.

[0020] According to yet another embodiment, the homogenization in step b) is performed once or several times, preferably 1 to 5 times, more preferably 1 to 3 times.

[0021] According to yet another embodiment, the homogenization in step b) is performed by milling.

[0022] According to one embodiment, the homogenization in step b) is carried out at a) a pressure of 50 to 900 bar, preferably 100 to 750 bar, and most preferably 200 to 650 bar; and / or b) an initial temperature of 5 to 95°C, preferably 10 to 80°C, and most preferably 15 to 60°C.

[0023] According to another embodiment, the spray drying in step c) is carried out at a) a pressure of 0.1 bar to 300 bar, preferably 5 bar to 100 bar, more preferably 6 bar to <50 bar, and most preferably 7 bar to 25 bar; and / or b) a temperature of 150°C to 950°C, preferably 175°C to 700°C, and most preferably 180°C to 550°C, measured as inlet temperature.

[0024] According to another aspect, there is provided a granulate 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 supplied by an external source, the bulk density of the granulate being 0.25 g / mL to 0.70 g / mL, preferably 0.28 g / mL to 0.65 g / mL, more preferably 0.30 g / mL to 0.60 g / mL, and most preferably 0.35 g / mL to 0.60 g / mL.

[0025] According to one embodiment, the granulate has a) a volume particle size d as measured by laser diffraction dry at 0.1 bar dispersion pressure of 50 to 500 μm, preferably 60 to 400 μm, and most preferably 70 to 350 μm 90 b) a volume median particle size d of 5 μm to 300 μm, preferably 10 μm to 200 μm, and most preferably 12 μm to 175 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 50 and c) a volume particle size d of 1 μm to 100 μm, preferably 1 μm to 90 μm, and most preferably 1 μm to 80 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 10 ; and / or d) spherical shape.

[0026] According to another embodiment, the granulate comprises particles of surface-reacted calcium carbonate having: a) a 1 m 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m 2 / g to 70m 2 / g BET specific surface area; and / or b) a volume median particle size d of 0.5 μm to 50 μm, preferably 0.7 μm to 25 μm, more preferably 0.8 μm to 20 μm, especially 1 μm to 10 μm measured by using laser diffraction 50 and / or c) mercury intrusion porosimetry at 0.15 cm 3 / g to 1.60cm 3 / g, preferably 0.30cm 3 / g to 1.50crn 3 / g, more preferably 0.30cm 3 / g to 1.40cm 3 / g, and most preferably 0.30cm 3 / g to 1.35cm 3 / g range of the intrusion specific pore volume within the particles.

[0027] According to yet another embodiment, the granules comprise at least one disintegrant, preferably, at least one disintegrant is selected from the group comprising crosslinked sodium carboxymethylcellulose, modified cellulose gum, insoluble crosslinked polyvinyl pyrrolidone, starch, modified starch, glycolic acid starch salts such as sodium starch glycolate, microcrystalline cellulose, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-cellulose esters, hydroxyalkyl-cellulose esters, carboxyalkyl-cellulose esters, alginates, microcrystalline cellulose and its polymorphs, ion exchange resins, gums, chitin, chitosan, clays, gellan gum, crosslinked polacrilin copolymers, agar, gelatin, dextrin, acrylic acid polymers, sodium carboxymethylcellulose / calcium carboxymethylcellulose, hydroxypropyl methylcellulose phthalate, shellac, effervescent mixtures such as bicarbonate in combination with one or more acids such as citric acid or tartaric acid, or mixtures thereof.

[0028] According to one embodiment, the granulate comprises the at least one disintegrant in an amount of 0.25 to 35 wt.-%, preferably 0.5 to 15 wt.-%, more preferably 0.5 to 10 wt.-%, even more preferably 0.7 to 10 wt.-%, most preferably 0.8 to 10 wt.-%, based on the total dry weight of the granulate.

[0029] According to another embodiment, the granulate is obtained by the process as defined herein.

[0030] According to another aspect, there is provided the use of a granulate as defined herein in a nutritional product, an agricultural product, a veterinary product, a cosmetic product, preferably a dry cosmetic and / or a dry skin care composition, a household product, a food, a packaged product, or a personal care product, preferably an oral care composition, or as an excipient in a pharmaceutical product.

[0031] It should be understood that for the purposes of the present invention, the following terms have the following meanings.

[0032] The term "surface-reacted" is used in the meaning of the present application to indicate that a material has been subjected to a process comprising reacting the material with H3O in an aqueous environment. + The ion donor treatment (eg, by using a water-soluble free acid and / or acid salt) results in partial dissolution of the material, followed by a crystallization process, which may occur in the absence or presence of additional crystallization additives.

[0033] In the context of the present invention, "H3O +Brønsted Acids and / or acid salts, i.e. salts containing an acidic hydrogen.

[0034] The term "acid" as used herein refers to an acid (e.g., H2SO4, HSO4) within the meaning defined by Bronsted and Lowry. - ).

[0035] "Water-insoluble" materials are defined within the meaning of the present invention as materials that, when mixed with deionized water and filtered at 20°C on a filter having a pore size of 0.2 μm to recover a liquid filtrate, provide less than or equal to 0.1 g of recovered solid material after evaporation of 100 g of said liquid filtrate at 95°C to 100°C. "Water-soluble" materials are defined as materials that result in the recovery of greater than 0.1 g of recovered solid material after evaporation of 100 g of said liquid filtrate at 95°C to 100°C.

[0036] "Natural ground calcium carbonate" (GCC) in the meaning of the present invention is calcium carbonate obtained from natural sources such as limestone, marble or chalk and processed by wet and / or dry processing such as grinding, sieving and / or classifying (e.g. by cyclones or classifiers).

[0037] "Precipitated calcium carbonate" (PCC) in the meaning of the present invention is a synthetic material obtained by precipitation after reaction of carbon dioxide and lime in an aqueous, semi-dry or moist environment or by precipitation of calcium and a carbonate ion source in water. PCC can be in amorphous, vaterite, calcite or aragonite crystalline form.

[0038] BET specific surface area is defined in the meaning of the present invention as the surface area of ​​a particle divided by the mass of the particle. As used herein, specific surface area is measured by adsorption using the BET isotherm (ISO 9277:2010) and is expressed in m 2 / g indicates.

[0039] When the term "comprises / comprising" is used in the present description and claims, it does not exclude other elements. For the purpose of the present invention, the term "consisting of" is considered to be a preferred embodiment of the term "comprises / comprising". If a group is defined hereinafter as comprising / comprising at least a certain number of embodiments, this is also to be understood as disclosing a group that preferably consists of only these embodiments.

[0040] Where an indefinite or definite article is used when referring to a singular noun eg "a", "an" or "the", this includes a plural of that noun, unless something else is specifically stated sometimes.

[0041] Terms such as "obtainable" or "definable" and "obtained" or "definable" are used interchangeably. Unless the context clearly dictates otherwise, this means, for example, that the term "obtained" is not intended to indicate, for example, that an embodiment must be obtained by, for example, following the sequence of steps of the term "obtained", although such a restrictive understanding is always included as a preferred embodiment by the term "obtained" or "definable".

[0042] According to the present invention, the process for producing granules comprising surface-reacted calcium carbonate necessarily comprises the following steps:

[0043] 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 acid treatment and / or is supplied from an external source;

[0044] b) homogenizing the aqueous suspension comprising the surface-reacted calcium carbonate of step a), and

[0045] 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.

[0046] In particular, it was found 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 compactibility and high mechanical stability.

[0047] In the following, further details of the present invention are mentioned, in particular the aforementioned process for producing granules comprising surface-reacted calcium carbonate.

[0048] One requirement of the present invention is that, according to step a), an aqueous suspension comprising surface-reacted calcium carbonate is provided, 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 supplied from an external source, preferably the carbon dioxide is formed in situ by acid treatment.

[0049] Surface-reacted calcium carbonate is natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more H3O + The reaction product of the ion donor in an aqueous medium, in which carbon dioxide is reacted with H3O + The ion donor is formed in situ and / or supplied from an external source. Preferably, the surface-reacted calcium carbonate is natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more H3O +The reaction product of the ion donor in an aqueous medium, in which carbon dioxide is reacted with H3O + The ion donor is formed in situ or supplied from an external source. More preferably, the surface-reacted calcium carbonate is natural ground calcium carbonate or precipitated calcium carbonate with carbon dioxide and one or more H3O + The reaction product of the ion donor in an aqueous medium, in which carbon dioxide is reacted with H3O + Ion donor treatment is formed in situ.

[0050] In the context of the present invention, H3O + The ion donor is a Bronsted acid and / or an acid salt.

[0051] 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 calcium carbonate or precipitated calcium carbonate; (b) adding to the suspension of step (a) a calcium carbonate having a pK at 20°C; a1 A value of 0 or less or a pK value of 0 or less at 20°C a1 (a) a calcium carbonate having a pK value of 0 to 2.5; 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 calcium carbonate or precipitated calcium carbonate; (B) providing at least one water-soluble acid; (C) providing gaseous CO2; and (D) contacting the natural calcium carbonate or precipitated calcium carbonate of step (A) with the at least one acid of step (B) and the CO2 of step (C), characterized in that: (i) the at least one acid of step B) has a pK value of 0.5 for the ionization of its first available hydrogen at 20°C. a1 greater than 2.5 and less than or equal to 7, and upon losing the first available hydrogen forms a corresponding anion capable of forming a water-soluble calcium salt, and (ii) after contacting the at least one acid with natural calcium carbonate or precipitated calcium carbonate, additionally provides at least one water-soluble salt having a pK at 20° C. in the case of a hydrogen-containing salt. a1 is greater than 7, and the salt anion of the water-soluble salt is capable of forming a water-insoluble calcium salt.

[0052] "Natural ground calcium carbonate" (GCC) is preferably selected from calcium carbonate-containing minerals selected from the group comprising marble, chalk, limestone and mixtures thereof. Natural calcium carbonate may contain additional naturally occurring components, such as aluminum silicate and the like.

[0053] Usually, the grinding of natural heavy calcium carbonate can be dry grinding or wet grinding step, and can be carried out with any conventional grinding device, for example, under the condition that pulverization is mainly caused by the impact with the second object, that is, in one or more of the following: ball mill, rod mill, vibrating mill, roller crusher, centrifugal impact mill, vertical bead mill, grinding machine, pin mill, hammer mill, pulverizer, shredder, deblocking machine (de-clumper), knife cutter or other such equipment known to the technician. In the case where the calcium carbonate-containing mineral material comprises the calcium carbonate-containing mineral material through wet grinding, the grinding step can be carried out under the condition that autogenous grinding occurs and / or by horizontal ball milling and / or vertical ball milling and / or other such methods known to the technician. The calcium carbonate-containing mineral material ground through wet treatment thus obtained can be washed and dehydrated by a known process (for example, by flocculation, filtration or forced evaporation) before drying. Subsequent drying step (if necessary) can be carried out with a single step (for example spray drying) or with at least two steps. It is also common to subject such mineral materials to beneficiation steps, such as flotation, bleaching or magnetic separation steps, to remove impurities.

[0054] "Precipitated calcium carbonate" (PCC) is a synthetic material in the sense of the present invention, which is usually precipitated after reaction of carbon dioxide and calcium hydroxide in an aqueous environment or obtained by precipitation of calcium ions and carbonate ions provided in the form of water-soluble salts (e.g., CaCl and NaCO) from solution. Another possible method for producing PCC is the lime soda process or the Solvay process in which PCC is a by-product of ammonia production. Precipitated calcium carbonate exists in three main crystalline forms: calcite, aragonite and vaterite, and each of these crystalline forms has many different polymorphs (crystal habits). Calcite has a trigonal structure, and its typical crystal habits are, for example, scalenohedral (S-PCC), rhombohedral (R-PCC), hexagonal prism, axonohedral, colloidal (C-PCC), cubic and prismatic (P-PCC). Aragonite has an orthorhombic structure, and its typical crystal habit is twinned hexagonal prism crystals, as well as various types of slender prisms, curved blades, steep pyramids, chisel-shaped crystals, branched trees, and coral or worm-like forms. Hexagonal calcium carbonate belongs to the hexagonal crystal system. The obtained PCC slurry can be mechanically dehydrated and dried.

[0055] According to one embodiment of the present invention, the precipitated calcium carbonate is a precipitated calcium carbonate preferably comprising an amorphous, aragonite, vaterite or calcite mineralogical crystal form, or a mixture thereof.

[0056] Calcium carbonate can be precipitated by mixing carbon dioxide and at least one H3O + The ion donor is prior to treatment by grinding in the same manner as described above for ground natural calcium carbonate.

[0057] According to one embodiment of the present invention, the natural calcium carbonate or precipitated calcium carbonate has a weight median particle size d 50 0.05 μm to 10.0 μm, preferably 0.2 μm to 5.0 μm, more preferably 0.4 μm to 3.0 μm, most preferably 0.6 μm to 1.2 μm, especially 0.7 μm. According to another embodiment of the present invention, the natural calcium carbonate or precipitated calcium carbonate is in the form of particles with a top cut particle size d 98 The particle size is in the range of 0.15 μm to 55 μm, preferably 1 μm to 40 μm, more preferably 2 μm to 25 μm, most preferably 3 μm to 15 μm, especially 4 μm.

[0058] Natural calcium carbonate and / or precipitated calcium carbonate can be used dry or suspended in water. Preferably, the corresponding slurry has a content of natural calcium carbonate or precipitated calcium carbonate in the following range: based on the weight of the slurry, 1 wt % to 90 wt %, more preferably 3 wt % to 60 wt %, even more preferably 5 wt % to 40 wt %, and most preferably 10 wt % to 25 wt %.

[0059] One or more H3O for preparing surface-reacted calcium carbonate + The ion donor can be H3O generated under preparation conditions. + ions, or any strong, medium or weak acid, or mixtures thereof. According to the present invention, at least one H3O + The ion donor can also generate H3O under preparation conditions. + Acidic salts of ions.

[0060] According to one embodiment, at least one H3O + The ion donor has a pK at 20°C. a1 A strong acid of 0 or less.

[0061] According to another embodiment, at least one H3O + The ion donor has a pK at 20°C. a1 A medium-strong acid with a pK value between 0 and 2.5. a1 is 0 or less, the acid is preferably selected from sulfuric acid, hydrochloric acid or a mixture thereof. If the pK at 20°C a1 0 to 2.5, then H3O + The ion donor is preferably selected from H2SO3, H3PO4, oxalic acid or a mixture thereof. + The ion donor may also be an acid salt, for example, a salt of a corresponding cation such as Li + 、Na + or K + At least partially neutralized HSO4 -or H2PO4 - ; or by corresponding cations such as Li + 、Na + , K + Mg 2+ or Ca 2+ At least partially neutralized HPO4 2- . At least one H3O + The ion donor may also be a mixture of one or more acids and one or more acid salts.

[0062] According to yet another embodiment, at least one H3O + The ion donor has a pK when measured at 20°C. a1 A weak acid having a pK value greater than 2.5 and less than or equal to 7 and having a corresponding anion capable of forming a water-soluble calcium salt. Subsequently, at least one water-soluble salt is additionally provided, which in the case of a hydrogen-containing salt has a pK value of greater than 2.5 and less than or equal to 7 when measured at 20°C. a1 Greater than 7, and its salt anion can form a water-insoluble calcium salt. According to this preferred embodiment, the pK of the weak acid at 20°C a1 The value is greater than 2.5 to 5, and more preferably, the weak acid is selected from acetic acid, formic acid, propionic acid and mixtures thereof. Exemplary cations of the water-soluble salt are selected from 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 phosphate, dihydrogen phosphate, monohydrogen phosphate, oxalate, silicate, mixtures thereof and hydrates thereof. In a more preferred embodiment, the anion is selected from phosphate, dihydrogen phosphate, monohydrogen phosphate, mixtures thereof and hydrates thereof. In a most preferred embodiment, the anion is selected from 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 preferably occurs within a time period of 10 minutes. More preferably, the salt is added in one step.

