# US 10,308,518 B2 · Method for the manufacturing of a suspension comprising a calcium carbonate-comprising material

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- Number: US 10,308,518 B2
- Document ID: US10308518B2
- Status: Granted
- Kind: B2
- Application number: 15/518,978
- Filed: 2015-10-30
- Published: 2017-08-24
- Granted: 2019-06-04
- Earliest claimed: 2014-11-07
- Assignees: Omya International AG
- Applicants: Omya International AG
- Inventors: Daniel Gantenbein; Espen Berg-Hansen; Rolf Endre Orten
- Web page: https://patentgrep.com/patent/US10308518B2

## CPC

- C01F 11/185: {After-treatment, e.g. grinding, purification, conversion of crystal morphology}
- A61K 8/19: containing inorganic ingredients
- A61Q 19/00: Preparations for care of the skin
- C04B 14/28: of calcium
- C08K 3/26: Carbonates; Bicarbonates
- C08K 9/04: Ingredients treated with organic substances {(treated with macromolecular compounds C08K9/08)}
- C09C 1/021: {Calcium carbonates}
- C09C 3/041: {Grinding}
- C09C 3/08: Treatment with low-molecular-weight {non-polymer} organic compounds {(C09C3/006, C09C3/048 take precedence)}
- C09D 7/45: Anti-settling agents
- C09D 7/62: modified by treatment with other compounds
- C09J 11/04: inorganic
- D21H 17/675: {Oxides, hydroxides or carbonates}
- D21H 19/385: {Oxides, hydroxides or carbonates}
- A61K 2800/10: General cosmetic use
- A61K 2800/612: By organic compounds
- C01P 2004/51: Particles with a specific particle size distribution
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2006/12: Surface area
- C01P 2006/22: Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
- C01P 2006/60: Optical properties, e.g. expressed in CIELAB-values
- C08K 2003/265: {Calcium, strontium or barium carbonate}
- C08K 2201/003: Additives being defined by their diameter
- C08K 2201/006: Additives being defined by their surface area
- C01F: COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides or polysulfides of magnesium, calcium, strontium, or barium C01B17/42; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia or cyanogen containing nitrogen and non-metals and optionally metals C01B21/082; amides or imides of silicon C01B21/087}; metal {imides or} amides C01B21/092, {C01B21/0923}; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20; {double sulfates of magnesium with sodium or potassium C01D5/12; with other alkali metals C01D15/00, C01D17/00})
- A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D)
- A61Q: SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C09C: TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES (treatment of materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone C04B14/00, C04B18/00, C04B20/00); PREPARATION OF CARBON BLACK {; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS}
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- C09J: ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES (preparation of glue or gelatine C09H)
- D21H: PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

The present invention relates to a process for the manufacturing of a calcium carbonate-comprising material, to a calcium carbonate-comprising material obtained by the process as well as the use of the calcium carbonate-comprising material for paper filler and paper coating applications, in plastics applications, in paints, in adhesives, in sealings, in concrete, in agriculture applications, in food applications, in cosmetic applications or in pharmaceutical applications.

## Claims

### Claim 1

A process for manufacturing a calcium carbonate-comprising material, the process comprising the steps of:
a) providing at least two aqueous suspensions comprising a calcium carbonate-comprising material, wherein
i) the first aqueous suspension has a solid content from 1.0 to 82.0 wt.-%, based on the total weight of the aqueous suspension, and a content of particles having a particle size <2 μm in the range from 1.0 to 30.0 wt.-%; and
ii) the second aqueous suspension has a solid content from 10.0 to 82.0 wt.-%, based on the total weight of the aqueous suspension, and a content of particles having a particle size <2 μm in the range from >30.0 to 100.0 wt.-%;
b) mixing the at least two aqueous suspensions provided in step a) to obtain an aqueous suspension mixture;
c) grinding the aqueous suspension mixture obtained in mixing step b).

### Claim 2 (depends on 1)

The process according to claim 1, wherein at least one dispersing agent is added to at least one of the at least two aqueous suspensions provided in step a) and/or to the aqueous suspension mixture obtained in mixing step b).

