# US 11,028,237 B2 · Method for preparing superabsorbent polymer and superabsorbent polymer prepared thereby

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- Number: US 11,028,237 B2
- Document ID: US11028237B2
- Status: Granted
- Kind: B2
- Application number: 16/341,804
- Filed: 2018-06-21
- Published: 2019-10-17
- Granted: 2021-06-08
- Earliest claimed: 2017-06-30
- Assignees: LG Chem, Ltd.
- Applicants: LG Chem, Ltd.
- Inventors: Taehee Kim; Sewoo Yang; Ji Young Hwang; Gi Cheul Kim
- Web page: https://patentgrep.com/patent/US11028237B2

## CPC

- C08J 3/075: Macromolecular gels
- C08L 71/02: Polyalkylene oxides
- A61L 15/60: Liquid-swellable gel-forming materials, e.g. super-absorbents
- B01J 20/267: {Cross-linked polymers}
- B01J 20/28047: {Gels}
- B01J 20/3028: {Granulating, agglomerating or aggregating}
- B01J 20/3042: {Use of binding agents; addition of materials ameliorating the mechanical properties of the produced sorbent}
- B01J 20/3085: {Chemical treatments not covered by groups B01J20/3007 - B01J20/3078}
- C08F 220/06: Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
- C08J 3/12: Powdering or granulating
- C08J 3/24: Crosslinking, e.g. vulcanising, of macromolecules (mechanical aspects B29C35/00; crosslinking agents C08K)
- C08J 3/245: {Differential crosslinking of one polymer with one crosslinking type, e.g. surface crosslinking}
- B01J 2220/68: Superabsorbents
- C08J 2333/14: of esters containing halogen, nitrogen, sulfur, or oxygen atoms in addition to the carboxy oxygen
- C08J 2471/02: Polyalkylene oxides
- 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)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- A61L: METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES (preservation of bodies or disinfecting characterised by the agents employed A01N; preserving, e.g. sterilising, food or foodstuffs A23; preparations for medical, dental or toiletry purposes A61K)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS

## Abstract

The present invention relates to a method for preparing a superabsorbent polymer that progresses dry mixing of fine powders and a specific powder type of polymer binder when reassembling fine powders generated during the preparation process of a superabsorbent polymer, and thus obviates the necessity for a moisture drying process after reassembling fine powders, thereby reducing thermal losses, improving productivity, and obtaining a superabsorbent polymer having excellent basic absorption properties, and a superabsorbent polymer prepared by the method.

## Claims

### Claim 1

A method for preparing a superabsorbent polymer, comprising:
conducting crosslinking polymerization of water soluble ethylenically unsaturated monomers comprising monomers having acid groups of which at least a part are neutralized, in the presence of an internal crosslinking agent, to form a hydrogel polymer comprising a first crosslinked polymer;
gel grinding the hydrogel polymer to form a gel ground hydrogel polymer;
drying the gel ground hydrogel polymer, and grinding and sieving the dried hydrogel polymer to form base polymer powders; and
heat treating the base polymer powders to progress surface crosslinking, in the presence of a surface crosslinking agent to produce the superabsorbent polymer,
wherein the method further comprises:
recovering fine powders, after sieving the dried hydrogel polymer;
reassembling the fine powders in the presence of a powder type of polymer binder to provide reassembled fine powders; and
introducing the reassembled fine powders in the step of gel grinding the hydrogel polymer to mix the reassembled fine powders with the hydrogel polymer before drying,
wherein the powder type of polymer binder consists of polyethylene oxide powders having a weight average molecular weight of 100,000 to 600,000 g/mol.

### Claim 2 (depends on 1)

The method for preparing a superabsorbent polymer according to claim 1, wherein the fine powders have an average particle diameter less than 150 μm and wherein the reassembling the fine powders comprises dry mixing the fine powders and the powder type of polymer binder under a solvent-free condition, and then reassembling the fine powders through heat treatment.

### Claim 3 (depends on 2)

The method for preparing a superabsorbent polymer according to claim 2, wherein the heat treatment is conducted at 105 to 180° C. for 10 to 20 minutes.

### Claim 4 (depends on 1)

The method for preparing a superabsorbent polymer according to claim 1, wherein the powder type of polymer binder is used in an amount of 1 to 100 parts by weight, based on 100 parts by weight of the fine powders.

