Method for reducing the hygroscopicity of a mineral material

Patent metadata

Field	Value
Publication number	US-2022119621-A1
Application number	US-202017422336-A
Country	US
Kind code	A1
Filing date	Feb 24, 2020
Priority date	Feb 26, 2019
Publication date	Apr 21, 2022
Grant date	—

Abstract

A method may reduce the hygroscopicity of a material including calcium carbonate using at least one copolymer for assisting in grinding which is neutralized in a particular way, as well as a method for packaging such a material. The copolymer may have a molecular mass measured by SEC in a range of from 4,000 to 20,000 g/mol, and a polydispersity index in a range of from 1.5 to 4.0, and may be prepared by polymerizing acrylic acid and/or methacrylic acid, optionally in salt form, and non-ionic monomer(s) including hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate, a C1-C5 acrylate ester, a C1-C5 methacrylate ester, or combinations thereof, wherein the carboxylic acid groups may be at least partially neutralized by 70 mol. % of Na+ and from 10 to 30 mol % of Na+, K+, and/or Li+.

First claim

1 . A method for reducing the hygroscopicity of a material comprising calcium carbonate and suitable for use in a polymeric material, the method comprising
treating the material with a grinding aid comprising a copolymer having a molecular mass MW, measured by SEC, in a range of from 4,000 to 20,000 g/mol, a polydispersity index (PI) range of from of from 1.5 to 4.0, and prepared by polymerizing: acrylic acid and/or methacrylic acid, optionally in salt form; and a non-ionic monomer comprising hydroxyethyl acrylate, hydroxypropylacrylate, hydroxyethylmethacrylate, hydroxypropylmethacrylate, C 1 -C 5 acrylate ester, C 1 -C 5 methacrylate ester, or a mixture of two or more of these, and wherein, in the copolymer(s), carboxylic acid groups are at least partially or totally neutralized by 70 mol. % of Na + , and 10 to 30 mol. % of Na + , K + , and/or Li + .

2 . The method according of claim 1 , comprising:
(A) preparing an aqueous suspension of the material, the aqueous suspension comprising water (A1), the material (A2), and the copolymer (A3); (B) wet grinding the material in the aqueous suspension, to obtain a ground suspension; and (C) partially separating the water (A1) from the ground suspension comprising the material as a ground material.

3 . The method of claim 2 , further comprising:
(D) drying the ground suspension of the ground material, to obtain a ground, dried material; and, optionally (E) treating the ground, dried material with at least one hydrophobizing agent.

4 . The method of claim 2 , wherein the ground material has a median particle diameter, d 50 , by weight, determined by settling, in a range of from 0.1 to 3 μm.

5 . The method of claim 2 4 , wherein the aqueous suspension in the preparing (A) comprises the material in a range of from 40 to 70 wt. %.

6 . The method of claim 2 , wherein the aqueous suspension obtained after separating (C) comprises at least 72 wt. %, of the ground material, relative to a total suspension weight.

7 . The method of claim 1 , wherein the carboxylic acid groups of the copolymer are neutralized to at least 80 mol. % by Na + .

8 . The method of claim 2 , wherein the grinding (B) is carried out in the presence of from 0.05 to 0.5 wt. % of the copolymer, relative to a weight of the material.

9 . The method of claim 2 , wherein the partially separating (C) is carried out mechanically and/or thermally, optionally under vacuum or optionally combined with suction.

10 . The method of claim 3 , further comprising:
drying the ground material by spray-drying, lyophilization, spraying, rotary kilning, a heating strip, air-pulsed heating, a fluidized bed, fluidized lyophilization and/or nozzle-drying.

11 . The method of claim 3 , wherein the hydrophobizing agent is:
a carboxylic acid; a succinic acid anhydride derivative mono-substituted by a straight, branched, or cyclic C 2 -C 30 -alkyl group, or a reaction product of the derivative; a mixture of phosphoric acid monoesters, phosphoric acid diesters, or reaction products thereof; a polyhydrogenosiloxane, an inert silicone compound, or mixture thereof; a C 6 -C 14 -aliphatic aldehyde; or a mixture of two or more of any of these.

12 . The method of claim 3 , wherein the ground, dried material comprises less than 0.5 wt. % of moisture relative to total material weight.

13 . The method of claim 1 , wherein the material as ground, dried, and optionally treated with at least one hydrophobizing agent, has a hygroscopicity less than or equal to 0.26 mg/m 2 ,
wherein the hygroscopicity is measured according to the method by exposing a sample mass to an atmosphere of 10% relative humidity for 2.5 hours at a temperature of 23±2° C., then increasing the relative humidity to 85% and exposing the sample thereto for 2.5 hours at a temperature of 23±2° C., measuring the sample mass again, then calculating a change in the sample mass in mg/g to determine the hygroscopicity of the material.

14 . The method of claim 1 , wherein, in the copolymer(s), the carboxylic acid groups are completely neutralized.

15 . The method of claim 2 , wherein the material is marble, limestone, chalk, dolomite, or a mixture thereof.

16 . The method of claim 2 , wherein the material is of synthetic origin.

17 . The method of claim 2 , wherein the material is vaterite, calcite, aragonite, or a mixture thereof.

18 . The method of claim 2 , wherein the ground material has a BET specific surface area, in accordance with standard ISO 9277 (2010), in a range of from 1 to 50 m 2 /g.

19 . The method of claim 2 , wherein the ground material has a median particle diameter, d 50 , by weight, determined by settling, in a range of from 0.1 to 2.8 μm.

Assignees

• Coatex Sas

Inventors

• Jacquemet Christian
• Mongoin Jacques
• Suau Jean-Marc

Classifications

• C08K9/04

  Ingredients treated with organic substances {(treated with macromolecular compounds C08K9/08)} · CPC title

• C08K3/26 Primary

  Carbonates; Bicarbonates · CPC title

• C01P2006/82

  water content · CPC title

• C09C3/10

  Treatment with macromolecular organic compounds {(C09C3/006 takes precedence)} · CPC title

• C09C1/02 Primary

  Compounds of alkaline earth metals or magnesium {(C09C1/0003, C09C1/0009, C09C1/0015, C09C1/0078 take precedence; dolomitic solids C09C1/009)} · CPC title