[0063] According to one embodiment of the present invention, at least one H3O + The ion donor is selected from hydrochloric acid, sulfuric acid, sulfurous acid, phosphoric acid, citric acid, oxalic acid, acetic acid, formic acid and mixtures thereof. Preferably, at least one H3O + The ion donor is selected from hydrochloric acid, sulfuric acid, sulfurous acid, phosphoric acid, oxalic acid, + 、Na + or K + ) at least partially neutralized H2PO4 - , by the corresponding cations (e.g. Li + 、Na + , K + Mg 2+ or Ca2+ ) at least partially neutralized HPO4 2- , and mixtures thereof; more preferably, at least one acid is selected from hydrochloric acid, sulfuric acid, sulfurous acid, phosphoric acid, oxalic acid or mixtures thereof, and most preferably, at least one H3O + The ion donor is phosphoric acid.

[0064] One or more H3O + The ion donor can be added to the suspension as a concentrated solution or a more dilute solution. Preferably, H3O + The molar ratio of ion donor to natural calcium carbonate or precipitated calcium carbonate is from 0.01 to 4, more preferably from 0.02 to 2, even more preferably from 0.05 to 1, and most preferably from 0.1 to 0.58.

[0065] As an alternative, H3O can also be added before suspending the natural calcium carbonate or precipitated calcium carbonate. + An ion donor is added to the water.

[0066] In a preferred embodiment, the surface-reacted calcium carbonate is natural ground calcium carbonate with carbon dioxide and one or more H3O + The reaction product of the ion donor in an aqueous medium, in which carbon dioxide is reacted with H3O + The ion donor process forms in situ and wherein H3O + The ion donor is phosphoric acid. In a more preferred embodiment, the surface-reacted calcium carbonate is a calcium carbonate-containing mineral with carbon dioxide and one or more H3O + The reaction product of an ion donor in an aqueous medium, the calcium carbonate-containing mineral being selected from the group consisting of marble, chalk, limestone and mixtures thereof, wherein carbon dioxide is reacted by H3O + Ion donor treatment in situ formation and H3O + The ion donor is phosphoric acid.

[0067] In the next step, the natural calcium carbonate or precipitated calcium carbonate is treated with carbon dioxide. If a strong acid such as sulfuric acid or hydrochloric acid is used for the H3O2 of the natural calcium carbonate or precipitated calcium carbonate, + Alternatively or additionally, carbon dioxide may be supplied by an external source.

[0068] H3O + The ion donor treatment and the treatment with carbon dioxide can be carried out simultaneously, which is the case when using strong or medium-strong acids. It is also possible to first use, for example, a solution with a pK at 20°C. a1 Medium to strong acid in the range of 0 to 2.5 H3O + Ion donor processes, where CO2 is formed in situ and therefore the CO2 process will automatically react with H3O +The ion donor treatment is carried out simultaneously, followed by an additional treatment with carbon dioxide supplied from an external source.

[0069] In a preferred embodiment, H3O + The ion donor treatment step and / or the carbon dioxide treatment step are repeated at least once, more preferably several times. According to one embodiment, at least one H3O is added for a period of at least about 5 minutes, preferably at least about 10 minutes, typically about 10 minutes to about 20 minutes, more preferably about 30 minutes, even more preferably about 45 minutes, sometimes about 1 hour or longer. + ion donor.

[0070] In H3O + After the ion donor treatment and the carbon dioxide treatment, the pH of the aqueous suspension measured at 20°C naturally reaches a value of greater than 6.0, preferably greater than 6.5, more preferably greater than 7.0, even more preferably greater than 7.5, thereby preparing a surface-reacted natural calcium carbonate or precipitated calcium carbonate in the form of an aqueous suspension with a pH of greater than 6.0, preferably greater than 6.5, more preferably greater than 7.0, even more preferably greater than 7.5.

[0071] Further details on the preparation of surface-reacted natural calcium carbonate are disclosed in WO0039222 A1, WO2004083316 A1, WO2005121257 A2, WO2009074492 A1, EP2264108 A1, EP2264109 A1 and US20040020410 A1, the contents of these references are hereby included in the present application.

[0072] Similarly, a surface-reacted precipitated calcium carbonate is obtained. As can be seen in detail from WO2009074492 A1, the surface-reacted precipitated calcium carbonate is obtained by reacting the precipitated calcium carbonate with H3O + The invention relates to a method for preparing a surface-reacted precipitated calcium carbonate, wherein the surface-reacted precipitated calcium carbonate comprises an at least partially crystallized insoluble calcium salt of the anion formed on the surface of at least part of the precipitated calcium carbonate, and contacting the anion with an anion dissolved in the aqueous medium and capable of forming a water-insoluble calcium salt in an aqueous medium to form a slurry of surface-reacted precipitated calcium carbonate, wherein the surface-reacted precipitated calcium carbonate comprises an at least partially crystallized insoluble calcium salt of the anion formed on the surface of at least part of the precipitated calcium carbonate.

[0073] The dissolved calcium ions correspond to the precipitated calcium carbonate by H3O + When the ions are dissolved, the dissolved calcium ions are in excess of the naturally occurring dissolved calcium ions, wherein the H3O + The ion is provided only in the form of a counterion to the anion (ie, by addition of an acid or non-calcium acid salt form of the anion) and in the absence of any other calcium ions or sources of calcium ion generation.

[0074] The excess dissolved 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 which generates a soluble neutral or acidic calcium salt in situ.

[0075] The H3O + The ions may be provided by adding an acid or acid salt of the anion, or by adding an acid or acid salt that simultaneously provides all or a portion of the excess dissolved calcium ions.

[0076] In another preferred embodiment of the preparation of surface-reacted natural calcium carbonate or precipitated calcium carbonate, natural 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, silicon dioxide, aluminum hydroxide, alkaline earth aluminates such as sodium aluminate or potassium aluminate, or mixtures thereof. Preferably, 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 natural calcium carbonate or precipitated calcium carbonate before the addition of acid and / or carbon dioxide.

[0077] Alternatively, the silicate and / or silicon dioxide and / or aluminum hydroxide and / or alkaline earth aluminate components can be added to the aqueous suspension of natural calcium carbonate or precipitated calcium carbonate when the reaction of natural calcium carbonate or precipitated calcium carbonate with acid and carbon dioxide has already begun. More details on the preparation of surface-reacted natural calcium carbonate or precipitated calcium carbonate in the presence of at least one silicate and / or silicon dioxide and / or aluminum hydroxide and / or alkaline earth aluminate component are disclosed in WO2004083316 A1, the content of which is hereby included in the present application.

[0078] The surface-reacted calcium carbonate can be kept in suspension, optionally further stabilized by a dispersant. Conventional dispersants known to the skilled person can be used. Preferred dispersants include polyacrylic acid and / or carboxymethyl cellulose.

[0079] Alternatively, the aqueous suspension may be dried to obtain a solid (ie, dry or containing a very small amount of water and not in a fluid form) surface-reacted natural calcium carbonate or precipitated calcium carbonate in the form of granules or powder.

[0080] In a preferred embodiment, the BET specific surface area of ​​the surface-reacted calcium carbonate measured using nitrogen and the BET method according to ISO 9277:2010 is 1 m 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m2 / g to 70m 2 / g.

[0081] It is also preferred that the volume median particle size d of the surface-reacted calcium carbonate particles measured by laser diffraction is 50 (or d 50 The particle size (volume) is 0.5 μm to 50 μm, preferably 0.7 μm to 25 μm, more preferably 0.8 μm to 20 μm, particularly 1 μm to 10 μm.

[0082] According to an exemplary embodiment, the surface-reacted calcium carbonate has:

[0083] a) a volume median particle size d of 0.5 μm to 50 μm, preferably 0.7 μm to 25 μm, more preferably 0.8 μm to 20 μm, especially 1 μm to 10 μm, measured by using laser diffraction 50 , and / or

[0084] b) 1 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m 2 / g to 70m 2 / g BET specific surface area.

[0085] Preferably, the surface-reacted calcium carbonate has:

[0086] a) a volume median particle size d of 0.5 μm to 50 μm, preferably 0.7 μm to 25 μm, more preferably 0.8 μm to 20 μm, especially 1 μm to 10 μm, measured by using laser diffraction 50 ,or

[0087] b) 1 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m 2 / g to 70m 2 / g BET specific surface area.

[0088] Alternatively, the surface-reacted calcium carbonate has:

[0089] a) a volume median particle size d50 of 0.5 μm to 50 μm, preferably 0.7 μm to 25 μm, more preferably 0.8 μm to 20 μm, especially 1 μm to 10 μm, as measured by using laser diffraction, and

[0090] b) 1 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m 2 / g to 70m 2 / g BET specific surface area.

[0091] Furthermore, it is preferred that the volume particle size d of the surface-reacted calcium carbonate particles is 98 (or d 98 The particle size (volume)) is 2 μm to 150 μm, preferably 4 μm to 100 μm, more preferably 6 μm to 80 μm, even more preferably 8 μm to 60 μm, and most preferably 10 μm to 30 μm.

[0092] Value d x represents the diameter at which x% of the particles have a diameter smaller than d x This means that 98 The value is the particle size that is smaller than 98% of all particles. 98 Values ​​are also designated as "top cut". d x Values ​​can be given as volume or weight percentage. Thus, d 50 The (weight) value is the weight median particle size, that is, 50% by weight of all particles are smaller than this size, and d 50 The (volume) value is the volume median particle size, ie, the particle size below which 50% by volume of all particles are smaller.

[0093] The "particle size" of the surface-reacted calcium carbonate herein is described as a particle size distribution based on volume. The "particle size" of the granules herein is described as a particle size distribution based on volume. Furthermore, the "particle size" of the surface-reacted calcium carbonate in the meaning of the present invention refers to the primary particle size.

[0094] Volume median particle size d 50 The d was measured using a Malvern Mastersizer 2000 or 3000 laser diffraction system.10 d 50 or 98 The value indicates the diameter value such that 10%, 50% or 98% by volume of the particles have a diameter smaller than this value, respectively. The raw data obtained by this measurement was analyzed using Mie theory, with a particle refractive index of 1.57 and an absorption index of 0.005.

[0095] Throughout the present invention, the volume-based particle size distribution is determined by laser diffraction.For example, the volume-based particle size distribution of a granulate is measured by laser diffraction dry at 0.1 bar dispersion pressure, as described in detail herein below in the Examples.

[0096] Preferably, the intrusion specific pore volume within the particle of the surface-reacted calcium carbonate calculated by mercury intrusion porosimetry is within 0.15 cm 3 / g to 1.60cm 3 / g, preferably 0.30cm 3 / g to 1.50cm 3 / g, more preferably 0.30cm 3 / g to 1.40cm 3 / g, and most preferably 0.30cm 3 / g to 1.35cm 3 / g range.

[0097] The specific pore volume was 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 equilibrium time used for each pressure step was 20 seconds. The sample material was sealed in a 5 cm 3 The 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).

[0098] The total pore volume seen in the cumulative intrusion data can be divided into two regions, where the intrusion data from 214μm down to about 1μm to 4μm shows that the coarse packing of the sample between any agglomerate structures plays an important role. Smaller than these diameters is the fine inter-particle packing of the particles themselves. If they also have intra-particle pores, this region appears bimodal, and by taking the specific pore volume in pores finer than the peak inflection point (i.e., finer than the bimodal inflection point) intruded by mercury, we thereby define the specific intra-particle pore volume. The sum of these three regions gives the total overall pore volume of the powder, but is strongly dependent on the original sample compaction / settling of the powder at the coarse pore end of the distribution.

[0099] By taking the first derivative of the cumulative intrusion curve, the pore size distribution based on the equivalent Laplace diameter is revealed (inevitably including pore shielding). The differential curve clearly shows the coarse agglomerate pore structure region, the inter-particle pore region, and the intra-particle pore region (if present). Knowing the intra-particle pore diameter range, the remaining inter-particle pore volume and the inter-agglomerate pore volume can be subtracted from the total pore volume to provide the desired pore volume of the internal pores alone, in terms of pore volume per unit mass (specific pore volume). Of course, the same subtraction principle applies to separating any other pore size regions of interest.

[0100] The particle internal pore size of the surface-reacted calcium carbonate determined by mercury porosimetry is preferably in the range of 0.004 to 1.6 μm, more preferably in the range of 0.005 to 1.3 μm, particularly preferably in the range of 0.006 to 1.15 μm and most preferably in the range of 0.007 to 1.0 μm.

[0101] The surface-reacted calcium carbonate comprises an at least partially crystalline water-insoluble calcium salt of an anion of at least one acid formed on the surface of natural ground calcium carbonate or precipitated calcium carbonate. According to one embodiment, the at least partially crystalline water-insoluble salt of an anion of at least one acid at least partially, preferably completely covers the surface of natural ground calcium carbonate or precipitated calcium carbonate. Depending on the at least one acid used, the anion can be sulfate, sulfite, phosphate, citrate, oxalate, acetate, formate and / or chloride.

[0102] As mentioned above, the surface-reacted calcium carbonate is provided in the form of an aqueous suspension.

[0103] Preferably, the solids content of the aqueous suspension of step a) is 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.

[0104] 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 are present in solid form in the liquid. An aqueous suspension is more viscous than the liquid from which it is formed and may have a higher density.

[0105] "Liquid" is usually an "aqueous solvent", which 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 invention, based on the gross weight of the aqueous solvent, the liquid comprises water in an amount of at least 80 wt %, preferably at least 90 wt %, more preferably at least 95 wt %, even more preferably at least 99 wt %. Preferably, the aqueous solvent consists of water, i.e., based on the gross weight of the liquid, the amount of water is 100 wt %.

[0106] It is further preferred that the aqueous suspension provided in step a) has a Brookfield viscosity at a temperature of +23°C (±2°C) at 100 rpm of from 25 mPas to 1000 mPas, preferably from 25 mPas to 700 mPas at +23°C (±2°C), more preferably from 25 mPas to 500 mPas at +23°C (±2°C), and most preferably from 50 mPas to 300 mPas at +23°C (±2°C).

[0107] According to step b) of the process of the invention, the aqueous suspension comprising the surface-reacted calcium carbonate of step a) is homogenized.

[0108] "Homogenization" in the meaning of the present invention is a step in which the particles of surface-reacted calcium carbonate in the aqueous suspension of step a) are brought into aggregates which are stronger in terms of granular stability after drying.

[0109] Homogenization can be performed using a variety of methods known in the art.

[0110] The homogenizing device can be selected from conventionally used devices for homogenizing purposes. Thus, the homogenizing device can be selected from the group comprising piston pumps, high shear devices, etc. For example, GEA Ariete NS3055 of GEA Mechanical Equiprnent Italia SpA can be used for homogenization in step b).

[0111] Alternatively, the homogenization in step b) is carried out by grinding. The homogenization in step b) can be carried out in a grinding or kneading device known in the art. Therefore, the grinding or kneading device can be selected from horizontal and vertical mills conventionally used for grinding purposes or kneaders conventionally used for kneading purposes. For example, the grinding 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.

[0112] It may be noted that, depending on the method used, there may be differences in the particle size distribution to be achieved.

