# US 11,111,464 B2 · Method of manufacturing an automatic dishwashing detergent product

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- Number: US 11,111,464 B2
- Document ID: US11111464B2
- Status: Granted
- Kind: B2
- Application number: 15/931,054
- Filed: 2020-05-13
- Published: 2020-08-27
- Granted: 2021-09-07
- Earliest claimed: 2014-07-02
- Assignees: Reckitt Benckiser Finish B.V.
- Applicants: Reckitt Benckiser Finish B.V.
- Inventors: Pavlinka Roy; Claudia Schmaelzle; Caroline Rigobert; Heike Weber; Helmut Witteler; Yannick Fuchs; Roland Bohn
- Web page: https://patentgrep.com/patent/US11111464B2

## CPC

- C08F 2/06: Organic solvent
- C08F 2/08: with the aid of dispersing agents for the polymer
- C08F 2/44: Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
- C08F 120/06: Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
- C11D 1/66: Non-ionic compounds {(C11D1/002, C11D1/004, C11D1/008 take precedence)}
- C11D 1/72: Ethers of polyoxyalkylene glycols
- C11D 3/2065: {Polyhydric alcohols}
- C11D 3/3757: {(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions}
- C11D 3/43: Solvents
- C11D 17/042: {Water soluble or water disintegrable containers or substrates containing cleaning compositions or additives for cleaning compositions}
- C11D 17/045: {Multi-compartment}
- C11D 2111/14: Hard surfaces
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C11D: DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL

## Abstract

A method of manufacturing an automatic dishwashing detergent product, provided as a discrete dosage unit and comprising a continuous, non-aqueous gel phase, includes manufacturing the gel phase by free radical polymerisation of monomer(s) in a non-aqueous reaction mixture to form a polymeric builder. The reaction mixture comprises at least one non-ionic surfactant which is an optionally end-capped alcohol alkoxylate; and one or more monomers comprising acrylic acid and optionally one or more further α,β-ethylenically unsaturated acids, wherein no more than 0.1 wt % of the total amount of the monomer(s) are crosslinking monomer(s).

## Claims

### Claim 1

An automatic dishwashing detergent product provided as a discrete dosage unit comprising a continuous, non-aqueous gel phase, the gel phase comprising 10 wt % to 50 wt. % of non-ionic surfactant and at least 20 wt % polymeric builder, wherein:
the polymeric builder is in a dissolved state in the non-aqueous gel phase,
the non-ionic surfactant is one or more optionally end-capped alcohol alkoxylates,
the polymeric builder is made by the free radical polymerization of acrylic acid monomer and optionally one or more further α,β-ethylenically unsaturated acids, wherein no more than 0.1 wt % of the total amount of the monomers are crosslinking monomers,
the free radical polymerization reaction occurs in a non-aqueous liquid reaction mixture comprising the non-ionic surfactant and 10 wt. % to 60 wt. % of at least one non-water solvent comprising a water-soluble organic solvent, without an intermediate step of drying the non-aqueous liquid to form a solid comprising the polymeric builder; and
the polymeric builder has a weight average molecular weight in the range of 1000-70000 g/mol.

### Claim 2 (depends on 1)

The automatic dishwashing detergent product of claim 1, wherein the gel phase is free of any ionic surfactant.

### Claim 3 (depends on 1)

The automatic dishwashing detergent product of claim 1, wherein the non-aqueous liquid reaction mixture comprises a monomer comprising acrylic acid.

### Claim 4 (depends on 1)

The automatic dishwashing detergent product of claim 1, wherein the non-aqueous liquid reaction mixture further comprises a monomer comprising α,β-ethylenically unsaturated acid.

### Claim 5 (depends on 1)

The automatic dishwashing detergent product of claim 1, wherein the non-ionic surfactant comprises an end-capped alcohol alkoxylate.

### Claim 6 (depends on 5)

The automatic dishwashing detergent product of claim 5, wherein the end-capped alcohol alkoxylate surfactant is liquid at 20° C.

### Claim 7 (depends on 1)

The automatic dishwashing detergent product of claim 1, wherein the alcohol alkoxylate non-ionic surfactant is of the formula R1—O-(EO)x(AO)y—R4, in which:
R1 is an alkyl group;
R4 is H or an optionally substituted alkyl group;
x is 1 to 100;
y is 0 to 100;
EO is ethylene oxide; and
each AO, when present, is independently propylene oxide or butylene oxide;
wherein x and y represent the average degrees of respective alkoxylation per molecule; and
wherein the order of EO and AO groups may be varied but the sum of x and y is at least 3.

### Claim 8 (depends on 1)

The automatic dishwashing detergent product of claim 1, wherein up to 40 mol % of acid groups in the polymeric builder are in neutralized form.

### Claim 9 (depends on 4)

The automatic dishwashing detergent product of claim 4, wherein the non-aqueous liquid reaction mixture comprises at least 20 wt % in total of the monomers.

### Claim 10 (depends on 4)

The automatic dishwashing detergent product of claim 4, wherein the non-aqueous liquid reaction mixture is free of crosslinking monomers.

### Claim 11 (depends on 4)

The automatic dishwashing detergent product of claim 4, wherein the α,β-ethylenically unsaturated acid is a carboxylic acid selected from the group consisting of methacrylic acid, ethacrylic acid, maleic acid, crotonic acid, itaconic acid, citraconic acid, mesaconic acid, glutaconic acid, aconitic acid, and fumaric acid.

### Claim 12 (depends on 4)

The automatic dishwashing detergent product of claim 4, wherein the weight ratio of acrylic acid to α,β-ethylenically unsaturated acid in the reaction mixture is in the range of 100:1 to 1:1.

### Claim 13 (depends on 1)

The automatic dishwashing detergent product of claim 1, wherein the water-soluble organic solvent is monopropylene glycol or dipropylene glycol.

### Claim 14 (depends on 1)

The automatic dishwashing detergent product of claim 1, wherein the non-water solvent is a water-soluble organic solvent selected from the group consisting of alkylene glycol, dialkylene glycol, monopropylene glycol, and dipropylene glycol.

### Claim 15 (depends on 1)

The automatic dishwashing detergent product of claim 1, wherein the non-aqueous liquid reaction mixture further comprises a chain transfer agent.

### Claim 16 (depends on 1)

The automatic dishwashing detergent product of claim 1, wherein the discrete dosage unit comprises a multi-compartment water-soluble container.

### Claim 17 (depends on 1)

The automatic dishwashing detergent product of claim 1, wherein the discrete dosage unit comprises a multi-compartment water-soluble container,
wherein the multi-compartment water-soluble container further comprises a solid composition in a different compartment of the multi-compartment water-soluble container, and
wherein the solid composition comprises a component selected from the group consisting of a bleach, an enzyme, a builder, and combinations thereof.
