# US 10,119,032 B2 · Process for the preparation of a mineral filler product

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- Number: US 10,119,032 B2
- Document ID: US10119032B2
- Status: Granted
- Kind: B2
- Application number: 15/116,373
- Filed: 2015-02-13
- Published: 2016-12-01
- Granted: 2018-11-06
- Earliest claimed: 2014-02-21
- Assignees: Omya International AG
- Applicants: Omya International AG
- Inventors: Samuel Rentsch; Fabio Ippolito; Matthias Buri; Patrick A. C. Gane
- Web page: https://patentgrep.com/patent/US10119032B2

## CPC

- C09C 1/021: {Calcium carbonates}
- C08K 9/04: Ingredients treated with organic substances {(treated with macromolecular compounds C08K9/08)}
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2006/12: Surface area
- C08K 2201/005: Additives being defined by their particle size in general
- C08K 2201/006: Additives being defined by their surface area
- 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}
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

A process for the preparation of a mineral filler product is disclosed, the process comprising a step of wet grinding a calcium carbonate-containing material in a mixture obtained by contacting the calcium carbonate-containing material with at least one grinding agent selected from specific styrene-maleic anhydride co-polymers and/or specific derivatives of styrene-maleic anhydride co-polymers.

## Claims

### Claim 1

A process for the preparation of a mineral filler product, the process comprising the steps of:
a) providing a calcium carbonate-containing material;
b) providing water;
c) providing at least one grinding agent;
d) wet grinding the calcium carbonate-containing material in a mixture obtained by contacting:
i) the calcium carbonate-containing material provided in step a), with
ii) the water provided in step b), and with
iii) the at least one grinding agent provided in step c) in any order in at least one grinding unit to obtain a wet ground mineral filler;
e) optionally classifying the wet ground mineral filler of step d) to obtain a coarse fraction and a fine fraction, wherein the coarse fraction is removed or subjected to wet grinding step d) and the fine fraction represents a fine mineral filler;
f) drying the wet ground mineral filler of step d) and/or the fine mineral filler of step e) to obtain a dried mineral filler having a total moisture content of less than or equal to 1.0 wt.-%, based on the total weight of said dried mineral filler; and
g) treating the dried mineral filler of step f) with a hydrophobizing agent to obtain a surface-treated product having a treatment layer on at least part of the surface of said product;
wherein the total moisture content in the mixture of step d) ranges from 15.0 to 50.0 wt.-%, based on the total weight of said mixture;
the amount of the at least one grinding agent provided in step c) ranges from 0.01 to 10.0 wt.-%, based on the total dry weight of the calcium carbonate-containing material;
the temperature in step d) ranges from 60° C. to 150° C.; and
the at least one grinding agent is selected from the group consisting of styrene-maleic anhydride co-polymers and derivatives of styrene-maleic anhydride co-polymers, said derivatives being selected from styrene-maleic anhydride co-polymers having partially or fully hydrolyzed maleic anhydride units, wherein said grinding agent has a monomer unit ratio (styrene units:maleic anhydride units, S:MA) of from 1:2 to 5:1 and a molecular weight MW of from 500 to 40,000 g/mol.

### Claim 2 (depends on 1)

The process according to claim 1, wherein the calcium carbonate-containing material provided in step a) is natural calcium carbonate.

### Claim 3 (depends on 1)

The process according to claim 1, wherein the calcium carbonate-containing material provided in step a) is selected from the group consisting of marble, limestone, chalk, dolomite, and any mixture thereof.

### Claim 4 (depends on 1)

The process according to claim 1, wherein the at least one grinding agent provided in step c) has a monomer unit ratio (S:MA) of from 1:1 to 4:1.

### Claim 5 (depends on 1)

The process according to claim 1, wherein the at least one grinding agent provided in step c) has a monomer unit ratio (S:MA) of from 1:1 to 3:1.

### Claim 6 (depends on 1)

The process according to claim 1, wherein the at least one grinding agent provided in step c) has a monomer unit ratio (S:MA) of from 1:1 to 2:1.

### Claim 7 (depends on 1)

The process according to claim 1, wherein the at least one grinding agent provided in step c) has a molecular weight MW of from 2,000 to 30,000 g/mol.

### Claim 8 (depends on 1)

The process according to claim 1, wherein the at least one grinding agent provided in step c) has a molecular weight MW of from 4,000 to 8,000 g/mol.

### Claim 9 (depends on 1)

The process according to claim 1, wherein the at least one grinding agent provided in step c) is partially or fully neutralized with cations selected from the group consisting of lithium, sodium, potassium, calcium, magnesium, ammonium, iminium, and any mixture thereof.

### Claim 10 (depends on 1)

The process according to claim 1, wherein the total moisture content in the mixture of step d) ranges from 18.0 to 35.0 wt.-%, based on the total weight of said mixture.

### Claim 11 (depends on 1)

The process according to claim 1, wherein the total moisture content in the mixture of step d) ranges from 20.0 to 28.0 wt.-%, based on the total weight of said mixture.

### Claim 12 (depends on 1)

The process according to claim 1, wherein the total moisture content in the mixture of step d) ranges from 22.0 to 25.0 wt.-%, based on the total weight of said mixture.

### Claim 13 (depends on 1)

The process according to claim 1, wherein the temperature in step d) ranges from 65° C. to 125° C.

### Claim 14 (depends on 1)

The process according to claim 1, wherein the temperature in step d) ranges from 70° C. to 115° C.

### Claim 15 (depends on 1)

The process according to claim 1, wherein the temperature in step d) ranges from 75° C. to 105° C.

### Claim 16 (depends on 1)

The process according to claim 1, wherein the wet ground mineral filler of step d) has a weight median particle d50 ranging from 0.1 to 8.0 μm.

### Claim 17 (depends on 1)

The process according to claim 1, wherein the wet ground mineral filler of step d) has a weight median particle d50 ranging from 0.2 to 5.0 μm.

### Claim 18 (depends on 1)

The process according to claim 1, wherein the wet ground mineral filler of step d) has a weight median particle d50 ranging from 0.4 to 3.0 μm.

### Claim 19 (depends on 1)

The process according to claim 1, wherein the dried mineral filler of step f) has a total moisture content of less than or equal to 0.5 wt.-%, based on the total weight of said dried mineral filler.

### Claim 20 (depends on 1)

The process according to claim 1, wherein the dried mineral filler of step f) has a total moisture content of less than or equal to 0.2 wt.-%, based on the total weight of said dried mineral filler.

### Claim 21 (depends on 1)

The process according to claim 1, wherein the dried mineral filler of step f) has a total moisture content of between 0.03 and 0.07 wt.-%, based on the total weight of said dried mineral filler.

### Claim 22 (depends on 1)

The process according to claim 1, wherein the hydrophobizing agent of step g) is selected from the group consisting of fatty acids having from 6 to 24 chain carbon atoms, mono-substituted succinic anhydrides, alkyl phosphoric acid esters, polyhydrogensiloxane, polydimethylsiloxane, and any mixture thereof.