[0113] The homogenization in step b) is performed once or several times. It should be understood that the number of times for performing step b) depends mainly on the pressure used and the surface-reacted calcium carbonate particles obtained in step b). Therefore, the technician can easily adjust the number of times for performing step b) according to the equipment or conditions used during step b). Therefore, the homogenization in step b) can be performed in a recirculation mode.

[0114] Preferably, the homogenization in step b) is performed 1 to 5 times, more preferably 1 to 3 times, ie 1 time, 2 times or 3 times, even more preferably 1 time or 2 times. More preferably, the homogenization in step b) is performed twice.

[0115] It will be appreciated that the homogenization in step b) is preferably performed by using a high pressure homogenizer.

[0116] In one embodiment, the homogenization in step b) is carried out at a pressure of 50 to 900 bar, preferably 100 to 750 bar, and most preferably 200 to 650 bar.

[0117] Additionally or alternatively, the homogenization in step b) is performed at an initial temperature of 5 to 95°C, preferably 10 to 80°C, and most preferably 15 to 60°C.

[0118] Therefore, preferably, the homogenization in step b) is carried out in the following manner:

[0119] a) a pressure of 50 to 900 bar, preferably 100 to 750 bar, and most preferably 200 to 650 bar, or

[0120] b) an initial temperature of 5°C to 95°C, preferably 10°C to 80°C, and most preferably 15°C to 60°C.

[0121] More preferably, the homogenization in step b) is carried out in the following manner:

[0122] a) a pressure of 50 to 900 bar, preferably 100 to 750 bar, and most preferably 200 to 650 bar, and

[0123] b) an initial temperature of 5°C to 95°C, preferably 10°C to 80°C, and most preferably 15°C to 60°C.

[0124] Preferably, in step b), the solids content of the aqueous suspension is 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.

[0125] It will be appreciated that the homogenization in step b) may result in an increase in the solids content of the aqueous suspension compared to the aqueous suspension subjected to step b). For example, the solids content of the aqueous suspension obtained in the homogenization step b) may be at least 1%, more preferably at least 2% and most preferably at least 3%, e.g. 3% to 4%, higher than the solids content of the aqueous suspension subjected to step b). This applies in particular if step b) is carried out in a homogenizer.

[0126] If step b) is performed by grinding, the solids content of the aqueous suspension obtained in the homogenization step b) is preferably 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).

[0127] It will be appreciated that homogenization by grinding is preferably carried out at a specific energy of 25 to 125 kWh / tonne to dry product, preferably 35 to 100 kWh / tonne to dry product.

[0128] Additionally or alternatively, homogenization by grinding is performed at an initial temperature of 5 to 95°C, preferably 10 to 80°C, and most preferably 15 to 60°C.

[0129] Therefore, preferably, the homogenization by grinding in step b) is carried out in the following:

[0130] c) a specific energy of 25 kWh / ton to 125 kWh / ton dry product, preferably 35 kWh / ton to 100 kWh / ton dry product, or

[0131] d) an initial temperature of 5°C to 95°C, preferably 10°C to 80°C, and most preferably 15°C to 60°C.

[0132] More preferably, the homogenization by grinding in step b) is carried out in the following:

[0133] c) a specific energy of 25 kWh / ton to 125 kWh / ton dry product, preferably 35 kWh / ton to 100 kWh / ton dry product, and

[0134] d) an initial temperature of 5°C to 95°C, preferably 10°C to 80°C, and most preferably 15°C to 60°C.

[0135] In one embodiment, at least one disintegrant is added before and / or during and / or after step b). Preferably, at least one disintegrant is added before or during or after step b), more preferably before or after step b). More preferably, at least one disintegrant is added after step b).

[0136] In one embodiment of the invention, at least one disintegrant comprises one disintegrant, preferably consists of one disintegrant. Alternatively, at least one disintegrant comprises two or more disintegrants, preferably consists of two or more disintegrants. For example, at least one disintegrant comprises two or three disintegrants, preferably consists of two or three disintegrants.

[0137] Preferably, the at least one disintegrant comprises, preferably consists of, one disintegrant.

[0138] It should be noted that disintegrants that can be used in the method of the present invention are generally those well known in the art of granulation.

[0139] It should be noted that any compound that is known as a disintegrant or that can function as a disintegrant can be used in the methods of the present invention.

[0140] In a preferred embodiment, at least one disintegrant may be selected from the group comprising: crosslinked sodium carboxymethylcellulose, modified cellulose gum, insoluble crosslinked polyvinyl pyrrolidone, starch, modified starch, glycolic acid starch salts such as sodium starch glycolate, microcrystalline cellulose, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-cellulose esters, hydroxyalkyl-cellulose esters, carboxyalkyl-cellulose esters, alginic acid, microcrystalline cellulose and its polymorphs, ion exchange resins, gums, chitin, chitosan, clay, gellan gum, crosslinked polacrilin copolymers, agar, gelatin, dextrin, acrylic acid polymers, sodium carboxymethylcellulose / calcium carboxymethylcellulose, hydroxypropyl methylcellulose phthalate, shellac, effervescent mixtures such as bicarbonate in combination with one or more acids such as citric acid or tartaric acid, or mixtures thereof. Preferably, at least one disintegrant is crosslinked sodium carboxymethylcellulose. At least one disintegrant may also be a super disintegrant. Super disintegrants that can be used in the methods of the present invention are generally those known in the art. Exemplary super disintegrants include, but are not limited to, cross-linked sodium carboxymethylcellulose, insoluble cross-linked polyvinyl pyrrolidone, sodium starch glycolate, and mixtures thereof.

[0141] If at least one disintegrant is added before and / or during and / or after step b), then at least one disintegrant is preferably added in an amount 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.

[0142] The at least one disintegrant may be added in dry form or in the form of an emulsion, dispersion or solution.

[0143] Thus, in one embodiment, a method for producing granules comprising surface-reacted calcium carbonate comprises the following steps:

[0144] 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 acid treatment and / or is supplied from an external source, preferably the carbon dioxide is formed in situ by acid treatment;

[0145] b) homogenizing the aqueous suspension comprising the surface-reacted calcium carbonate of step a),

[0146] 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, and

[0147] d) adding at least one disintegrant to the aqueous suspension before and / or during and / or after step b).

[0148] Alternatively, the method may comprise a step d) of mechanically and / or physically disintegrating the aqueous suspension comprising the surface-reacted calcium carbonate before and / or during and / or after step b).

[0149] Such mechanical and / or physical disintegration may be performed by any method known to the skilled person to be suitable for such purpose. For example, the mechanical and / or physical disintegration step d) may be performed by an ultrasound probe or the like.

[0150] Thus, in one embodiment, a method for producing granules comprising surface-reacted calcium carbonate comprises the following steps:

[0151] 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 acid treatment and / or is supplied from an external source, preferably the carbon dioxide is formed in situ by acid treatment;

[0152] b) homogenizing the aqueous suspension comprising the surface-reacted calcium carbonate of step a),

[0153] 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, and

[0154] d) mechanically and / or physically disintegrating the aqueous suspension comprising the surface-reacted calcium carbonate before and / or during and / or after step b).

[0155] It will be appreciated that further additives suitable for improving mouthfeel, palatability or controlled release, such as mannitol, carboxymethylcellulose or ground calcium carbonate (GCC), may be added before and / or during and / or after step b), preferably before or after step b), most preferably after step b).

[0156] Such additives, if added, are preferably added in an amount of 0.3 to 40 wt%, preferably 0.5 to 30 wt%, more preferably 1 to about 25 wt%, based on the total dry weight of the surface-reacted calcium carbonate.

[0157] According to step c) of the present invention, liquid is removed from the aqueous suspension comprising surface-reacted calcium carbonate of step b) by spray drying to obtain granules comprising surface-reacted calcium carbonate.

[0158] The spray drying equipment can be selected from the conventional equipment used for the purpose of spray drying. Therefore, the spray dryer can be selected from the group including rotary atomizer, fountain nozzle, two-fluid nozzle, pressure nozzle, combination nozzle, etc. Preferably, the spray drying step c) is carried out by using a rotary atomizer or a two-fluid nozzle. If the homogenization step b) is carried out by grinding, the spray dryer can be selected from the spray dryer used conventionally for spray drying, for example, the spray dryer can be selected from the group including a rotary atomizer, a fountain nozzle, two-fluid nozzle, pressure nozzle, combination nozzle, etc. About the fountain nozzle, it should be noted that it can also be referred to as a pressure nozzle running in a fountain (or co-current) mode. In one embodiment, the homogenization step b) is carried out by grinding and the spray drying step c) is carried out by using a rotary atomizer. It should be understood that different conditions will be set for different spray drying techniques to achieve the desired granular material. However, the technician knows how to adjust such conditions for different spray drying techniques.

[0159] For example, if a pressure nozzle is used, the spray drying in step c) is carried out as follows:

[0160] a) a feed pressure of 0.1 bar to 300 bar, preferably 5 bar to 100 bar, more preferably 6 bar to <50 bar, and most preferably 7 bar to 25 bar, and / or

[0161] b) a temperature of 150°C to 950°C, preferably 175°C to 700°C and most preferably 180°C to 550°C, measured as inlet temperature.

[0162] In one embodiment, if a pressure nozzle is used, the spray drying in step c) is carried out in the following:

[0163] a) a feed pressure of 0.1 bar to 300 bar, preferably 5 bar to 100 bar, more preferably 6 bar to <50 bar, and most preferably 7 bar to 25 bar, or

[0164] b) a temperature of 150°C to 950°C, preferably 175°C to 700°C and most preferably 180°C to 550°C, measured as inlet temperature.

[0165] Preferably, if a pressure nozzle is used, the spray drying in step c) is carried out in the following:

[0166] a) a feed pressure of 0.1 bar to 300 bar, preferably 5 bar to 100 bar, more preferably 6 bar to <50 bar, and most preferably 7 bar to 25 bar, and

[0167] b) a temperature of 150°C to 950°C, preferably 175°C to 700°C and most preferably 180°C to 550°C, measured as inlet temperature.

[0168] In one embodiment, if a two-fluid nozzle is used, the spray drying in step c) is carried out in the following:

[0169] a) a feed pressure of 0.1 bar to 300 bar, preferably 5 bar to 100 bar, more preferably 6 bar to <50 bar, and most preferably 7 bar to 25 bar, and / or

[0170] b) an orifice diameter of 0.8 mm to 1.8 mm, preferably 0.9 mm to 1.6 mm, and most preferably 1.05 mm to 1.5 mm, and / or

[0171] c) a temperature of 150°C to 950°C, preferably 175°C to 700°C, and most preferably 180°C to 550°C, measured as inlet temperature, and / or

[0172] d) A gas pressure to the nozzle of 1 to 7 bar, preferably 1.5 to 6.5 bar, and most preferably 2 to 6 bar.

[0173] For example, if a two-fluid nozzle is used, the spray drying in step c) is carried out as follows:

[0174] a) a feed pressure of 0.1 bar to 300 bar, preferably 5 bar to 100 bar, more preferably 6 bar to <50 bar, and most preferably 7 bar to 25 bar, or

[0175] b) an orifice diameter of 0.8 mm to 1.8 mm, preferably 0.9 mm to 1.6 mm, and most preferably 1.05 mm to 1.5 mm, or

[0176] c) a temperature of 150°C to 950°C, preferably 175°C to 700°C, and most preferably 180°C to 550°C, measured as inlet temperature, or

[0177] d) A gas pressure to the nozzle of 1 to 7 bar, preferably 1.5 to 6.5 bar, and most preferably 2 to 6 bar.

[0178] Alternatively, if a two-fluid nozzle is used, the spray drying in step c) is carried out in the following:

[0179] a) a feed pressure of 0.1 bar to 300 bar, preferably 5 bar to 100 bar, more preferably 6 bar to <50 bar, and most preferably 7 bar to 25 bar, and

[0180] b) an orifice diameter of 0.8 mm to 1.8 mm, preferably 0.9 mm to 1.6 mm, and most preferably 1.05 mm to 1.5 mm, and

[0181] c) a temperature of 150°C to 950°C, preferably 175°C to 700°C, and most preferably 180°C to 550°C, measured as inlet temperature, and

[0182] d) A gas pressure to the nozzle of 1 to 7 bar, preferably 1.5 to 6.5 bar, and most preferably 2 to 6 bar.

[0183] It will be appreciated that two-fluid nozzles are well known in the art and include, for example, combination nozzles from GEA-Niro of Denmark.

[0184] In one embodiment, if a rotary atomizer is used, the spray drying in step c) is carried out in the following:

[0185] a) a feed pressure of 0.5 to 8 bar, preferably 1 to 6.5 bar, and most preferably 2 to 4.5 bar, and / or

[0186] b) a rotating wheel speed of ≤ 11000 rpm, preferably 8000 to 11000 rpm, more preferably 9000 to 10000 rpm (at a wheel diameter of d = 150 mm and / or a speed of 73 m / sec), and / or

[0187] c) a temperature of 150°C to 950°C, preferably 175°C to 700°C, and most preferably 180°C to 550°C, measured as inlet temperature.

[0188] For example, if a rotary atomizer is used, the spray drying in step c) is carried out as follows:

[0189] a) a feed pressure of 0.5 to 8 bar, preferably 1 to 6.5 bar, and most preferably 2 to 4.5 bar, or

[0190] b) a rotating wheel speed of ≤ 11000 rpm, preferably 8000 to 11000 rpm, more preferably 9000 to 10000 rpm (at a wheel diameter of d = 150 mm and / or a speed of 73 m / sec), or

[0191] c) a temperature of 150°C to 950°C, preferably 175°C to 700°C, and most preferably 180°C to 550°C, measured as inlet temperature.

[0192] Alternatively, if a rotary atomizer is used, the spray drying in step c) is carried out in the following:

[0193] a) a pressure of 0.5 to 8 bar, preferably 1 to 6.55 bar, and most preferably 2 to 4.5 bar, and

[0194] b) a rotating wheel speed of ≤ 11000 rpm, preferably 8000 to 11000 rpm, more preferably 9000 to 10000 rpm (at a wheel diameter of d = 150 mm and / or a speed of 73 m / sec), and

[0195] c) a temperature of 150°C to 950°C, preferably 175°C to 700°C, and most preferably 180°C to 550°C, measured as inlet temperature.

[0196] In one embodiment, if a fountain nozzle is used, the spray drying in step c) is carried out in the following:

[0197] a) a feed pressure of 8 to 60 bar, preferably 10 to 25 bar, and most preferably 11 to 18 bar, and / or

[0198] b) a temperature of 150°C to 950°C, preferably 175°C to 700°C and most preferably 180°C to 550°C, measured as inlet temperature.

[0199] For example, if a fountain nozzle is used, the spray drying in step c) is carried out as follows:

[0200] a) a feed pressure of 8 to 60 bar, preferably 10 to 25 bar, and most preferably 11 to 18 bar, or

[0201] b) a temperature of 150°C to 950°C, preferably 175°C to 700°C and most preferably 180°C to 550°C, measured as inlet temperature.

[0202] Alternatively, if a fountain nozzle is used, the spray drying in step c) is carried out in the following:

[0203] a) a pressure of 8 to 60 bar, preferably 10 to 25 bar, and most preferably 11 to 18 bar, and

[0204] b) a temperature of 150°C to 950°C, preferably 175°C to 700°C and most preferably 180°C to 550°C, measured as inlet temperature.

[0205] The granulate obtained in step c) is preferably in dry form, ie in free-flowing form.

[0206] The term "dried" granulate is understood as a material having less than 4% by weight of water relative to the weight of the granulate. The % water may be determined by heating the granulate to 105°C in a drying chamber using a method according to ISO 787-2.