### Claim 3 (depends on 2)

The process according to claim 2, wherein the at least one dispersing agent is selected from the group consisting of sodium, potassium, calcium, magnesium, lithium, strontium, primary amine, secondary amine, tertiary amine, and/or ammonium salts, whereby the amine salts are linear or cyclic, of at least partly neutralized homopolymers or copolymers of (meth)acrylic acid, maleic acid, fumaric acid, itaconic acid and derivatives of these acids, esters or amides, methylmethacrylate, methylacrylate, acrylamide, sodium hydrogen phosphate, polyphosphates, alkalipolyphosphates, carboxymethylcellulose, steric dispersants, comb polymers, and any mixture thereof.

### Claim 4 (depends on 2)

The process according to claim 2, wherein the at least one dispersing agent is sodium polyacrylate having a molecular weight Mw of from 4,000 to 10,000 g/mol.

### Claim 5 (depends on 2)

The process according to claim 2, wherein the at least one dispersing agent is sodium polyacrylate having a molecular weight Mw of from 4,000 to 8,000 g/mol.

### Claim 6 (depends on 1)

The process according to claim 1, wherein the BET specific surface area of
i) the calcium carbonate-comprising material in the aqueous suspension mixture obtained in grinding step c) has a BET specific surface area of between 0.1 and 30.0 m2/g, as measured using nitrogen and the BET method according to ISO 9277, or
ii) the calcium carbonate-comprising material in the aqueous suspension mixture obtained in grinding step c) has a BET specific surface area between 0.1 and 2.0 m2/g lower than the BET specific surface area of a calcium carbonate-comprising material manufactured by a process using water instead of the second aqueous suspension.

### Claim 7 (depends on 1)

The process according to claim 1, wherein the BET specific surface area of
i) the calcium carbonate-comprising material in the aqueous suspension mixture obtained in grinding step c) has a BET specific surface area of between 1.0 and 20.0 m2/g, as measured using nitrogen and the BET method according to ISO 9277, or
ii) the calcium carbonate-comprising material in the aqueous suspension mixture obtained in grinding step c) has a BET specific surface area between 0.1 and 1.5 m2/g lower than the BET specific surface area of a calcium carbonate-comprising material manufactured by a process using water instead of the second aqueous suspension.

### Claim 8 (depends on 1)

The process according to claim 1, wherein the BET specific surface area of
i) the calcium carbonate-comprising material in the aqueous suspension mixture obtained in grinding step c) has a BET specific surface area of between 2.0 and 14.0 m2/g, as measured using nitrogen and the BET method according to ISO 9277, or
ii) the calcium carbonate-comprising material in the aqueous suspension mixture obtained in grinding step c) has a BET specific surface area between 0.2 and 1.0 m2/g lower than the BET specific surface area of a calcium carbonate-comprising material manufactured by a process using water instead of the second aqueous suspension.

### Claim 9 (depends on 1)

The process according to claim 1, wherein the BET specific surface area of
i) calcium carbonate-comprising material in the aqueous suspension mixture obtained in grinding step c) has a BET specific surface area of between 8.0 and 10.0 m2/g, as measured using nitrogen and the BET method according to ISO 9277, and
ii) the calcium carbonate-comprising material in the aqueous suspension mixture obtained in grinding step c) has a BET specific surface area between 0.2 and 1.0 m2/g lower than the BET specific surface area of a calcium carbonate-comprising material manufactured by a process using water instead of the second aqueous suspension.

### Claim 10 (depends on 1)

The process according to claim 1, wherein the aqueous suspension mixture obtained in grinding step c) has a Brookfield viscosity of between 50 and 5,000 mPa·s.

### Claim 11 (depends on 1)

The process according to claim 1, the aqueous suspension mixture obtained in grinding step c) has a Brookfield viscosity of between 75 and 1,500 mPa·s.

### Claim 12 (depends on 1)

The process according to claim 1, wherein the aqueous suspension mixture obtained in grinding step c) has a Brookfield viscosity of between 150 and 500 mPa·s.

### Claim 13 (depends on 1)

The process according to claim 1, wherein the calcium carbonate-comprising material in the aqueous suspension mixture obtained in grinding step c) has a
i) top cut particle size d98 of ≤50.0 μm, and/or
ii) weight median particle size d50 between 0.1 and 10.0 μm.

