# US 10,865,144 B2 · Method for producing a dispersant

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- Number: US 10,865,144 B2
- Document ID: US10865144B2
- Status: Granted
- Kind: B2
- Application number: 15/554,984
- Filed: 2016-03-03
- Published: 2018-02-15
- Granted: 2020-12-15
- Earliest claimed: 2015-03-13
- Assignees: BASF SE
- Applicants: BASF SE
- Inventors: Torben Gaedt; Joachim Dengler; Martin Winklbauer; Manfred Bichler; Oliver Mazanec
- Web page: https://patentgrep.com/patent/US10865144B2

## CPC

- C04B 24/281: {Polyepoxides}
- C04B 28/04: Portland cements
- C04B 40/0042: {Powdery mixtures}
- C08J 3/122: {Pulverisation by spraying}
- C08K 3/346: {Clay}
- C04B 2103/0057: {added as redispersable powders}
- C04B 2103/408: {Dispersants}
- 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
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)

## Abstract

The invention relates to a method for producing a dispersant, comprising the steps of a) providing at least one water-soluble polymer comprising polyether groups, b) providing an inorganic component comprising at least one phyllosilicate which has an integral sheet charge of 0, 1 or 2, c) producing an aqueous suspension comprising the at least one water-soluble polymer comprising polyether groups and the inorganic component comprising the at least one phyllosilicate, and d) spray-drying the aqueous suspension to give a solid. Additionally disclosed is the use of the dispersant of the invention in an inorganic binder composition.

## Claims

### Claim 1

A method for producing a dispersant, comprising the steps of
a) providing at least one water-soluble polymer comprising polyether groups,
b) providing an inorganic component, comprising at least one phyllosilicate which has an integral sheet charge of 0, 1 or 2,
c) preparing an aqueous suspension comprising the at least one water-soluble polymer comprising polyether groups and the inorganic component comprising the at least one phyllosilicate,
d) spray-drying the aqueous suspension to give a solid.

### Claim 2 (depends on 1)

The method according to claim 1, wherein the polyether groups of the at least one water-soluble polymer are polyether groups of structural unit (I),
*—U—(C(O))k—X-(AlkO)n—W (I)
where
* indicates the bonding site to the polymer,
U is a chemical bond or an alkylene group having 1 to 8 carbon atoms,
X is oxygen, sulfur or a group NR1,
k is 0 or 1,
n is an integer whose average value based on the polymer is in the range from 3 to 300,
Alk is C2-C4 alkylene, it being possible for Alk to be identical or different within the group (Alk-O)n,
W is a hydrogen, a C1-C6 alkyl or an aryl radical or is the group Y—F, where
Y is a linear or branched alkylene group having 2 to 8 carbon atoms and may carry a phenyl ring,
F is a 5- to 10-membered nitrogen heterocycle which is bonded via nitrogen and which as ring members, besides the nitrogen atom and besides carbon atoms, may have 1, 2 or 3 additional heteroatoms, selected from oxygen, nitrogen, and sulfur, it being possible for the nitrogen ring members to have a group R2, and for 1 or 2 carbon ring members to be present in the form of a carbonyl group,
R1 is hydrogen, C1-C4 alkyl or benzyl, and
R2 is hydrogen, C1-C4 alkyl or benzyl.

### Claim 3 (depends on 1)

The method according to claim 1, wherein the water-soluble polymer comprises at least one group from the series consisting of carboxyester, carboxyl, phosphono, sulfino, sulfo, sulfamido, sulfoxy, sulfoalkyloxy, sulfinoalkyloxy, and phosphonooxy.

### Claim 4 (depends on 1)

The method according to claim 1, wherein the water-soluble polymer comprising polyether groups represents a polycondensation product comprising
(II) a structural unit comprising an aromatic or heteroaromatic and the polyether group, and
(III) a phosphated structural unit comprising an aromatic or heteroaromatic.

### Claim 5 (depends on 4)

The method according to claim 4, wherein the structural units (II) and (III) are represented by the following general formulae
A-U—(C(O))k—X-(AlkO)n—W (II)
where
A is identical or different and is represented by a substituted or unsubstituted, aromatic or heteroaromatic compound having 5 to 10 carbon atoms in the aromatic system, the other radicals possessing the definition stated for structural unit (I);
where
D is identical or different and is represented by a substituted or unsubstituted, aromatic or heteroaromatic compound having 5 to 10 carbon atoms in the aromatic system
where
E is identical or different and is represented by N, NH or O
where
m=2 if E=N and m=1 if E=NH or O
where
R3 and R4 independently of one another are identical or different and are represented by a branched or unbranched C1 to C10 alkyl radical, C5 to C8 cycloalkyl radical, aryl radical, heteroaryl radical or H
where b
is identical or different and is represented by an integer from 0 to 300.