[0207] The granular material obtained by the inventive method has a favorable bulk density. Therefore, in another aspect, the present invention relates to a granular material comprising surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is a reaction product of natural heavy 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 supplied by an external source, and the bulk density of the granular material is 0.25 g / mL to 0.70 g / mL. Preferably, the granular material comprises surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is a reaction product of natural heavy 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 the bulk density of the granular material is 0.25 g / mL to 0.70 g / mL.

[0208] For example, the bulk density of the granules is from 0.28 g / mL to 0.65 g / mL, more preferably from 0.30 g / mL to 0.60 g / mL and most preferably from 0.35 g / mL to 0.60 g / mL.

[0209] It will be appreciated that the granulate preferably has a very specific particle size distribution which can be adjusted depending on the process used.

[0210] In particular, the granules have:

[0211] a) Volume particle size of 50 μm to 500 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure d 90 ,

[0212] b) volume median particle size of 5 μm to 300 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure d 50 ,as well as

[0213] c) Volume particle size d of 1 μm to 100 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 10 .

[0214] Preferably, the granules have:

[0215] a) Volume particle size of 60 μm to 400 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure d 90 ,

[0216] b) volume median particle size of 10 μm to 200 μm as measured by laser diffraction, dry at 0.1 bar dispersion pressure 50 ,as well as

[0217] c) Volume particle size d of 1 μm to 90 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 10 .

[0218] Most preferably, the granules have:

[0219] a) Volume particle size of 70 μm to 350 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 90 ,

[0220] b) volume median particle size of 12 μm to 175 μm as measured by laser diffraction, dry at 0.1 bar dispersion pressure d 50 ,as well as

[0221] c) Volume particle size d of 1 μm to 80 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 10 .

[0222] In one embodiment, in particular if step b) is carried out in a homogenizer, the granules have:

[0223] d) a volume particle size of 50 μm to 500 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 90 ,

[0224] e) a volume median particle size of 20 μm to 300 μm as measured by laser diffraction, dry at 0.1 bar dispersion pressure 50 ,as well as

[0225] f) volume particle size d of 2 μm to 100 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 10 .

[0226] Preferably, the granules have:

[0227] d) a volume particle size of 60 μm to 400 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 90 ,

[0228] e) a volume median particle size of 30 μm to 200 μm as measured by laser diffraction, dry at 0.1 bar dispersion pressure 50 ,as well as

[0229] f) volume particle size d of 3 μm to 90 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 10 .

[0230] Most preferably, the granules have:

[0231] d) a volume particle size of 70 μm to 350 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 90 ,

[0232] e) a volume median particle size of 50 μm to 175 μm as measured by laser diffraction, dry at 0.1 bar dispersion pressure 50 ,as well as

[0233] f) volume particle size d of 10 μm to 80 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 10 .

[0234] Additionally or alternatively, the pellets have a spherical shape. "Spherical shape" in the meaning of the present invention refers to pellets having nearly the same diameter on all axes in three-dimensional space.

[0235] Therefore, the granules preferably have

[0236] a) a volume particle size d of 50 to 500 μm, preferably 60 to 400 μm, and most preferably 70 to 350 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 90 ,

[0237] a) a volume median particle size d of 5 μm to 300 μm, preferably 10 μm to 200 μm, and most preferably 12 μm to 175 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 50 ,as well as

[0238] b) a volume particle size of 1 μm to 100 μm, preferably 1 μm to 90 μm, and most preferably 1 μm to 80 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 10 ,or

[0239] c) Spherical shape.

[0240] Alternatively, the granules have:

[0241] a) a volume particle size d of 50 to 500 μm, preferably 60 to 400 μm, and most preferably 70 to 350 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 90 ,

[0242] b) a volume median particle size d of 5 μm to 300 μm, preferably 10 μm to 200 μm, and most preferably 12 μm to 175 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 50 ,as well as

[0243] c) a volume particle size d of 1 μm to 100 μm, preferably 1 μm to 90 μm, and most preferably 1 μm to 80 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 10 ,as well as

[0244] d) Spherical shape.

[0245] For example, in particular if step b) is carried out in a homogenizer, the granules have:

[0246] b) a volume particle size d of 50 to 500 μm, preferably 60 to 400 μm, and most preferably 70 to 350 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 90 ,

[0247] d) a volume median particle size d of 20 μm to 300 μm, preferably 30 μm to 200 μm, and most preferably 50 μm to 175 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 50 ,as well as

[0248] e) a volume particle size d of 2 μm to 100 μm, preferably 3 μm to 90 μm, and most preferably 10 μm to 80 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 10 ,or

[0249] f) Spherical shape.

[0250] Alternatively, the granules have:

[0251] e) a volume particle size d of 50 to 500 μm, preferably 60 to 400 μm, and most preferably 70 to 350 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 90 ,

[0252] f) a volume median particle size d of 20 μm to 300 μm, preferably 30 μm to 200 μm, and most preferably 50 μm to 175 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 50 ,as well as

[0253] g) a volume particle size d of 2 μm to 100 μm, preferably 3 μm to 90 μm, and most preferably 10 μm to 80 μm as measured by laser diffraction dry at 0.1 bar dispersion pressure 10 ,as well as

[0254] h) Spherical shape.

[0255] It should also be noted that the granules exhibit an advantageous stability. In particular, the granules exhibit a higher stability than a granule obtained by the same process but lacking the step of homogenizing the aqueous suspension comprising the surface-reacted calcium carbonate. For example, the granules have a ratio d of (0.5 bar) to (0.1 bar) of ≥40, more preferably ≥50, even more preferably ≥60, and most preferably ≥70, such as in the range of 70 to 120 or 70 to 110. 50 Additionally or alternatively, the granules have a ratio d of (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 to 90 or 35 to 80. 50 Determined stability.

[0256] In one embodiment, the granules have a ratio d of (0.5 bar) to (0.1 bar) of ≥40, more preferably ≥50, even more preferably ≥60, and most preferably ≥70, such as in the range of 70 to 120 or 70 to 110. 50 The stability determined by the ratio d of (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 to 90 or 35 to 80. 50 Determined stability.

[0257] Furthermore, the specific surface area of ​​the granules as measured by the BET nitrogen method is preferably ≥ 15.0 m 2 For example, the specific surface area of ​​granules measured using nitrogen and the BET method according to ISO9277:2010 is 15.0 m 2 / g to 200.0m2 / g.

[0258] Additionally, the specific pore volume of the granules calculated by mercury intrusion porosimetry is 0.15 cm 3 / g to 2.75cm 3 / g, preferably 0.30cm 3 / g to 2.50cm 3 / g, and most preferably 0.40cm 3 / g to 2.00cm 3 / g range.

[0259] The granules comprise a BET specific surface area of ​​preferably 1 m 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m 2 / g to 70m 2 / g of particles of surface-reacted calcium carbonate.

[0260] It is further preferred that the granules comprise a volume median particle size d measured by using laser diffraction. 50 The surface-reacted calcium carbonate particles are 0.5 μm to 50 μm, preferably 0.7 μm to 25 μm, more preferably 0.8 μm to 20 μm, especially 1 μm to 10 μm.

[0261] According to an exemplary embodiment, the granulate comprises particles of surface-reacted calcium carbonate having:

[0262] a) a volume median particle size d50 of 0.5 μm to 50 μm, preferably 0.7 μm to 25 μm, more preferably 0.8 μm to 20 μm, especially 1 μm to 10 μm, measured by using laser diffraction, and / or

[0263] b) 1 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m 2 / g to 70m 2 / g BET specific surface area.

[0264] Preferably, the granulate comprises particles of surface-reacted calcium carbonate having:

[0265] a) a volume median particle size d50 of 0.5 μm to 50 μm, preferably 0.7 μm to 25 μm, more preferably 0.8 μm to 20 μm, especially 1 μm to 10 μm, measured by using laser diffraction, or

[0266] b) 1 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m 2 / g to 70m 2 / g BET specific surface area.

[0267] Alternatively, the granulate comprises particles of surface-reacted calcium carbonate having:

[0268] a) a volume median particle size d of 0.5 μm to 50 μm, preferably 0.7 μm to 25 μm, more preferably 0.8 μm to 20 μm, especially 1 μm to 10 μm, measured by using laser diffraction 50 ,as well as

[0269] b) 1 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m 2 / g to 70m 2 / g BET specific surface area.

[0270] Furthermore, it may be preferred that the granules have a volume particle size d 98 (or d 98 The particles of surface-reacted calcium carbonate have a (volume) diameter of 2 μm to 150 μm, preferably 4 μm to 100 μm, more preferably 6 μm to 80 μm, even more preferably 8 μm to 60 μm, and most preferably 10 μm to 30 μm.

[0271] It is further preferred that the granules contain an intrusion specific pore volume within the granules calculated by mercury intrusion porosimetry measurement of 0.15 cm 3 / g to 1.60cm 3 / g, preferably 0.30cm 3 / g to 1.50cm 3 / g, more preferably 0.30cm 3 / g to 1.40cm 3 / g, and most preferably 0.30cm 3 / g to 1.35cm 3 Particles of surface-reacted calcium carbonate in the range of 100 Å / g.

[0272] According to an exemplary embodiment, the granulate comprises particles of surface-reacted calcium carbonate having:

[0273] a) a volume median particle size d50 of 0.5 μm to 50 μm, preferably 0.7 μm to 25 μm, more preferably 0.8 μm to 20 μm, especially 1 μm to 10 μm, measured by using laser diffraction, and / or

[0274] b) 1 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m 2 / g to 70m 2 / g BET specific surface area, and / or

[0275] c) Calculated by mercury intrusion porosimetry at 0.15 cm 3 / g to 1.60cm 3 / g, preferably 0.30cm 3 / g to 1.50cm 3 / g, more preferably 0.30cm 3 / g to 1.40cm 3 / g, and most preferably 0.30cm 3 / g to 1.35cm 3 / g, and most preferably 0.30cm 3 / g to 0.90cm 3 / g range of the intrusion specific pore volume within the particles.

[0276] Preferably, the granulate comprises particles of surface-reacted calcium carbonate having:

[0277] a) a volume median particle size d of 0.5 μm to 50 μm, preferably 0.7 μm to 25 μm, more preferably 0.8 μm to 20 μm, especially 1 μm to 10 μm, measured by using laser diffraction50 ,or

[0278] b) 1 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m 2 / g to 70m 2 / g BET specific surface area, or

[0279] c) Calculated by mercury intrusion porosimetry at 0.15 cm 3 / g to 1.60cm 3 / g, preferably 0.30crn 3 / g to 1.50cm 3 / g, more preferably 0.30cm 3 / g to 1.40cm 3 / g, and most preferably 0.30cm 3 / g to 1.35cm 3 / g, and most preferably 0.30cm 3 / g to 0.90cm 3 / g range of the intrusion specific pore volume within the particles.

[0280] Alternatively, the granulate comprises particles of surface-reacted calcium carbonate having:

[0281] a) a volume median particle size d of 0.5 μm to 50 μm, preferably 0.7 μm to 25 μm, more preferably 0.8 μm to 20 μm, especially 1 μm to 10 μm, measured by using laser diffraction 50 ,as well as

[0282] b) 1 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 200m 2 / g, preferably 2m 2 / g to 150m 2 / g, more preferably 20m 2 / g to 140m 2 / g, most preferably 40m 2 / g to 70m 2 / g BET specific surface area, and

[0283] c) Calculated by mercury intrusion porosimetry at 0.15 cm 3 / g to 1.60cm3 / g, preferably 0.30cm 3 / g to 1.50cm 3 / g, more preferably 0.30cm 3 / g to 1.40cm 3 / g, and most preferably 0.30cm 3 / g to 1.35cm 3 / g range of the intrusion specific pore volume within the particles.

[0284] In one embodiment, the granules contain at least one disintegrant or any compound that can be used as a disintegrant. For example, at least one disintegrant is selected from the group comprising: crosslinked sodium carboxymethylcellulose, modified cellulose gum, insoluble crosslinked polyvinyl pyrrolidone, starch, modified starch, glycolic acid starch salts such as sodium starch glycolate, microcrystalline cellulose, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-cellulose esters, hydroxyalkyl-cellulose esters, carboxyalkyl-cellulose esters, alginic acid, microcrystalline cellulose and its polymorphs, ion exchange resins, gums, chitin, chitosan, clays, gellan gum, crosslinked polacrilin copolymers, agar, gelatin, dextrin, acrylic acid polymers, sodium carboxymethylcellulose / calcium carboxymethylcellulose, hydroxypropyl methylcellulose phthalate, shellac, effervescent mixtures such as bicarbonates in combination with one or more acids such as citric acid or tartaric acid, or mixtures thereof.

[0285] If present, the granules comprise at least one disintegrant (or any compound that can be used as a disintegrant) in an amount of 0.25% to 35% by weight, preferably 0.5% to 15% by weight, more preferably 0.5% to 10% by weight, even more preferably 0.7% to 10% by weight, and most preferably 0.8% to 10% by weight, based on the total dry weight of the granules. In one embodiment, the granules comprise at least one disintegrant (or any compound that can be used as a disintegrant) in an amount of 0.25% to 35% by weight, preferably 0.5% to 15% by weight, more preferably 0.5% to 10% by weight, even more preferably 1.0% to 10% by weight, and most preferably 1.5% to 10% by weight, based on the total dry weight of the granules. It is particularly preferred that the granulate comprises at least one disintegrant (or any compound that can be used as a disintegrant) in an amount of 0.8 to 8 wt.-%, preferably 0.8 to 6 wt.-%, more preferably 0.8 to 5 wt.-%, and most preferably 0.8 to 4 wt.-%, based on the total dry weight of the granulate.

[0286] It will be appreciated that the granulate is preferably obtained by a process as defined herein.

[0287] Therefore, the granulate is preferably obtained by a process comprising the following steps:

[0288] 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 acid treatment and / or is supplied from an external source, preferably the carbon dioxide is formed in situ by acid treatment;

[0289] b) homogenizing the aqueous suspension comprising the surface-reacted calcium carbonate of step a), and

[0290] 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.

[0291] If the granulate comprises at least one disintegrant (or any compound that can act as a disintegrant), the granulate is preferably obtained by a process comprising the following steps:

[0292] 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 acid treatment and / or is supplied from an external source, preferably the carbon dioxide is formed in situ by acid treatment;

[0293] b) homogenizing the aqueous suspension comprising the surface-reacted calcium carbonate of step a),

[0294] 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, and

[0295] d) adding at least one disintegrant (or any compound that can act as a disintegrant) to the aqueous suspension before and / or during and / or after step b).

[0296] Additionally or alternatively, the granules are treated with the at least one active ingredient and / or an inactive precursor thereof such that the at least one active ingredient and / or an inactive precursor thereof is substantially only present on the outer surface of the granules.

[0297] The term "active ingredient" in the meaning of the present invention refers to a substance which has a specific effect on an organism and causes a specific reaction in humans, animals, microorganisms and / or plants.

[0298] Preferably, at least one active ingredient and / or an inactive precursor thereof is provided in liquid form.

[0299] 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 an inactive precursor thereof, which flows easily under the pressure conditions and temperature used (i.e., the pressure and temperature at which the granules are mixed with the at least one active ingredient and / or an inactive precursor thereof).

[0300] Thus, it is understood that at least one active ingredient and / or its inactive precursor may be liquid in a temperature range of 5° C. to 200° C., preferably 10° C. to 120° C., and most preferably 10° C. to 100° C. For example, at least one active ingredient and / or its inactive precursor may be liquid in a temperature range of 5° C. to 200° C., preferably 10° C. to 120° C., and most preferably 10° C. to 100° C. under ambient pressure conditions (i.e., at atmospheric pressure). Alternatively, at least one active ingredient and / or its inactive precursor may be liquid in a temperature range of 5° C. to 200° C., preferably 10° C. to 120° C., and most preferably 10° C. to 100° C. under reduced pressure conditions (e.g., a pressure of 100 mbar to 700 mbar).