### Claim 14 (depends on 1)

The process according to claim 1, wherein the calcium carbonate-comprising material in the aqueous suspension mixture obtained in grinding step c) has a
i) top cut particle size d98 of ≤20.0 μm, and/or
ii) weight median particle size d50 between 0.5 and 5.0 μm.

### Claim 15 (depends on 1)

The process according to claim 1, wherein the calcium carbonate-comprising material in the aqueous suspension mixture obtained in grinding step c) has a
i) top cut particle size d98 of ≤10.0 μm, and/or
ii) weight median particle size d50 between 1.0 and 2.0 μm.

### Claim 16 (depends on 1)

The process according to claim 1, wherein the solid content
i) of the first aqueous suspension is from 30.0 to 78.0 wt.-%, based on the total weight of the aqueous suspension, and/or
ii) of the second aqueous suspension is from 30.0 to 40.0 wt.-%, based on the total weight of the aqueous suspension, and/or
iii) of the aqueous suspension mixture obtained in grinding step c) is from 20.0 to 80.0 wt.-%, based on the total weight of the aqueous suspension.

### Claim 17 (depends on 1)

The process according to claim 1, wherein the solid content
i) of the first aqueous suspension is from 50.0 to 76.0 wt.-%, based on the total weight of the aqueous suspension, and/or
ii) of the second aqueous suspension is from 34.0 to 43.0 wt.-%, based on the total weight of the aqueous suspension, and/or
iii) of the aqueous suspension mixture obtained in grinding step c) is from 50.0 to 62.0 wt.-%, based on the total weight of the aqueous suspension.

### Claim 18 (depends on 1)

The process according to claim 1, wherein at least one of the at least two aqueous suspensions provided in step a) is subjected to a concentration step, mechanical dewatering by means of settling, or forced settling by a centrifuge.

### Claim 19 (depends on 1)

The process according to claim 1, wherein the calcium carbonate-comprising material is selected from group consisting of natural calcium carbonate, precipitated calcium carbonate, dolomite, and any mixture thereof.

### Claim 20 (depends on 1)

The process according to claim 1, wherein the calcium carbonate-comprising material is natural calcium carbonate from marble, chalk and/or limestone.

### Claim 21 (depends on 1)

The process according to claim 1, wherein the at least two aqueous suspensions provided in step a) comprise the first and the second aqueous suspension in an amount of more than 10.0 wt.-%.

### Claim 22 (depends on 1)

The process according to claim 1, wherein the at least two aqueous suspensions provided in step a) comprise the first and the second aqueous suspension in an amount of more than 30.0 wt.-%.

### Claim 23 (depends on 1)

The process according to claim 1, wherein the at least two aqueous suspensions provided in step a) comprise the first and the second aqueous suspension in an amount of more than 60.0 wt.-%.

### Claim 24 (depends on 1)

The process according to claim 1, wherein the at least two aqueous suspensions provided in step a) comprise the first and the second aqueous suspension in an amount of more than 65.0 wt.-%.

### Claim 25 (depends on 1)

The process according to claim 1, wherein the at least two aqueous suspensions provided in step a) consist of the first and the second aqueous suspension.

### Claim 26 (depends on 1)

The process according to claim 1, further comprising the aqueous suspension mixture obtained in grinding step c) to remove at least a portion of water by mechanical means and/or thermal means.

### Claim 27 (depends on 1)

The process according to claim 1, further comprising the steps of
e) drying the aqueous suspension mixture obtained in grinding step c) or the aqueous suspension mixture obtained in concentrating step d) to remove at least a portion of water to obtain a partially dewatered calcium carbonate-comprising material or to obtain a dried calcium carbonate-comprising material; and optionally
f) treating the dried calcium carbonate-comprising material obtained after step e) with at least one dispersing agent and re-diluting it to obtain an aqueous suspension comprising a dispersed calcium carbonate-comprising material, and/or
g) treating the dried calcium carbonate-comprising material obtained after step e) with at least one saturated aliphatic linear or branched carboxylic acid and/or with at least one mono-substituted succinic anhydride and/or at least one mono-substituted succinic acid and/or salty reaction product(s) and/or with at least one phosphoric acid ester blend of one or more phosphoric acid mono-ester and/or reaction products thereof and one or more phosphoric acid di-ester and/or reaction products thereof to obtain a hydrophobized calcium carbonate-comprising material.