US-12624216-B2 - Method for the production of free-flowing granules

US12624216B2US 12624216 B2US12624216 B2US 12624216B2US-12624216-B2

Abstract

The present invention refers to a method for the production of granules comprising surface-reacted calcium carbonate, granules comprising a surface-reacted calcium carbonate having a bulk density ranging from 0.25 to 0.70 g/mL, preferably from 0.28 to 0.65 g/mL, more preferably from 0.30 to 0.60 g/mL, and most preferably from 0.35 to 0.60 g/mL and the use of the granules n a nutraceutical product, agricultural product, veterinary product, cosmetic product, preferably in a dry cosmetic and/or dry skin care composition, home product, food product, packaging product or personal care product, preferably in an oral care composition, or as excipient in a pharmaceutical product.

Inventors

Laura DE MIGUEL
Marc Maurer
Alain Cremaschi
Francine KARL
Iñigo SESMA PARDO
Gaëlle MOHLER
Javier CAMARGO
LALIT SHARMA
Wolfgang Höpfl

Assignees

OMYA INTERNATIONAL AG

Dates

Publication Date: 20260512
Application Date: 20210426
Priority Date: 20200428

Claims (7)

1 . Granules comprising a surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is a reaction product of natural ground or precipitated calcium carbonate with carbon dioxide and one or more acids, wherein the carbon dioxide is formed in situ by the acid treatment and/or is supplied from an external source, the granules having a bulk density ranging from 0.25 to 0.70 g/mL, and wherein the granules have a volume particle size d 90 of from 50 to 500 μm, a volume median particle size d 50 of from 5 to 300 μm, and a volume particle size d 10 of from 1 to 100 μm, as measured dry at 0.1 bar dispersion pressure by laser diffraction and a spherical shape.
2 . The granules according to claim 1 , wherein the granules comprise particles of surface-reacted calcium carbonate having a) a BET specific surface area of from 1 m 2 /g to 200 m 2 /g, measured using nitrogen and the BET method according to ISO 9277:2010, and/or b) a volume median grain diameter d 50 of from 0.5 to 50 μm, measured by using laser diffraction, and/or c) an intra-particle intruded specific pore volume within the range from 0.15 to 1.60 cm 3 /g, calculated from a mercury intrusion porosimetry measurement.
3 . The granules according to claim 1 , wherein the granules comprise at least one disintegrant.
4 . The granules according to claim 3 , wherein the granules comprise the at least one disintegrant in an amount ranging from 0.25 to 35 wt.-%, based on the total dry weight of the granules.
5 . The granules according to claim 1 , wherein the granules are obtained by a method comprising the steps of: a) providing an aqueous suspension comprising a surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is a reaction product of natural ground or precipitated calcium carbonate with carbon dioxide and one or more acids, wherein the carbon dioxide is formed in situ by the acid treatment and/or is supplied from an external source; b) homogenizing the aqueous suspension comprising a surface-reacted calcium carbonate of step a), and c) removing the liquid from the aqueous suspension comprising a surface-reacted calcium carbonate of step b) by means of spray drying for obtaining granules comprising surface-reacted calcium carbonate.
6 . A nutraceutical product, agricultural product, veterinary product, cosmetic product, home product, food product, packaging product, personal care product, or pharmaceutical product comprising the granules according to claim 1 .
7 . The granules according to claim 3 , wherein the at least one disintegrant is selected from the group comprising sodium croscarmellose, modified cellulose gums, insoluble cross-linked polyvinylpyrrolidones, starches, modified starches, starch glycolates, micro crystalline cellulose, pregelatinized starch, sodium carboxymethyl starch, low-substituted hydroxypropyl cellulose, homopolymers of N-vinyl-2-pyrrolidone, alkyl-, hydroxyalkyl-, carboxyalkyl-cellulose esters, alginic acid, microcrystalline cellulose and its polymorphic forms, ion exchange resins, gums, chitin, chitosan, clays, gellan gum, crosslinked polacrillin copolymers, agar, gelatine, dextrines, acrylic acid polymers, carboxymethylcellulose sodium/calcium, hydroxpropyl methyl cellulose phthalate, shellac, effervescent mixtures in combination with one or more acids, or mixtures thereof.