[0301] In one embodiment, at least one active ingredient and / or its inactive precursor is liquid under ambient temperature and pressure conditions, for example, at room temperature (e.g., about 5°C to 35°C, preferably 10°C to 30°C and most preferably 15°C to 25°C) and at atmospheric pressure.

[0302] Alternatively, at least one active ingredient and / or an inactive precursor thereof is molten at the use temperature (e.g., about 35°C to 200°C, preferably 45°C to 120°C and most preferably 55°C to 100°C) and under ambient pressure conditions (i.e., at atmospheric pressure) or under reduced pressure conditions (e.g., a pressure of 100 mbar to 700 mbar).

[0303] Alternatively, at least one active ingredient and / or an inactive precursor thereof is dissolved in the solvent. That is, at least one active ingredient and / or an inactive precursor thereof and the solvent form a system in which no discrete solid particles are observed in the solvent and thus form a "solution".

[0304] In one embodiment of the present invention, the solvent is selected from the group consisting of water, methanol, ethanol, n-butanol, isopropanol, n-propanol, acetone, dimethyl sulfoxide, dimethylformamide, tetrahydrofuran, vegetable oils and their derivatives, animal oils and their derivatives, molten fats and waxes, and mixtures thereof. Preferably, the solvent is water, ethanol and / or acetone. More preferably, the solvent is water.

[0305] For example, at least one active ingredient and / or its inactive precursor may be a chiral compound. Thus, at least one active ingredient and / or its inactive precursor encompasses (R)-enantiomers, (S)-enantiomers and mixtures thereof, such as racemic mixtures.

[0306] Additionally or alternatively, at least one active ingredient and / or its inactive precursor may be an isomeric compound. Thus, at least one active ingredient and / or its inactive precursor encompasses (Z)-isomers, (E)-isomers and mixtures thereof. For example, if the active ingredient is specified as cinnamaldehyde, cinnamaldehyde may be present as (Z)-cinnamaldehyde and / or (E)-cinnamaldehyde.

[0307] For example, at least one active ingredient and / or its inactive precursor is selected from the group consisting of: fragrances; flavors; herbal extracts and oils; fruit extracts and oils; nutrients; trace minerals; insect repellents; foods; cosmetics; flame retardants; enzymes; macromolecules; pesticides; fertilizers; preservatives; antioxidants; reactive chemicals; pharmaceutically active agents and / or nutritionally active agents and / or veterinary active agents of synthetic origin, semi-synthetic origin, natural origin thereof or pharmaceutically inactive precursors and / or nutritionally inactive precursors and / or veterinary inactive precursors, and mixtures thereof.

[0308] The fragrance is preferably an alcohol, aldehyde and / or ketone having a molecular weight of at least about 100 g / mol and is used alone or in combination with other fragrances to impart an odor, fragrance, flavor or aroma. For example, the fragrance may be selected from the group consisting of 2,4-dimethyl-3-cyclohexene-1-methanol (floralol), 2,4-dimethylcyclohexanemethanol (dihydrofloralol), 5,6-dimethyl-1-methylvinylbicyclo[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 (isogeraniol), 4- (1-methylethyl) cyclohexanemethanol (mayol), α-3,3-trimethyl-2-norbornanemethanol, 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-norbornaneethanol (patchomint), 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 (water-soluble alcohol), 2-(cyclododecyl)propan-1-ol (hydroxy-ambran), 2,2-dimethyl-3-(3-methyl)- 2-Methyl-3-phenylpropanol, 3-phenyl-2-propene-1-ol (cinnamyl alcohol), 2-methyl-3-phenyl-2-propene-1-ol (methylcinnamyl alcohol), α-pentyl-3-phenyl-2-propene-1-ol (α-pentyl-cinnamyl alcohol), ethyl 3-hydroxy-3-phenylpropionate, 2-(4-methylphenyl)-2-propanol, 3-(4-methylcyclohex-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, 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 (Iron), 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 (sandalore), (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-methylvinyl)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 (lavender alcohol), 2-ethyl-2-isoprene-3-hexenol, 1-hydroxy Methyl-4-isopropenyl-1-cyclohexene (dihydrocuminol), 1-methyl-4-isopropenylcyclohex-6-en-2-ol (carveol), 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 (rootanol), 4-isopropyl-cyclohexanol, 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-isopropyl Cyclohexan-3-ol, 1-methyl-4-isopropylcyclohexan-8-ol (dihydroterpineol), 1,2-dimethyl-3-(1-methylethyl)cyclohexan-1-ol, heptyl alcohol, 2,4-dimethylheptan-1-ol, 6-heptyl-5-hepten-2-ol (isolinalool), 2,4-dimethyl-2,6-heptadienol, 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] heptane-2-ol, 2,6-dimethylheptane-2-ol (dimetol), 2,6,6-trimethylbicyclo[1.3.3]heptane-2-ol, octanol, 2-octenol, 2-methyloctan-2-ol, 2-methyl-6-methylene-7-octen-2-ol (geranyl alcohol), 7-methyloctan-1-ol, 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 (sandalol), 3,7-dimethyl-1,6-octadien-3-ol (linalool), 3,7-dimethyloctan-1-ol (pelargol), 3,7-dimethyloctan-3-ol (tetrahydrolinalool), 2,4-octadien-1-ol, 3,7-dimethyl-6-octan-3-ol (dihydrolinalool), 2,6-dimethyl-7-octan-2-ol (dihydrogeranol), 2,6-dimethyl-5,7-octadien-2-ol, 4,7-dimethyl-4-vinyl-6-octan-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-octan-2-ol, 2,6-dimethyl-3,5-octadien-2-ol (allo-octenol), 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-dioxa-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 (isobutyl linalool), 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 (farnesol), 3,7,11-trimethyl-1,6,10,-dodecatrien-3-ol (nerolidol), 3,7,11,15-tetramethylhexadecan-2-en-1-ol (phytol), 3,7,11,15-tetramethylhexadecan-1-en-3-ol (isophytol), benzyl alcohol, p-methoxybenzyl alcohol (anisyl alcohol), p-cymene-7-ol (cuminol), 4-methylbenzyl alcohol, 3,4- Methyldioxybenzyl 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), amyl o-hydroxybenzoate, ethyl 2-hydroxy-benzoate, 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 (fennel alcohol), 3a,4,5,6,7,7a-hexahydro-2,4-dimethyl-4,7-methoxy-1H-inden-5-ol, 3a,4,5,6,7,7a -hexahydro-3,4-dimethyl-4,7-endomethano-1H-inden-5-ol, 2-methyl-2-vinyl-5-(1-hydroxy-1-methylethyl)tetrahydrofuran, β-caryophyllene alcohol, vanillin, ethyl vanillin, cinnamaldehyde, benzaldehyde, phenylacetaldehyde, heptaldehyde, octanal, decanal, undecylaldehyde, undecylenal, dodecanal, tridecanal, methylnonylaldehyde, didecical, anisaldehyde, citronellal, citronellylaldehyde, cyclamenaldehyde, α-hexylcinnamaldehyde, hydroxycitronellal, α-methylcinnamaldehyde, methylnonylacetaldehyde, propylphenylaldehyde, citral, perillaldehyde, tolualdehyde, toluylacetaldehyde, cuminaldehyde, Salicylaldehyde, alpha-amylcinnamaldehyde and piperonal, and mixtures thereof.

[0309] Various essential oils, herbal extracts and / or fruit extracts can also be used, preferably those with various medicinal or dietary supplement properties. Essential oils, herbal extracts and / or fruit extracts are generally extracts or aromatic plants, plant parts, fruits or fruit parts that can be used for medicine or can be used for seasoning. Suitable herbal extracts and / or fruit extracts can be used alone or with various mixtures. Commonly used essential oils, herbal extracts and / or fruit extracts include: Echinacea, goldenseal, calendula, rosemary, thyme, Kava Kava, aloe, bloodroot, grapefruit seed extract, black cohosh, ginseng, guarana, bilberry, ginkgo, St. John's wort, evening primrose oil, yohimbe bark, green tea, ephedra, maca (Maca), raspberry, lutein, ginger, oil containing eugenol and combinations thereof.

[0310] A variety of nutrients can be used, including almost any vitamin, mineral, and / or phytochemical. For example, the following can be used: vitamin A, vitamin B1, vitamin B6, vitamin B12, vitamin B2, vitamin B6, vitamin D, vitamin E (i.e., tocopherol), vitamin K, thiamine, riboflavin, biotin, folic acid, niacin, pantothenic acid, Q10, alpha lipoic acid, dihydrolipoic acid, curcumin, xanthophyll, beta-cryptoxanthin, lycopene, lutein, zeaxanthin, astaxanthin, beta-carotene, carotene, mixed carotenoids, polyphenols, flavonoids, sodium, potassium, calcium, magnesium, sulfur, chlorine, choline, and / or phytochemicals such as carotenoids, chlorophyll, phyllo Green acid, fiber, flavonoids, anthocyanidins, cyaniding, delphinidin, malvaceae pigment, pelargonium pigment, peony pigment, morning glory pigment, flavanols, catechins, epicatechin, epigallocatechin, epigallocatechin gallate, theaflavins, thearubigins, proanthocyanidins, flavonols, quercetin, kaempferol, myricetin, isorhamnetin, flavononeshesperetin, naringenin, eriodictyol, tangeretin, flavonoids, apigenin, luteolin, lignans, phytoestrogens, resveratrol, isoflavones, daidzein, genistein, glycitein, soy isoflavones and combinations thereof. Examples of nutrients that may be used as active ingredients are set forth in US Patent Application Publication Nos. 20030157213 Al, 20030206993, and 20030099741 Al, which are incorporated herein by reference in their entirety for all purposes.

[0311] In one embodiment, trace minerals such as manganese, zinc, copper, fluorine, molybdenum, iodine, cobalt, chromium, selenium, phosphorus, and combinations thereof may be used.

[0312] The enzymes may include, but are not limited to, coenzyme Q10, pepsin, phytase, trypsin, lipase, protease, cellulase, lactase, and combinations thereof.

[0313] The pesticide is preferably any known herbicide, insecticide, insect growth regulator, nematicide, termite, molluscicide, piscicide, avicide, rodenticide, predacide, bactericide, insect repellent, animal repellent, antimicrobial, fungicide, disinfectant (antimicrobial agent) and disinfectant known to the skilled person.

[0314] It should be noted that the preservative can be any such compound known to the skilled person. For example, the preservative can include, but is not limited to, phenoxyethanol; ethylhexylglycerin; parabens, such as methylparaben, ethylparaben, propylparaben, butylparaben, and mixtures thereof; benzalkonium chloride; chlorobutanol; benzyl alcohol; cetylpyridinium chloride; tartaric acid; lactic acid; malic acid; acetic acid; benzoic acid; sodium benzoate; sorbic acid; potassium sorbate; and mixtures thereof.

[0315] The antioxidant is preferably selected from the group comprising: butylated hydroxyanisole (BHA); butylated hydroxytoluene (BHT); gallic acid esters / salts; carotenoids; polyphenols, such as resveratrol, flavonoids and mixtures thereof; derivatives of polyphenols; tocopherol and its salts; beta-carotene; ubiquinone; tocotrienols; dihydroquercetin; antioxidants of natural origin; and mixtures thereof. If the antioxidant is of natural origin, the antioxidant may be, for example, a conifer extract, a maritime pine bark extract (e.g., from Horphag, Switzerland). ), and / or emblica fruit extract (e.g. from Sabinsa, Germany ).

[0316] The pharmaceutically active agent or pharmaceutically inactive precursor thereof is preferably selected from the group comprising pharmaceutically active agents or pharmaceutically inactive precursors of synthetic origin, semi-synthetic origin, natural origin and combinations thereof.

[0317] Therefore, pharmaceutically active agents refer to pharmaceutically active agents of synthetic origin, semi-synthetic origin, natural origin and combinations thereof. In addition, pharmaceutically inactive precursors of pharmaceutically active agents refer to pharmaceutically inactive precursors of synthetic origin, semi-synthetic origin, natural origin and combinations thereof and will be activated into the respective pharmaceutically active agents at a later stage.

[0318] Activation of such pharmaceutically inactive precursors is known to the skilled person and is commonly used, for example, for activation in the stomach and / or the gastrointestinal tract, such as acidic activation or trypsin or chymotrypsin cleavage.

[0319] It is within the purview of the skilled artisan that the activation methods mentioned are of illustrative character only and are not intended to be limiting.

[0320] It should be noted that the pharmaceutically active agent or a pharmaceutically inactive precursor thereof may be any such compound known to the skilled person.

[0321] Thus, pharmaceutically active agents include any compound that provides prophylactic and / or therapeutic properties when administered to humans and / or animals. Examples include, but are not limited to: pharmaceutically active agents, therapeutically active agents, veterinary active agents, nutritional agents, and growth regulators.

[0322] The pharmaceutically active agent or its pharmaceutically inactive precursor may be an anti-inflammatory agent. Such agents may include, but are not limited to, non-steroidal 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. Pat. No. 4,985,459 to Sunshine et al., which is incorporated herein by reference in its entirety with respect to the description of such NSAIDs. Examples of useful NSAIDs include acetylsalicylic acid, ibuprofen, naproxen, benzyl alcohol, phenoxyethanol, phenoxyethanol, styrene ... Profen, flurbiprofen, fenoprofen, fenbufen, ketoprofen, indoprofen, pirprofen, carprofen, oxaprozin, pranoprofen, microprofen, sulfur Also useful are cholesterol anti-inflammatory drugs such as hydrocortisone, and COX-2 inhibitors such as meloxicam, celecoxib, rofecoxib, valdecoxib, etoricoxib, or mixtures thereof. Any mixture of the above anti-inflammatory agents may be used.

[0323] Other materials that can be used as pharmaceutically active agents or pharmaceutically inactive precursors thereof include commonly known oral and throat products. These products include, but are not limited to, upper respiratory agents such as phenylephrine, diphenhydramine, dextromethorphan, bromhexine, and chlorpheniramine; gastrointestinal agents such as famotidine, loperamide, and simethicone; antifungal agents such as miconazole nitrate; antibiotics; and analgesics such as ketoprofen and fluribuprofen.

[0324] The pharmaceutically active agent or its pharmaceutically inactive precursor may also be selected from sodium metabisulfite, butylated hydroxytoluene, butylated hydroxyanisole.