### Claim 5 (depends on 1)

The method for preparing a superabsorbent polymer according to claim 1, wherein the reassembled fine powders are mixed in an amount of 10 to 30 parts by weight, based on 100 parts by weight of the hydrogel polymer before drying.

### Claim 6 (depends on 1)

The method for preparing a superabsorbent polymer according to claim 1, wherein the gel grinding of the hydrogel polymer is conducted two or more times.

### Claim 7 (depends on 1)

The method for preparing a superabsorbent polymer according to claim 1, wherein the water soluble ethylenically unsaturated monomers include one or more of anionic monomers and salts thereof selected from acrylic acid, methacrylic acid, maleic anhydride, fumaric acid, crotonic acid, itaconic acid, 2-acryloylethane sulfonic acid, 2-methacryloylethane sulfonic acid, 2-(meth)acryloyl propane sulfonic acid, and 2-(meth)acrylamide-2-methylpropane sulfonic acid; non-ionic hydrophilic group-containing monomers selected from (meth)acrylamide, N-substituted (meth)acrylate, 2-hydroxyethyl (meth)acrylate, 2-hydroxypropyl (meth)acrylate, methoxy polyethylene glycol (meth)acrylate, and polyethylene glycol (meth)acrylate; or amino group-containing unsaturated monomers selected from (N,N)-dimethylaminoethyl (meth)acrylate, (N,N)-dimethylaminopropyl (meth)acrylamide, and quaternized products thereof.

### Claim 8 (depends on 1)

The method for preparing a superabsorbent polymer according to claim 1, wherein the first crosslinked polymer includes a polymer formed by the crosslinking polymerization of the water soluble ethylenically unsaturated monomers, in the presence of a polyol poly(meth)acrylate-based first internal crosslinking agent selected from the group consisting of trimethylolpropane tri(meth)acrylate, ethylene glycol di(meth)acrylate, polyethylene glycol di(meth)acrylate, propylene glycol di(meth)acrylate, polypropylene glycol di(meth)acrylate, butanediol di(meth)acrylate, butylene glycol di(meth)acrylate, diethylene glycol di(meth)acrylate, hexanediol di(meth)acrylate, triethylene glycol di(meth)acrylate, tripropylene glycol di(meth)acrylate, tetraethylene glycol di(meth)acrylate, dipentaerythritol pentaacrylate, glycerin tri(meth)acrylate, and pentaerythritol tetraacrylate; and an allyl(meth)acrylate-based second internal crosslinking agent.

### Claim 9 (depends on 1)

The method for preparing a superabsorbent polymer according to claim 1, wherein the internal crosslinking agent includes a polyol poly(meth)acrylate-based first internal crosslinking agent and an allyl (meth)acrylate-based second internal crosslinking agent, and
the first internal crosslinking agent is included in a content of 0.4 parts by weight to 1 part by weight, based on 100 parts by weight of a monomer composition comprising the internal crosslinking agent and water soluble ethylenically unsaturated monomers, and the second internal crosslinking agent is included in a content of 0.008 parts by weight to 0.5 parts by weight, based on 100 parts by weight of the monomer composition.

### Claim 10 (depends on 1)

The method for preparing a superabsorbent polymer according to claim 1, wherein the surface crosslinking agent includes an alkylene carbonate-based compound or a polyhydric alcohol compound.

### Claim 11 (depends on 1)

The method for preparing a superabsorbent polymer according to claim 1, wherein the powder type of polymer binder is used in an amount of 10 to 25 parts by weight, based on 100 parts by weight of the fine powders.

### Claim 12

A superabsorbent polymer comprising:
base polymer powders comprising a first crosslinked polymer of water soluble ethylenically unsaturated monomers having acid groups of which at least a part are neutralized;
a surface crosslink layer formed on the base polymer powders, and comprising a second crosslinked polymer in which the first crosslinked polymer is additionally crosslinked by a surface crosslinking agent;
reassembled fine powders; and
a powder type of polymer binder consisting of polyethylene oxide powders having a weight average molecular weight of 100,000 to 600,000 g/mol;
wherein a centrifuge retention capacity (CRC) of the superabsorbent polymer for a saline solution having 0.9 wt % sodium chloride in aqueous solution for 30 minutes is 30 g/g to 45 g/g.

### Claim 13 (depends on 12)

The superabsorbent polymer according to claim 12, wherein the superabsorbent polymer has a particle diameter of 150 to 850 μm.