Description

CROSS REFERENCE TO RELATED APPLICATIONS This application is a U.S. National Phase filing under 35 U.S.C. § 371 of International Application PCT/EP2021/060793, filed on Apr. 26, 2021, and published as WO 2021/219529 A1 on Nov. 4, 2021. PCT/EP2021/060793 claims priority from European application number 20171934.1, filed on Apr. 28, 2020, European application number 20184509.6 filed on Jul. 7, 2020, and European application number 20204917.7 filed on Oct. 30, 2020. The entire contents of each of these prior applications are hereby incorporated herein by reference. The present invention refers to a method for the production of granules comprising surface-reacted calcium carbonate, granules comprising a surface-reacted calcium carbonate having a bulk density ranging from 0.25 to 0.70 g/mL, preferably from 0.28 to 0.65 g/mL, more preferably from 0.30 to 0.60 g/mL, and most preferably from 0.35 to 0.60 g/mL and the use of the granules in a nutraceutical product, agricultural product, veterinary product, cosmetic product, preferably in a dry cosmetic and/or dry skin care composition, home product, food product, packaging product or personal care product, preferably in an oral care composition, or as excipient in a pharmaceutical product. In many applications such as pharmaceutical, nutraceutical, agricultural, veterinary, cosmetic, home, food, packaging and personal care product granules are of considerable importance and more preferred than powders. Thus, agglomeration of powders leading to granules typically having a size range between 0.2 to 4.0 mm depending on their subsequent use is widely used to improve physical properties of powders like wettability, flowability, bulk density and product appearance. Furthermore, granulation is carried out, e.g. to prevent the segregation of the constituents of powder mixes, to prevent dusting or to improve flowability. Granulation, i.e. the process in which the primary powder particles are made to adhere to form larger, multiparticle entities is a process of collecting particles together by creating bonds between them e.g. by a binding agent. One of the most important types of granulation is wet granulation, wherein granules are formed by the addition of a granulation liquid onto a powder bed which is under the influence of an impeller. The agitation resulting in the system along with the wetting of the components within the formulation results in the agglomeration of the primary powder particles to produce wet granules. The granulation liquid contains a solvent which must be volatile so that it can be removed by drying, and be non-toxic. Water mixed into the powders can form bonds between powder particles that are strong enough to lock them together. However, once the water dries, the agglomerates may fall apart. Therefore, water may not be strong enough to create and hold a bond. In such instances, the granulation liquid includes a binder. Regarding surface-reacted calcium carbonate, also granules are generally known. For example, in EP2264108 A1 (WO2010146530 A1), it is mentioned that the surface-reacted calcium carbonate obtained from the process described therein may be in the form of a cake, granules or a powder, and also in several documents describing different uses of surface-reacted calcium carbonate, such as in water purification, as a controlled release carrier, in fast disintegrating dosage forms, or gastroretentive drug formulation and delivery systems (EP1975310 B1, EP1982759 B1, EP1974807 B1, EP1974806 B1, EP2589430 A1, WO2010037753 A1, EP2719373 A1, or EP2719376 A1), granules are generally mentioned. These granules, however, which are either obtained as a result of the basic process of producing surface-reacted calcium carbonate, or by (wet) granulation, suffer from several disadvantages, such as e.g. inferior bulk density, flow properties and compactability as well as low mechanical stability. Furthermore, wet granulation requires the use of a binder which is less advantageous. Thus, surface-reacted calcium carbonate can be granulated using various methods, but the conventional processes, in the absence of binder, do not provide the desired result, i.e. high bulk density, flow properties and compactability as well as high mechanical stability. Thus, it is the object of the present invention to provide a method for the production of granules comprising surface-reacted calcium carbonate having a high bulk density, flow properties and compactability as well as high mechanical stability. A further object of the present invention is to improve the aforementioned characteristics without the use of a binder. One or more of the foregoing and other objects are solved by the subject-matter as defined herein in the independent claim. Advantageous embodiments of the present invention are defined in the corresponding sub-claims. The present invention thus relates to a method for the production of granules comprising surface-reacted calcium carbonate, the method compris