[0325] The pharmaceutically active agent or pharmaceutically inactive precursor thereof may also be selected from ephedrine, magaldrate, pseudoephedrine, sildenafil, lidocaine, benzalkonium chloride, caffeine, phenylephrine, amfepramone, orlistat, sibutramine, acetaminophen, aspirin, glitazones, metformin, chlorpromazine, dimenhydrinat, domperidone, meclizine, metoclopramide, ondansetron, prednisolone, promethazine, acrivastine, cetirizine, cinnarizine, clemastine, cyclizine, desloratadine, dexchlorpheniramine, dimenhydrinate, ebastine, fexofenadine, ibuprofen, levolevoproricin, loratadine, meclizine, mizolastine, promethazine, miconazole, chlorhexidine diacetate, diacetate), fluoride, decapeptide KSL, aluminum fluoride, amino chelated calcium, ammonium fluoride, ammonium fluorosilicate, ammonium monofluorophosphate, calcium fluoride, calcium gluconate, calcium glycerophosphate, calcium lactate, calcium monofluorophosphate, calcium carbonate, urea, cetylpyridinium chloride, chlorhexidine, chlorhexidine digluconate, chlorhexidine chloride, chlorhexidine diacetate, CPP casein phosphopeptide, hexetidine (hexetedine), octadecene ammonium fluoride, potassium fluorosilicate, potassium chloride, potassium monofluorophosphate, sodium bicarbonate, sodium carbonate, sodium fluoride, sodium fluorosilicate, sodium monofluorophosphate, sodium tripolyphosphate, stannous fluoride, stearyl trihydroxyethylpropylenediamine dihydrofluoride, strontium chloride, tetrapotassium pyrophosphate, tetrasodium pyrophosphate, tripotassium orthophosphate, trisodium orthophosphate, alginic acid, aluminum hydroxide, sodium bicarbonate, cetylpyridinium chloride ... denafil, 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 glycosides, 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, cetylpyridinium chloride, chlorhexidine, fluoride, lidocaine, amphotericin, miconazole, nystatin, fish oil, ginkgo biloba biloba), ginseng, ginger, goldenrod, saw palmettopalmetto), 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, loperamide, simethicone, acetylsalicylic acid, sucralfate, clotrimazole, fluconazole, itraconazole, ketoconazole, terbinafine, allopurinol, probenecid, atorvastatin, fluvastatin, lovastatin, niacin, pravastatin, rosuvastatin, simvastatin, pilocarpine, naproxen, alendronate, etidronate, raloxifene, risedronate, benzodiazepine disulfiram, naltrexone, buprenorphine, codeine, dextropropoxyphene, fentanyl, hydromorphone, ketobemidone, ketoprofen, methadone, morphine, naproxen, nicomorphine, oxycodone, pethidine, tramadol, amoxicillin, ampicillin, azithromycin, ciprofloxacin, clarithromycin, doxycycline, erythromycin, fusidic acid, lymecycline, metronidazole, moxifloxacin, ofloxacin, oxytetracycline, phenoxymethyl penicillin phenoxymethylpenicillin, rifamycin, roxithromycin, sulfamethoxazole, tetracycline, trimethoprim, vancomycin, acarbose, glibenclamide, gliclazide, glimepiride, glipizide, insulin, repaglinide, tolbutamide, oseltamivir, acyclovir, famciclovir, penciclovir, valganciclovir, amlodipine, diltiazem, felodipine, nifedipine, verapamil, finasteride, minoxidil, cocaine, buprenorphine (buphrenorphin), clonidine, methadone, naltrexone, calcium antagonists, clonidine, ergotamine, beta-blockers, aceclofenac, celecoxib, dexiprofen, etodolac, indomethacin, ketoprofen, ketorolac, lornoxicam, meloxicam, nabumetone, O iroxicam, parecoxib, phenylbutazone, piroxicam, tiaprofenic acid, tolfenamic acid, aripiprazole, chlorpromazine, chlorprothixene, clozapine, flupentixol, fluphenazine, haloperidol, lithium carbonate, lithium citrate, melperone, penfluridol, percynanchum, perphenazine, pimozide, pipampirone, prochlorperazine, risperidone, thioridazine, fluconazole, itraconazole, ketoconazole, voriconazole, opium, benzodiazepine class, Hydroxine, meprobamate, phenothiazines, aluminum aminoacetate, esomeprazole, famotidine, magnesium oxide, nizatidine, omeprazole, pantoprazole, fluconazole, itraconazole, ketoconazole, metronidazole, amphetamine, atenolol, bisoprolol fumarate, metoprolol, metoprolol, pindolol, propranolol, auranofin, and bendrazine.

[0326] Other examples of useful pharmaceutically active agents or pharmaceutically inactive precursors thereof may comprise an active ingredient selected from the therapeutic group consisting of analgesics, anesthetics, antipyretics, antiallergics, antiarrhythmics, appetite suppressants, antifungals, anti-inflammatory agents, bronchodilators, cardiovascular drugs, coronary vasodilators, cerebral vasodilators, peripheral vasodilators, anti-infectives, psychotropics, antimanics, stimulants, antihistamines, laxatives, decongestants, gastrointestinal sedatives, sexual dysfunction agents, disinfectants, antidiarrheals, antianginal substances, vasodilators, antihypertensives, vasoconstrictors antidepressants, antipsychotics, antineoplastic agents, anticoagulants, antithrombotic agents, hypnotics, sedatives, antiemetics, antinauseants, anticonvulsants, neuromuscular agents, glycemic and hypoglycemic agents, thyroid and antithyroid drugs, diuretics, antispasmodics, uterine relaxants, diet pills, appetite suppressants, antispasmodics, protein anabolic agents, erythropoietic agents, antiasthmatic agents, expectorants, antitussives, mucolytics, anti-uricemic agents agents), dental agents, breath fresheners, antacids, antidiuretics, anti-flatulents, beta blockers, tooth whiteners, enzymes, coenzymes, proteins, energy enhancers, fibers, probiotics, prebiotics, NSAIDs, antitussives, decongestants, antihistamines, expectorants, antidiarrheals, hydrogen antagonists, proton pump inhibitors, systemic non-selective CNS depressants, systemic non-selective CNS stimulants, selective CNS function modulators, antiparkinsonian agents, narcotic analgesics, analgesics-antipyretics, psychopharmacological agents, and sexual dysfunction agents.

[0327] Examples of useful pharmaceutically active agents or pharmaceutically inactive precursors thereof may also include: casein glycomacropeptide glyco-macro-peptide, CGMP), triclosan, cetylpyridinium chloride, domiphene bromide, quaternary ammonium salts, zinc components, sanguinarine, fluoride, Alexidine, octonidine, EDTA, aspirin, acetaminophen, ibuprofen, ketoprofen, diflunisal, fenoprofen calcium, naproxen, tolmetin sodium, indomethacin, benzonatate, caramiphene edisylate, menthol, dextromethorphan hydrobromide, theobromine hydrochloride, chlorphendianol hydrochloride, pseudoephedrine hydrochloride, phenylephrine, phenylpropanolamine, pseudoephedrine sulfate, brompheniramine maleate, chlorpheniramine maleate, carbinoxamine maleate, clemastine fumarate, dextrochlorpheniramine maleate, diphenhydramine hydrochloride, diphenpyralide hydrochloride, azatadine maleate, diphenhydramine citrate, doxylamine succinate, promethazine hydrochloride, pyrilamine maleate, tripelenamine citrate, triprolidine hydrochloride, acrivastine, loratadine, brompheniramine, dexbrompheniamine, guaifenesin, ipecac, potassium iodide, terpene glycol hydrate, loperamide, famotidine, ranitidine, omeprazole, lansoprazole, fatty alcohols, barbiturates, caffeine, strychnine, picrotoxin, pentylenetetrazol, phenyhydantoin, phenobarbital, primidone, carbamazepine, ethosuximide, methsuximide, phensuximide, trimethadione, diazepam, benzodiazepine The anesthetics include phenacetamide, phenbutyrylamide, acetazolamide, sultimethoxazole, bromide, levodopa, amantadine, morphine, heroin, hydromorphone, methotrexate, oxymorphone, levormorphan, codeine, hydrocodone, oxycodone (Xycodone), nalorphine, naloxone, naltrexone, salicylates, phenylbutazone, indomethacin, phenacetin, chlorpromazine, levomepromazine, haloperidol, clozapine, reserpine, imipramine, tranylcypromine, phenelzine, lithium, sildenafil citrate, tadalafil and vardenafil CL. For example, eugenol can be used as an anesthetic.

[0328] Examples of useful pharmaceutically active agents or pharmaceutically inactive precursors thereof may include active ingredients selected from the group consisting of ace-inhibitors, antianginal agents, antiarrhythmic agents, antiasthmatics, anticholesterolemic agents, analgesics, anesthetics, anticonvulsants, antidepressants, antidiabetics, antidiarrheal preparations, antidotes, antihistamines, antihypertensives, anti-inflammatory agents, antilipid agents, antimanic agents, antinausea agents, antistroke agents, antithyroid preparations, antitumor agents, antiviral agents, acne drugs, alkaloids, amino acid preparations, sedatives. cough remedies, anti-uremic agents, antiviral drugs, anabolic agents, systemic and non-systemic anti-infective agents, anti-neoplastic agents, anti-Parkinson's syndrome agents, anti-rheumatic agents, appetite stimulants, biological response modifiers, blood regulators, bone metabolism regulators, cardiovascular drugs, central nervous system stimulants, cholinesterase inhibitors, contraceptives, decongestants, dietary supplements, dopamine receptor agonists, endometriosis control agents, enzymes, erectile dysfunction treatment agents such as sildenafil citrate (currently sold as Viagra TM sales), fertility agents, gastrointestinal agents, homeopathic agents, hormones, hypercalcemia and hypocalcemia control agents, immunomodulators, immunosuppressants, migraine preparations, motion sickness treatment agents, muscle relaxants, obesity control agents, osteoporosis preparations, oxytocin, anti-parasympathetic agents, parasympathomimetics, prostaglandins, psychotherapeutic agents, respiratory system agents, sedatives, smoking cessation aids (e.g., bromocriptine), sympathetic blockers, tremor preparations, urinary tract agents, vasodilators, laxatives, antacids, ion exchange resins, antipyretics and combinations thereof.

[0329] Examples of pharmaceutically active agents or pharmaceutically inactive precursors thereof that are contemplated may also include antacids, H2-antagonists and analgesics. For example, antacid dosage forms may be prepared using the single ingredient calcium carbonate or in combination with magnesium hydroxide and / or aluminum hydroxide. In addition, antacids may be combined with H2-antagonists.

[0330] Analgesics include opioids and opioid derivatives such as Oxycontin TM , ibuprofen, aspirin, acetaminophen, and combinations thereof, which may optionally include caffeine.

[0331] Other useful pharmaceutically active agents or pharmaceutically inactive precursors thereof may include: antidiarrheal agents (e.g. Immodium TM AD), antihistamines, antitussives, decongestants, vitamins and breath fresheners. Also contemplated for use herein are antianxiety agents such as Xanax TM ; Antipsychotics such as Clozaril TM and Haldol TM ; Nonsteroidal anti-inflammatory agents (NSAIDs) such as ibuprofen, naproxen sodium, Voltaren TM and Lodine TM Antihistamines, such as Claritin TM Hismanal TM 、Relafen TM and Tavist TM ; Antiemetics, such as Kytril TM and Cesamet TM ; Bronchodilators, such as Bentolin TM , Proventil TM Antidepressants, such as Prozac TM , Zoloft TM and Paxil TM ; Anti-migraine agents, such as Imigra TM ; ACE-inhibitors, such as Vasotec TM , Capoten TM and Zestril TM ; Anti-Alzheimer's agents, such as Nicergoline TM ; and CaH-antagonists, such as Procardia TM , Adalat TM and Calan TM .

[0332] Popular H2-antagonists contemplated for use in the present invention include cimetidine, ranitidine hydrochloride, famotidine, nizatidine, ebrotidine, mifentidine, roxatidine, pisatidine, and aceroxatidine.

[0333] Active antacid ingredients may include, but are not limited to, the following: aluminum hydroxide, dihydroxyaluminiumaminoacetate, aminoacetic acid, aluminum phosphate, sodium dihydroxyaluminium carbonate, bicarbonate, bismuth aluminate, bismuth carbonate, bismuth subcarbonate, bismuth subgallate, bismuth subnitrate, bismuth subsalicylate, calcium phosphate, citrate ion (acid or salt), aminoacetic acid, hydrated magnesium aluminate sulfate, magnesium plus aluminum, magnesium aluminosilicate, magnesium carbonate, magnesium glycinate, magnesium hydroxide, magnesium oxide, magnesium trisilicate, milk solids, aluminum mono-orbasic calcium phosphate, calcium orthophosphate, potassium bicarbonate, sodium tartrate, sodium bicarbonate, magnesium aluminosilicate, tartaric acid and salts.

[0334] In some 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, salicyl alcohol, and combinations thereof. In some embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor can be selected from palliatives, such as slippery elmbark, 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.

[0335] In some embodiments, the pharmaceutically active agent or pharmaceutically inactive precursor thereof can be selected from antitussive ingredients such as chlorpheniramine hydrochloride, codeine, codeine phosphate, codeine sulfate, dextromethorphan, dextromethorphan hydrobromide, diphenhydramine citrate and diphenhydramine hydrochloride, and combinations thereof.

[0336] 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 other embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor can be selected from cough suppressants. Such cough suppressants can be divided into two groups: those that change the structure or production of sputum, such as mucolytics and expectorants; and those that inhibit the cough reflex, such as codeine (narcotic cough suppressants), antihistamines, dextromethorphan, and isoproterenol (non-narcotic cough suppressants).

[0337] In some further embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor may be an antitussive selected from the group comprising 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, dimenhydrinate, diphenhydramine, doxylamine, hydroxyzine, meclizine, phenindamine, phenyltoloxamine, promethazine, mepyramine, tripeliramine, triprolidine, and combinations thereof. In some embodiments, the pharmaceutically active agent or its pharmaceutically inactive precursor may be selected from antihistamines without sedative effects, such as astemizole, cetirizine, ebastine, fexofenadine, loratadine, terfenadine, and combinations thereof.

[0338] For example, the one or more active ingredients are selected from fragrances, flavors, essential oils, insecticides, fungicides, pharmaceutically active agents or pharmaceutically inactive precursors thereof such as bactericides and / or anesthetics, and mixtures thereof.

[0339] If the granulate comprises at least one active ingredient and / or an inactive precursor thereof, the at least one active ingredient and / or an inactive precursor thereof is preferably present in the granulate in an amount of 0.5 to 80 wt. %, preferably 10.0 to 70 wt. %, and most preferably 20 to 60 wt. %, based on the total dry weight of the granulate.

[0340] It should also be noted that the granules of the invention have improved flowability, compactability and mechanical stability compared to granules produced by a process lacking the homogenization step b).

[0341] Furthermore, the granules are ready-to-use granules in other processes for producing dispersible dosage forms. Such dosage forms are tablets, microtablets, pills, capsules, jelly beans or chewing gums comprising these granules.

[0342] Furthermore, the granules and the above-mentioned dosage forms can be used in nutritional products, agricultural products, veterinary products, cosmetic products, household products, foods, packaged products or personal care products, or as excipients in pharmaceutical products.

[0343] It should be understood that the cosmetic product is preferably a dry cosmetic and / or dry skin care composition, more preferably a dry cosmetic composition. For example, the dry cosmetic composition is a makeup powder, which includes eye shadow, powder makeup, lip powder, face powder, body powder or blush. According to another embodiment, the cosmetic product is a dry skin care composition. For example, the dry skin care composition can be a skin care powder, which includes shaving powder, body powder, baby powder, foot powder and deodorant powder. According to another embodiment, the dry cosmetic and / or dry skin care composition is a dry cosmetic and skin care composition.

[0344] 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, an adhesive, a composition applied to a mouth strip (mouthstrip) or an oral adhesive patch, a (chewable) tooth tablet, a chewable lozenge or a chewing gum, preferably a toothpaste, a tooth powder, a tooth powder or a (chewable) tooth tablet.

[0345] Such minitablets or tablets are well known in the art and have a particle size customary for the product to be prepared.

[0346] For example, the weight median particle size of a mini-tablet or tablet as measured by mechanical sieving is d 50 It is 0.1 mm to 20.0 mm, preferably 0.2 mm to 15.0 mm, and more preferably 0.3 mm to 10.0 mm.

