Preparation method of porous super absorbent polymer

Patent metadata

Field	Value
Publication number	US-10562992-B2
Application number	US-201716090722-A
Country	US
Kind code	B2
Filing date	Dec 13, 2017
Priority date	Dec 26, 2016
Publication date	Feb 18, 2020
Grant date	Feb 18, 2020

Abstract

The present disclosure relates to a preparation method of a porous super absorbent polymer including the steps of preparing a monomer neutralized solution by adding an internal cross-linking agent, an initiator, an inorganic filler, and a nonionic surfactant to a neutralized solution obtained by neutralizing at least 80 mol % of a water soluble ethylene-based unsaturated monomer containing acidic groups; high-shear mixing the monomer neutralized solution; preparing a hydrogel polymer from the high-shear mixed monomer neutralized solution by thermal polymerization or photopolymerization; and preparing a base resin powder by drying, pulverizing, and classifying the hydrogel polymer.

First claim

The invention claimed is:

1. A preparation method of a porous super absorbent polymer, comprising the steps of:
preparing a monomer neutralized solution by adding an internal cross-linking agent, an initiator, an inorganic filler, and a nonionic surfactant to a neutralized solution obtained by neutralizing at least 80 mol % of a water soluble ethylene-based unsaturated monomer containing acidic groups;
high-shear mixing the monomer neutralized solution;
preparing a hydrogel polymer from the high-shear mixed monomer neutralized solution by thermal polymerization or photopolymerization; and
preparing a base resin powder by drying, pulverizing, and classifying the hydrogel polymer.

2. The preparation method of a porous super absorbent polymer of claim 1 ,
wherein the nonionic surfactant is used in an amount of 0.1 to 5 parts by weight based on 100 parts by weight of the water soluble ethylene-based unsaturated monomer containing acidic groups.

3. The preparation method of a porous super absorbent polymer of claim 1 ,
wherein the nonionic surfactant comprises at least one selected from the group consisting of alkylene glycol, polyethylene glycol, poly(ethylene-propylene) glycol, polyvinyl alcohol, polyoxyethylene alkyl ether, sorbitan ester of fatty acid, fatty acid diethanolamine and alkyl monoglyceryl ether.

4. The preparation method of a porous super absorbent polymer of claim 1 ,
wherein the step of high-shear mixing the monomer neutralized solution comprises a step of mixing the monomer neutralized solution at a rate of 1,000 to 20,000 rpm.

5. The preparation method of a porous super absorbent polymer of claim 1 ,
wherein the step of high-shear mixing the monomer neutralized solution is carried out for 1 min to 100 min.

6. The preparation method of a porous super absorbent polymer of claim 1 ,
further comprising a step of adding a basic compound to the water soluble ethylene-based unsaturated monomer containing acidic groups to form a neutralized solution which is at least 80 mol % neutralized.

7. The preparation method of a porous super absorbent polymer of claim 1 ,
wherein the water soluble ethylene-based unsaturated monomer comprises at least one selected from the group consisting of: an anionic monomer of acrylic acid, methacrylic acid, maleic anhydride, fumalic acid, crotonic acid, itaconic acid, 2-acryloylethane sulfonic acid, 2-methacryloylethane sulfonic acid, 2-(meth)acryloylpropane sulfonic acid, or 2-(meth)acrylamide-2-methyl propane sulfonic acid, and a salt thereof;
a nonionic hydrophilic monomer of (meth)acrylamide, N-substituted (meth)acrylate, 2-hydroxyethyl(meth)acrylate, 2-hydroxypropyl(meth)acrylate, methoxypolyethyleneglycol(meth)acrylate, or polyethyleneglycol(meth)acrylate; and
an amino-containing unsaturated monomer of (N,N)-dimethylaminoethyl(meth)acrylate or (N,N)-dimethylaminopropyl(meth)acrylamid, and a quaternary compound thereof.

8. The preparation method of a porous super absorbent polymer of claim 1 ,
wherein the internal cross-linking agent comprises at least one selected from the group consisting of polyethylene glycol diacrylate (PEGDA), glycerine diacrylate, glycerine triacrylate, unmodified or ethoxylated trimethylol triacrylate (TMPTA), hexanediol diacrylate, and triethylene glycol diacrylate.

9. The preparation method of a porous super absorbent polymer of claim 1 ,
wherein the inorganic particle is a silica nanoparticle or an alumina nanoparticle surface-modified with a cross-linkable or hydrophilic functional group containing at least one functional group selected from the group consisting of a (meth)acrylate-based functional group, an allyl group, a vinyl group, an epoxy group, a hydroxyl group, an isocyanate group and an amine group.

10. The preparation method of a porous super absorbent polymer of claim 1 ,
further comprising a step of further cross-linking the surface of the base resin powder in the presence of a surface cross-linking agent to form a surface cross-linked layer.

11. The preparation method of a porous super absorbent polymer of claim 10 ,
wherein the surface cross-linking agent comprises at least one selected from the group consisting of ethylene glycol, 1,4-butanediol, 1,6-hexanediol, propylene glycol, 1,2-hexanediol, 1,3-hexanediol, 2-methyl-1,3-propanediol, 2,5-hexanediol, 2-methyl-1,3-pentanediol, 2-methyl-2,4-pentanediol, tripropylene glycol, glycerol, ethylene carbonate and propylene carbonate.

12. The preparation method of a porous super absorbent polymer of claim 1 ,
wherein the water soluble ethylene-based unsaturated compound is included in an amount of 20 to 60 wt % in the monomer neutralized solution.

Assignees

• Lg Chemical Ltd

Inventors

• Yoon Ki Youl
• Joo Hyo Sook
• Kim Gi Cheul
• Choi Hyeon
• Kim Ju Eun

Classifications

• C08J3/075

  Macromolecular gels · CPC title

• C08J2333/10

  Homopolymers or copolymers of methacrylic acid esters · CPC title

• C08K5/00

  Use of organic ingredients · CPC title

• C08J2333/08

  Homopolymers or copolymers of acrylic acid esters · CPC title

• C08F6/02

  Neutralisation of the polymerisation mass, e.g. killing the catalyst (short-stopping C08F2/42 ){also removal of catalyst residues} · CPC title