### Claim 6 (depends on 4)

The method according to claim 4, wherein the polycondensation product comprises a further structural unit (IV) which is represented by the following formula
where
Y independently of one another is identical or different and is represented by (II), (III) or further constituents of the polycondensation product
R5 and R6 are identical or different and are represented by H, CH3, COOH, or a substituted or unsubstituted, aromatic or heteroaromatic compound having 5 to 10 carbon atoms.

### Claim 7 (depends on 1)

The method according to claim 1, wherein the water-soluble polymer comprising polyether groups represents at least one copolymer which is obtainable by polymerizing a mixture of monomers comprising
(V) at least one ethylenically unsaturated monomer which comprises at least one radical from the series consisting of carboxylic acid, carboxylic salt, carboxylic ester, carboxylic amide, carboxylic anhydride, and carboxylic imide
and
(VI) at least one ethylenically unsaturated monomer comprising the polyether group.

### Claim 8 (depends on 7)

The method according to claim 7, wherein the ethylenically unsaturated monomer (V) is represented by at least one of the following general formulae from the group of (Va), (Vb), and (Vc)
where
R7 and R8 independently of one another are hydrogen or an aliphatic hydrocarbon radical having 1 to 20 carbon atoms
B is H, —COOMa, —CO—O(CqH2qO)r—R9, or —CO—NH—(CqH2qO)r—R9
M is hydrogen, a mono-, di- or trivalent metal cation, ammonium ion or an organic amine radical
a is ⅓, ½ or 1
R9 is hydrogen, an aliphatic hydrocarbon radical having 1 to 20 carbon atoms, a cycloaliphatic hydrocarbon radical having 5 to 8 carbon atoms, or an optionally substituted aryl radical having 6 to 14 carbon atoms
q independently of one another for each (CqH2qO) unit is identical or different and is 2, 3 or 4, and
r is 0 to 200
Z is O, or NR16
R16 independently at each occurrence is identical or different and is represented by a branched or unbranched C1- to C10-alkyl radical, C5- to C8 cycloalkyl radical, aryl radical, heteroaryl radical or H,
where
R19 and R11 independently of one another are hydrogen or an aliphatic hydrocarbon radical having 1 to 20 carbon atoms, a cycloaliphatic hydrocarbon radical having 5 to 8 carbon atoms, or an optionally substituted aryl radical having 6 to 14 carbon atoms
R12 is identical or different and is represented by (CnH2n)—SO3H where n=0, 1, 2, 3 or 4, (CnH2n)—OH where n=0, 1, 2, 3 or 4; (CnH2n)—PO3H2 where n=0, 1, 2, 3 or 4, (CnH2n)—OPO3H2 where n=0, 1, 2, 3 or 4, (C6H4)—SO3H, (C6H4)—PO3H2, (C6H4)—OPO3H2, or (CnH2n)—NR14b where n=0, 1, 2, 3 or 4 and b=2 or 3
R13 is H, —COOMa, —OC—O(CqH2qO)r—R9, or —CO—NH—(CqH2qO)r—R9,
where Ma, R9, q, and r possess definitions stated above
R14 is hydrogen, an aliphatic hydrocarbon radical having 1 to 10 carbon atoms, a cycloaliphatic hydrocarbon radical having 5 to 8 carbon atoms, or an optionally substituted aryl radical having 6 to 14 carbon atoms
Q is identical or different and is represented by NH, NR15 or O; where R15 is an aliphatic hydrocarbon radical having 1 to 10 carbon atoms, a cycloaliphatic hydrocarbon radical having 5 to 8 carbon atoms, or an optionally substituted aryl radical having 6 to 14 carbon atoms.

### Claim 9 (depends on 1)

The method according to claim 1, wherein the at least one water-soluble polymer comprising polyether groups has an average molar weight (Mw) of between 5000 and 150,000 g/mol, as determined by gel permeation chromatography.

### Claim 10 (depends on 1)

The method according to claim 1, wherein the solid obtained after spray drying is in the form of powder or granules.

### Claim 11 (depends on 1)

The method according to claim 1, wherein amounts used in steps a) and b) are selected such that the solid obtained after the spray drying comprises
5 to 70 wt % of the at least one water-soluble polymer comprising polyether groups and
30 to 95 wt % of the at least one phyllosilicate which has an integral sheet charge of 0, 1 or 2.

### Claim 12 (depends on 1)

The method according to claim 1, wherein the at least one phyllosilicate is a 1:1 clay mineral having a sheet charge of 0.

### Claim 13 (depends on 1)

The method according to claim 1, wherein b) the inorganic component has an average particle size (d50%) as determined by laser diffractometry of between 100 nm and 2000 nm.