[0347] The following examples and tests will illustrate the present invention but are not intended to limit the present invention in any way. BRIEF DESCRIPTION OF THE DRAWINGS

[0348] Figure 1 Shown are SEM results of granules obtained for SRCC1 by using a homogenizer for homogenization and a fountain nozzle for spray drying.

[0349] Figure 2 Shown are SEM results of granules obtained for SRCC2 by using a homogenizer for homogenization and a fountain nozzle for spray drying.

[0350] Figure 3 Shown are SEM results of granules obtained for SRCC3 by using a homogenizer for homogenization and a fountain nozzle for spray drying.

[0351] Figure 4 Shown are SEM results of granules obtained for SRCC4 by using a homogenizer for homogenization and a fountain nozzle for spray drying. Figure 5Further shown are SEM results of a section through a granulate obtained for SRCC2 by spray drying in a fountain nozzle.

[0352] Figure 6 Shown are SEM results of granules obtained for SRCC5 by using a mill for homogenization and a rotary atomizer for spray drying.

[0353] Figure 7 Shown are SEM results of granules obtained for SRCC6 by using a mill for homogenization and a rotary atomizer for spray drying.

[0354] Figure 8 Results are shown for tablet hardness [N] as a function of primary compression force [kN] for tablets prepared from granules prepared according to the invention by spray drying in a rotary atomizer compared to two commercial filler samples.

[0355] Fig. 9 Results are shown for 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 to two commercial filler samples. Example

[0356] Measurement method

[0357] Hereinafter, the measurement methods performed in the examples are described.

[0358] Particle size distribution

[0359] The median particle size d was determined by volume in a wet cell using a Malvern Mastersizer 2000 or 3000 laser diffraction system (Malvern Instruments Plc., UK). 50 (volume) and volume-determined top cut particle size d 98 (volume) and volume particle size d 90 (volume) and d 10 (Volume) for evaluation. 50 (volume) or d 98 The (volume) value indicates a diameter value that makes the diameter of 50 volume % or 98 volume % of the particles less than this value, respectively. The raw data obtained by this measurement are analyzed using Mie theory, with a particle refractive index of 1.57 and an absorption index of 0.005. The method and instrument are known to the technician and are commonly used to determine the particle size distribution of fillers and pigments. The sample is measured under dry conditions without any prior treatment.

[0360] The median particle size d is determined by weight measurement using the sedimentation method. 50 (weight), sedimentation method is the analysis of sedimentation behavior in a weight field. TM The measurement was performed with a 5120. The method and the instrument are known to the skilled person and are commonly used to determine the particle size distribution of fillers and pigments. The measurement was performed in an aqueous solution of 0.1 wt. % Na4P2O7. The sample was dispersed and subjected to ultrasound using a high-speed stirrer.

[0361] Said methods and instruments are known to the skilled person and are commonly used for determining the particle size of fillers and pigments.

[0362] If not stated otherwise in the following Examples section, volumetric particle size was assessed in a wet cell using a Malvern Mastersizer 2000 laser diffraction system (Malvern Instruments Plc., UK).

[0363] Specific surface area (SSA)

[0364] The specific surface area is measured by the BET method according to ISO 9277: 2010 using nitrogen after conditioning the sample by heating for a period of 30 minutes at 110°C when a disintegrant is used or at 250°C when the sample contains no disintegrant. If the sample is in the form of an aqueous suspension, the sample is 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.

[0365] Intrusion specific pore volume in particles (in cm 3 / g)

[0366] The specific pore volume was 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 equilibrium time used for each pressure step was 20 seconds. The sample material was sealed in a 5 cm 3The 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).

[0367] The total pore volume seen in the cumulative intrusion data can be divided into two regions, where the intrusion data from 214 μm down to about 1 μm to 4 μm shows that the coarse packing of the sample between any agglomerate structures plays an important role. Smaller than these diameters is the fine inter-particle packing of the particles themselves. If they also have intra-particle pores, this region appears bimodal, and the specific intra-particle pore volume is defined by taking the specific pore volume in pores finer than the inflection point of the peak (i.e., finer than the bimodal inflection point) caused by mercury intrusion. The sum of these three regions gives the total overall pore volume of the powder, but is strongly dependent on the original sample compaction / settling of the powder at the coarse pore end of the distribution.

[0368] By taking the first derivative of the cumulative intrusion curve, the pore size distribution based on the equivalent Laplace diameter is revealed (inevitably including pore shielding). The differential curve clearly shows the coarse agglomerate pore structure region, the inter-particle pore region, and the intra-particle pore region (if present). Knowing the intra-particle pore diameter range, the remaining inter-particle pore volume and the inter-agglomerate pore volume can be subtracted from the total pore volume to provide the desired pore volume of the internal pores alone, in terms of pore volume per unit mass (specific pore volume). Of course, the same subtraction principle applies to separating any other pore size regions of interest.

[0369] Bulk density

[0370] 100 ± 0.5 g of the corresponding material was carefully loaded into a 250 mL measuring 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:

[0371] Loose bulk density [g / mL] = weighed sample [g] / total volume [mL]

[0372] And record the results accurate to 0.01g / mL.

[0373] Brookfield Viscosity

[0374] The Brookfield viscosity is measured by a Brookfield viscometer (RVT type) at 25°C ± 1°C using a suitable spindle at 100 rpm after 30 seconds and is expressed in mPa·s.

[0375] Weight solids of the material in the suspension (wt%)

[0376] The weight solids content is determined by dividing the weight of the solid material by the total weight of the aqueous suspension.The weight of the solid material is determined by weighing the solid material obtained by evaporating the aqueous phase of the slurry and drying the obtained material to constant weight.

[0377] Granule stability and granulate particle size distribution

[0378] A Malvern Mastersizer 3000 (Malvern Instruments Plc., UK) in combination with a Malvern AeroS dry dispersion unit and a dry cell was used to determine d 50 The particle size distribution of the granules in the fineness range of 5 μm to 300 μm. The method used is described in the Mastersizer 3000 Basic Guide, the Mastersizer 3000 Manual and the Manual for Aero Series Dry dispersion unit available through Malvern Instruments Ltd. Approximately 10 ml of sample is loaded into the Aero S through the corresponding sieve. The sample is measured dry. The results are expressed in V% (volume %). The feed rate is completed at 0.1 bar, 0.5 bar and 1.5 bar to show the granule stability.

[0379] A feed rate of 0.1 bar was used to determine the particle size distribution of the granules.

[0380] Scanning electron microscopy (SEM)

[0381] The sample was prepared by diluting 50 μl to 150 μl slurry sample with 5 ml water. The amount of slurry sample depends on the solid content, the average value of the particle size and the particle size distribution. The diluted sample was filtered using a 0.8 μm membrane filter. A finer filter was used when the filtrate was turbid. The double-sided conductive adhesive tape was mounted on the SEM stub. The SEM stub was then gently pressed into the still wet filter cake on the filter. The SEM stub was then sputtered with 8 nm Au. Studies under FESEM (Zeiss Sigma VP) were carried out at 5 kV (Au). Subsequently, the Sigma VP field emission scanning electron microscope (Carl Zeiss AG, Germany) and a secondary electron detector (SE2) were used in a high vacuum (<10 -2 The prepared samples were examined at 4000 Pa.

[0382] Mechanical screening

[0383] Mechanical sieving was carried out in a vibrating sieving shaker RETSCHAS 200 equipped with Easy Sieve software, a sieve according to ISO 3310 (including sieve pan) and a balance (0.1 g). 120 g was used for sieving. The sample to be measured was made homogeneous to ensure the reproducibility of the sieving to the greatest extent possible. The sample material to be measured was placed in the upper test sieve. Sieving was carried out using the following method: sieving time: 3 minutes / amplitude: 1.0 / interval: 10 seconds.

[0384] 2. Materials used

[0385] Surface reacted calcium carbonate (SRCC1)

[0386] SRCC was obtained by adjusting the weight-based median particle size d from Omya SAS, Orgon 50 350 liters of an aqueous suspension of ground calcium carbonate are prepared in a mixing vessel with a solids content of ground limestone calcium carbonate having a solids content of 1.3 μm (by weight) (as determined by sedimentation) such that a solids content of 10 wt.-%, based on the total weight of the aqueous suspension, is obtained.

[0387] While the slurry was mixed at a speed of 6.2 m / sec, 11.2 kg of phosphoric acid was added to the suspension in the form of an aqueous solution containing 30 wt % phosphoric acid over a period of 20 minutes at a temperature of 70° C. After the addition of the acid, the slurry was stirred for an additional 5 minutes before being removed from the vessel.

[0388] The obtained slurry (SRCC1) had a solid content of 25.7 wt% based on the total weight of the slurry and a Brookfield viscosity of 554 mPa·s.

[0389] The properties of the surface-reacted calcium carbonate are summarized in Table 1 below.

[0390] Table 1

[0391]

[0392] Other Materials

[0393] Croscarmellose Sodium - Ac-di-sol, from JRS

[0394] 3. Homogenization and drying of SRCC by spraying

[0395] A. Homogenization

[0396] SRCC2

[0397] The slurry of surface-reacted calcium carbonate (SRCC1) was then diluted down to a solid content of about 20.1 wt.-% based on the total weight of the slurry. Subsequently, 500 L of the slurry were pumped twice through a homogenizer GEA Ariete NS3055 of GEA Mechanical Equipment Italia S.pA at a pressure of 500 bar, a temperature of 50° C. to 70° C. and a feed rate of 400 L / hour at a closed screw position and a small nozzle.

[0398] The obtained slurry (SRCC2) had a solid content of 23.4 wt.-%, based on the total weight of the slurry.

[0399] After passing through the homogenizer twice, the surface-reacted calcium carbonate had the properties listed in Table 2 below.

[0400] Table 2:

[0401]

[0402] SRCC3

[0403] The slurry of surface-reacted calcium carbonate (SRCC1) was diluted down to a solid content of about 18.9 wt.-% based on the total weight of the slurry. Subsequently, 500 L of the slurry was pumped three times through a homogenizer GEA Ariete NS3055 of GEA Mechanical Equipment Italia S.pA at a pressure of 500 bar, a temperature of 50° C. to 70° C. and a feed rate of 400 L / hour with the screw position closed and a small nozzle.

[0404] The obtained slurry (SRCC3) had a solid content of 18.9 wt % based on the total weight of the slurry.

[0405] After passing through the homogenizer three times, the surface-reacted calcium carbonate had the properties listed in Table 3 below.

[0406] Table 3:

[0407]

[0408] SRCC4

[0409] The slurry of surface-reacted calcium carbonate (SRCC1) 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 down to a solid content of about 20.5 wt% based on the total weight of the slurry. Subsequently, 500 L of the slurry were pumped twice through a homogenizer GEA Ariete NS3055 of GEA Mechanical Equipment Italia SpA at a pressure of 500 bar, a temperature of 50° C. to 70° C. and a feed flow of 400 L / hour at a closed screw position and a small nozzle.

[0410] The obtained slurry (SRCC4) had a solid content of 20.5 wt.-%, based on the total weight of the slurry.

[0411] After passing through the homogenizer twice, the surface-reacted calcium carbonate had the properties listed in Table 4 below.

[0412] Table 4:

[0413]

[0414] SRCC5

[0415] The slurry of surface-reacted calcium carbonate (SRCC1) was diluted down to a solid content of about 20.1 wt.-% based on the total weight of the slurry. The slurry was then ground in a 25 L vertical stirred media mill of Siegmund Linder containing 33 kg of silibeads ZY-E 0.4 / 0.6 mm at a feed rate of 82 L / hour, a tip speed of 5.0 m / second and a specific energy of about 55 kWh / ton.

[0416] The obtained slurry (SRCC5) had a solid content of 20.2 wt.-%, based on the total weight of the slurry.

[0417] After grinding, the surface-reacted calcium carbonate had the properties listed in Table 5 below.

[0418] Table 5:

[0419]

[0420] SRCC6

[0421] The slurry of surface-reacted calcium carbonate (SRCC1) was diluted down to a solid content of about 22.6 wt% based on the total weight of the slurry. The slurry was then ground in a Siegmund Linder 25L vertical stirred media mill containing 33kg of sharp beads ZY-E 0.4 / 0.6mm at a feed rate of 82L / hour, a tip speed of 5.0m / second and a specific energy of about 55kWh / ton.

[0422] The obtained slurry (SRCC6) had a solid content of 22.9 wt.-%, based on the total weight of the slurry.

[0423] After grinding, the surface-reacted calcium carbonate had the properties listed in Table 6 below.

[0424] Table 6:

[0425]

[0426] SRCC7

[0427] SRCC7 was obtained by adjusting the weight-based median particle size d from Omya SAS, Orgon 50 350 liters of an aqueous suspension of ground calcium carbonate are prepared in a mixing vessel with a solids content of ground limestone calcium carbonate having a solids content of 1.3 μm (by weight) (as determined by sedimentation) such that a solids content of 10 wt.-%, based on the total weight of the aqueous suspension, is obtained.

[0428] While the slurry was mixed at a speed of 6.2 m / sec, 11.2 kg of phosphoric acid was added to the suspension in the form of an aqueous solution containing 30 wt % phosphoric acid over a period of 20 minutes at a temperature of 70° C. After the addition of the acid, the slurry was stirred for an additional 5 minutes before being removed from the vessel.

[0429] The obtained slurry (SRCC7) had a solid content of 25.2 wt.-%, based on the total weight of the slurry, and a Brookfield viscosity of 365 mPa.s.

[0430] The properties of the surface-reacted calcium carbonate are summarized in Table 7 below.

[0431] Table 7

[0432]

[0433] SRCC8

[0434] A slurry of surface-reacted calcium carbonate (SRCC7) was ground in a Siegmund Linder 200 L vertical stirred media mill containing 250 kg of sharp beads ZY-E 0.4 / 0.6 mm at a feed rate of 1775 L / hour, a tip speed of 10.0 m / second and a specific energy of about 65.8 kWh / ton.

[0435] The obtained slurry (SRCC8) had a solid content of 21.7 wt.-%, based on the total weight of the slurry.

[0436] After grinding, the surface-reacted calcium carbonate had the properties listed in Table 8 below.

[0437] Table 8:

[0438]

[0439] SRCC9

[0440] A slurry of surface-reacted calcium carbonate (SRCC7) was ground in a Siegmund Linder 200 L vertical stirred media mill containing 250 kg of sharp beads ZY-E 0.4 / 0.6 mm at a feed rate of 2010 L / hour, a tip speed of 10.0 m / second and a specific energy of about 58.1 kWh / ton.

[0441] The obtained slurry (SRCC8) had a solid content of 20.1 wt.-%, based on the total weight of the slurry.

[0442] After grinding, the surface-reacted calcium carbonate had the properties listed in Table 9 below.

[0443] Table 9:

[0444]

[0445] B. Drying

[0446] The obtained slurries, namely SRCC1, SRCC2, SRCC3, SRCC4, SRCC5, SRCC6, SRCC8 and SRCC9, were then dried by removing liquid from the slurry containing surface-reacted calcium carbonate by means of spray drying using a rotary atomizer, a two-fluid nozzle or a fountain nozzle from GEA-Niro, Denmark.

[0447] The settings used for spray drying are listed in Table 10 below.

[0448] Table 10:

[0449]

[0450] *: refers to the pressure of the feed entering the dryer

[0451] The results of the granules obtained are listed in Table 11 below.

[0452] Table 11:

[0453]

[0454] * : refers to the pressure of the feed entering the dryer

[0455] Table 12 below summarizes the ratios d of (0.5 bar) to (0.1 bar) and (1.5 bar) to (0.1 bar). 50 and d 10 Determined granule stability. From Table 12 it can be concluded that the granules prepared by a process comprising a step of homogenizing an aqueous suspension comprising 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 process but lacking a step of homogenizing an aqueous suspension comprising surface-reacted calcium carbonate (i.e. granule SRCC1). In addition, Figures 1 to 4 A comparison of the SEM results of granules obtained by homogenization in a homogenizer and by spray drying in a fountain nozzle (i.e., granules SRCC1, granules SRCC2, granules SRCC3, and granules SRCC4) is shown. It should be noted that the SEM results of granules obtained by spray drying in a rotary atomizer or a two-fluid nozzle are similar. Figure 5 Further shown is a section through a granulate obtained by spray drying in a fountain nozzle, ie granulate SRCC2. Figure 6 and Figure 7 A comparison of the SEM results of granules obtained by homogenization in a mill and by spray drying in a rotary atomizer (i.e., granules SRCC5 and granules SRCC6) is shown. It should be noted that the SEM results of the granules obtained by spray drying in a fountain nozzle or a two-fluid nozzle are similar. In addition, it should be noted that the granules prepared by a homogenization step performed on an industrial scale (i.e., granules SRCC8 and granules SRCC9) show the same granule stability as the granules prepared by a homogenization step performed on a laboratory scale (i.e., granules SRCC2, granules SRCC3, granules SRCC4, granules SRCC5 and SRCC6). It should be noted that the samples after grinding may be slightly inferior in terms of physical data (friability / bulk density), but their performance is the same.

[0456] Table 12:

[0457]

[0458]

[0459] * Evaluations were performed in a wet cell using a Malvern Mastersizer 3000 laser diffraction system (Malvern Instruments Plc., UK).

[0460] The granules prepared according to the invention were further analyzed with regard to their compactability. For the tests, tablets were prepared in which the obtained granules SRCC2, SRCC3, SRCC5 and SRCC6 were first mixed with cross-linked carboxymethylcellulose 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 obtained mixture was mixed again in a Turbula mixer (Willy A. Bachofen, Turbula T10B) for 5 minutes. Tablets of two comparative filler samples, one filler based on calcium orthophosphate and the other filler based on calcium hydrogen phosphate, were prepared in the same manner. In contrast, the granules of SRCC4 were mixed only with lubricant (magnesium stearate, Ligamed MF-2-V, Cas #557-04-0, Peter Greven) in a Turbula mixer (Willy A. Bachofen, Turbula T10B) for 5 minutes. The mixture was then used to prepare tablets in a Fette 1200i using EU1 "tool, 10 mm filling cam, 8 standard convex 10 mm punches and a tableting speed of 10000 tablets / hour. The filling depth was adjusted to obtain a compression force of 2 kN up to 20 kN, and the tablet weight was fixed at 160 mg. Tablets of two comparative filler samples, one filler based on calcium orthophosphate and the other filler based on calcium hydrogen phosphate, were prepared in the same way.

[0461] Table 13 below lists the amounts [in % by weight] of the individual ingredients in the prepared tablets.

[0462] Table 13:

[0463]

[0464]

[0465] Tablet hardness [N] of tablets as a function of primary compression force [kN] is shown in Figure 8 middle. Figure 8The results of tablets prepared from granules prepared according to the invention by spray drying in a rotary atomizer are shown in comparison with two commercial filler samples, namely one filler based on calcium orthophosphate and another filler based on calcium hydrogen phosphate. It can be concluded that the tablets prepared from granules prepared according to the invention show a better hardness versus primary compression force relationship and therefore better compactability than the commercial filler samples. It should be noted that the compactability results of 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.

[0466] The granules prepared according to the invention were further analyzed with regard to their disintegration properties.

[0467] Disintegration time was determined by using the DisiTest 50 automatic tablet disintegration tester from Pharmatron. For the test, a beaker was filled with 700 mL of tap water. The water was heated to 37.0°C and then 6 tablets from each sample as prepared and 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 monitored.

[0468] Fig. 9 The disintegration time [seconds] of tablets prepared from granules prepared according to the invention by spray drying in a rotary atomizer is shown as a function of tablet hardness [N] compared to two commercial filler samples, namely one filler based on calcium orthophosphate and another filler based on calcium hydrogen phosphate. It can be concluded that the tablets prepared from granules prepared according to the invention show a favorable relationship of disintegration time versus hardness. It should be noted that the results of the relationship of disintegration time versus hardness of 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.

Claims

1. A method for producing a granular material comprising surface-reacted calcium carbonate, the method 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 acid treatment and / or is supplied from an external source; b) homogenizing the aqueous suspension comprising surface-reacted calcium carbonate of step a), and c) removing liquid from said 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 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 or mixtures thereof.

3. The process according to claim 1 or 2, wherein the surface-reacted calcium carbonate in the aqueous suspension of step a) has: a) Volume median particle size of 0.5 μm to 50 μm measured by using laser diffraction 50 , and / or b) 1 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 200m 2 / g BET specific surface area.

4. The process according to claim 1 or 2, wherein the surface-reacted calcium carbonate in the aqueous suspension of step a) has: a) Volume median particle size of 0.7 μm to 25 μm measured by using laser diffraction 50 ,or b) 2 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 150m 2 / g BET specific surface area.

5. The process according to claim 1 or 2, wherein the surface-reacted calcium carbonate in the aqueous suspension of step a) has: a) Volume median particle size of 0.8 μm to 20 μm measured by using laser diffraction 50 ,or b) 20 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 140m 2 / g BET specific surface area.

6. The method according to claim 1 or 2, wherein the solid content of the aqueous suspension of step a) is in the range of 1 wt% to 40 wt%, based on the total weight of the aqueous suspension.

7. The method according to claim 1 or 2, wherein the solid content of the aqueous suspension of step a) is in the range of 5% to 35% by weight, based on the total weight of the aqueous suspension.

8. The method according to claim 1 or 2, wherein the solid content of the aqueous suspension of step a) is in the range of 7 wt% to 26 wt%, based on the total weight of the aqueous suspension.

9. The process according to claim 1 or 2, wherein at least one disintegrant is added before and / or during and / or after step b).

10. The method according to claim 1 or 2, wherein at least one disintegrant is added before and / or during and / or after step b), the at least one disintegrant being selected from the group consisting of cross-linked sodium carboxymethylcellulose, modified cellulose gum, insoluble cross-linked polyvinyl pyrrolidone, starch, modified starch, 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 carboxymethylcellulose / calcium carboxymethylcellulose, hydroxypropyl methylcellulose phthalate, shellac, effervescent mixtures, or mixtures thereof.

11. The method according to claim 1 or 2, wherein at least one disintegrant is added before and / or during and / or after step b), the at least one disintegrant being selected from the group comprising crosslinked sodium carboxymethylcellulose, starch, sodium starch glycolate, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-cellulose esters, hydroxyalkyl-cellulose esters, carboxyalkyl-cellulose esters, alginic acid, microcrystalline cellulose and its polymorphs, ion exchange resins, gums, chitin, chitosan, clay, gellan gum, crosslinked polacrilin copolymers, agar, gelatin, dextrin, acrylic acid polymers, sodium carboxymethylcellulose / calcium carboxymethylcellulose, hydroxypropyl methylcellulose phthalate, shellac, bicarbonate in combination with one or more acids, or mixtures thereof.

12. The method according to claim 1 or 2, wherein at least one disintegrant is added before and / or during and / or after step b), wherein the at least one disintegrant is selected from the group consisting of cross-linked sodium carboxymethylcellulose, modified cellulose gum, insoluble cross-linked polyvinyl pyrrolidone, starch, starch glycolate, 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 carboxymethylcellulose / calcium carboxymethylcellulose, hydroxypropyl methylcellulose phthalate, shellac, effervescent mixtures, or mixtures thereof.

13. The process according to claim 9, wherein the at least one disintegrant is added before and / or during and / or after step b) in an amount of 0.3 to 10 wt.-%, based on the total dry weight of the surface-reacted calcium carbonate.

14. The process according to claim 9, wherein the at least one disintegrant is added before and / or during and / or after step b) in an amount of 0.5 to 8 wt.-%, based on the total dry weight of the surface-reacted calcium carbonate.

15. The process according to claim 9, wherein the at least one disintegrant is added before and / or during and / or after step b) in an amount of 1 wt.-% to about 5 wt.-%, based on the total dry weight of the surface-reacted calcium carbonate.

16. The method according to claim 1 or 2, wherein the homogenization in step b) is performed once or several times.

17. The method according to claim 1 or 2, wherein the homogenization in step b) is performed 1 to 5 times.

18. The method according to claim 1 or 2, wherein the homogenization in step b) is performed 1 to 3 times.

19. The method according to claim 1 or 2, wherein the homogenization in step b) is performed by grinding.

20. The method according to claim 1 or 2, wherein the homogenization in step b) is carried out in the following: a) a pressure of 50 bar to 900 bar, and / or b) An initial temperature of 5°C to 95°C.

21. The method according to claim 1 or 2, wherein the homogenization in step b) is carried out in the following: a) a pressure of 100 bar to 750 bar, and / or b) an initial temperature of 10°C to 80°C.

22. The method according to claim 1 or 2, wherein the homogenization in step b) is carried out in the following: a) a pressure of 200 bar to 650 bar, and / or b) An initial temperature of 15°C to 60°C.

23. The method according to claim 1 or 2, wherein the spray drying in step c) is carried out under the following conditions: a) a pressure of 0.1 bar to 300 bar, and / or b) Temperatures of 150° C. to 950° C. measured as inlet temperature.

24. The method according to claim 1 or 2, wherein the spray drying in step c) is carried out under the following conditions: a) a pressure of 5 bar to 100 bar, and / or b) Temperatures between 175°C and 700°C measured as inlet temperature.

25. The method according to claim 1 or 2, wherein the spray drying in step c) is carried out under the following conditions: a) a pressure of 6 bar to < 50 bar, and / or b) Temperatures of 180° C. to 550° C. measured as inlet temperature.

26. A granular material 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 supplied from an external source, the bulk density of the granular material being from 0.25 g / mL to 0.70 g / mL, The granular material has: a) Volume particle size of 50 μm to 500 μm measured by laser diffraction dry at 0.1 bar dispersion pressure d 90 , b) Volume median particle size of 5 μm to 300 μm measured by laser diffraction, dry at 0.1 bar dispersion pressure d 50 ,as well as c) Volume particle size d between 1 μm and 100 μm measured by laser diffraction dry at 0.1 bar dispersion pressure 10 ,and d) Spherical shape.

27. The granular material of claim 26, having a bulk density of 0.28 g / mL to 0.65 g / mL.

28. The granular material of claim 26, having a bulk density of 0.30 g / mL to 0.60 g / mL.

29. The granular material of claim 26, wherein the granular material has: a) Volume particle size of 60 μm to 400 μm measured by laser diffraction dry at 0.1 bar dispersion pressure d 90 .

30. The granular material of claim 26, wherein the granular material has: b) Volume median particle size of 10 μm to 200 μm measured by laser diffraction, dry at 0.1 bar dispersion pressure d 50 .

31. The granular material of claim 26, wherein the granular material has: c) Volume particle size d of 1 μm to 90 μm measured by laser diffraction dry at 0.1 bar dispersion pressure 10 .

32. The granular material of claim 26, wherein the granular material has: a) Volume particle size of 70 μm to 350 μm measured by laser diffraction dry at 0.1 bar dispersion pressure d 90 .

33. The granular material of claim 26, wherein the granular material has: b) Volume median particle size of 12 μm to 175 μm measured by laser diffraction, dry at 0.1 bar dispersion pressure d 50 .

34. The granular material of claim 26, wherein the granular material has: c) Volume particle size d of 1 μm to 80 μm measured by laser diffraction dry at 0.1 bar dispersion pressure 10 .

35. The granular material of claim 26, wherein the granular material comprises particles of surface-reacted calcium carbonate having: a) 1 m3 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) Volume median particle size of 0.5 μm to 50 μm measured by using laser diffraction 50 , and / or c) Calculated by mercury intrusion porosimetry at 0.15 cm 3 / g to 1.60cm 3 / g range of the intrusion specific pore volume within the particles.

36. The granular material of claim 26, wherein the granular material comprises particles of surface-reacted calcium carbonate having: a) 2m3 measured using nitrogen and BET method according to ISO 9277:2010 2 / g to 150m 2 / g BET specific surface area, or b) Volume median particle size of 0.7 μm to 25 μm measured by using laser diffraction 50 ,or c) Calculated by mercury intrusion porosimetry at 0.30 cm 3 / g to 1.50cm 3 / g range of the intrusion specific pore volume within the particles.

37. The granular material of claim 26, wherein the granular material comprises particles of surface-reacted calcium carbonate having: a) 20 m3 measured using nitrogen and the BET method according to ISO 9277:2010 2 / g to 140m 2 / g BET specific surface area, or b) Volume median particle size of 0.8 μm to 20 μm measured by using laser diffraction 50 ,or c) Calculated by mercury intrusion porosimetry at 0.30 cm 3 / g to 1.40cm 3 / g range of the intrusion specific pore volume within the particles.

38. The granulation of claim 26, wherein the granulation comprises at least one disintegrant.

39. The granulation according to claim 26, wherein the granulation comprises at least one disintegrant selected from the group consisting of cross-linked sodium carboxymethylcellulose, modified cellulose gum, insoluble cross-linked polyvinyl pyrrolidone, starch, modified starch, 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, hydroxypropyl methylcellulose phthalate, shellac, effervescent mixtures, or mixtures thereof.

40. The granulate according to claim 26, wherein the granulate comprises at least one disintegrant selected from the group consisting of crosslinked sodium carboxymethylcellulose, starch, sodium starch glycolate, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-cellulose esters, hydroxyalkyl-cellulose esters, carboxyalkyl-cellulose esters, alginic acid, microcrystalline cellulose and its polymorphs, ion exchange resins, gums, chitin, chitosan, clay, gellan gum, crosslinked polacrilin copolymer, agar, gelatin, dextrin, acrylic acid polymers, sodium carboxymethylcellulose / calcium carboxymethylcellulose, hydroxypropyl methylcellulose phthalate, shellac, bicarbonate in combination with one or more acids, or mixtures thereof.

41. The granulation according to claim 26, wherein the granulation comprises at least one disintegrant selected from the group consisting of cross-linked sodium carboxymethylcellulose, modified cellulose gum, insoluble cross-linked polyvinyl pyrrolidone, starch, starch glycolate, 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, hydroxypropyl methylcellulose phthalate, shellac, effervescent mixtures, or mixtures thereof.

42. The granulation according to claim 38, wherein the granulation comprises the at least one disintegrant in an amount of 0.25 wt% to 35 wt% based on the total dry weight of the granulation.

43. The granulation according to claim 38, wherein the granulation comprises the at least one disintegrant in an amount of 0.5 wt% to 15 wt% based on the total dry weight of the granulation.

44. The granulation according to claim 38, wherein the granulation comprises the at least one disintegrant in an amount of 0.5 wt% to 10 wt% based on the total dry weight of the granulation.

45. The granulate according to claim 26, wherein the granulate is obtained by the method according to claim 1.

46. ​​Use of the granulate according to claim 26 in agricultural and household products, in the preparation of veterinary products and in the preparation of personal care products, or as an excipient in pharmaceutical products.

47. Use of the granulate according to claim 26 in nutritional and cosmetic products.

48. Use of the granulate according to claim 26 in food.

49. Use of the granulate according to claim 26 in packaging products.

50. Use of the granulate according to claim 26 in the preparation of a dry skin care composition and in the preparation of an oral care composition.

51. Use of the granular material according to claim 26 in dry cosmetics.

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