Superabsorbent polymer and preparation method thereof

Patent metadata

Field	Value
Publication number	US-11466131-B2
Application number	US-201916756921-A
Country	US
Kind code	B2
Filing date	Sep 17, 2019
Priority date	Nov 13, 2018
Publication date	Oct 11, 2022
Grant date	Oct 11, 2022

Abstract

Provided are a superabsorbent polymer and a preparation method thereof, including preparing a base resin and conducting surface modification of the base resin in the presence of an inorganic filler. The method of preparing the superabsorbent polymer of the present invention may provide a superabsorbent polymer having improved rewetting property and liquid permeability.

First claim

The invention claimed is:

1. A method of preparing a superabsorbent polymer, comprising:
preparing a base resin by crosslinking polymerization of an acrylic acid-based monomer having acidic groups, of which at least a part is neutralized, and an internal crosslinking agent;
preparing a surface crosslinking solution by dry-mixing the base resin with an inorganic filler and, subsequently, mixing with an epoxy-based surface crosslinking agent by dissolving in water to form the surface crosslinking solution; and
performing surface modification of the base resin by raising the temperature of the surface crosslinking solution,
wherein the epoxy-based surface crosslinking agent includes a first epoxy crosslinking agent having an epoxy equivalent weight of 100 g/eq or more to less than 130 g/eq and a second epoxy crosslinking agent having an epoxy equivalent weight of 130 g/eq to 200 g/eq.

2. The method of claim 1 , wherein the first epoxy crosslinking agent is included in an amount of 0.01 part by weight to 0.1 part by weight with respect to 100 parts by weight of the base resin, and the second epoxy crosslinking agent is included in an amount of 0.001 part by weight to 0.1 part by weight with respect to 100 parts by weight of the base resin.

3. The method of claim 1 , wherein the first epoxy crosslinking agent is one or more selected from the group consisting of ethyleneglycol diglycidyl ether and diethyleneglycol diglycidyl ether.

4. The method of claim 1 , wherein the second epoxy crosslinking agent is one or more selected from the group consisting of glycerol polyglycidyl ether, diglycerol polyglycidyl ether, polyglycerol polyglycidyl ether, and sorbitol polyglycidyl ether.

5. The method of claim 1 , wherein a hydrophobic material having HLB of 0 or more and 6 or less is further included during preparation of the surface crosslinking solution.

6. The method of claim 5 , wherein the hydrophobic material includes one or more of glyceryl stearate, glycol stearate, magnesium stearate, glyceryl laurate, sorbitan stearate, sorbitan trioleate, or PEG-4 dilaurate.

7. The method of claim 5 , wherein the hydrophobic material is mixed in an amount of 0.001 part by weight to 0.5 parts by weight with respect to 100 parts by weight of the base resin.

8. The method of claim 1 , wherein the surface modification is performed at a temperature of 120° C. to 190° C.

9. The method of claim 1 , wherein the preparing the base resin includes:
forming a water-containing gel polymer by polymerizing a monomer composition including the acrylic acid-based monomer having acidic groups, of which at least a part is neutralized, the internal crosslinking agent, and a polymerization initiator;
drying the water-containing gel polymer;
pulverizing the dried polymer; and
size-sorting the pulverized polymer.

10. A superabsorbent polymer comprising a base resin including a crosslinked polymer which is prepared by crosslinking polymerization of an acrylic acid-based monomer having acidic groups, of which at least a part is neutralized; and a double surface-modified layer which is formed on a particle surface of the base resin, and is prepared by additionally crosslinking the crosslinked polymer via two kinds of epoxy-based surface crosslinking agents having different epoxy equivalent weights,
wherein the double surface-modified layer includes an inorganic filler, and the two kinds of epoxy-based surface crosslinking agents include a first epoxy crosslinking agent having an epoxy equivalent weight of 100 g/eq or more to less than 130 g/eq and a second epoxy crosslinking agent having an epoxy equivalent weight of 130 g/eq to 200 g/eq.

11. The superabsorbent polymer of claim 10 , wherein the superabsorbent polymer has an absorption rate (vortex time) of 40 seconds or less.

12. The superabsorbent polymer of claim 10 , wherein the superabsorbent polymer has a liquid permeability (unit: second) of 35 seconds or less, as measured according to the following Equation 1:
Liquid permeability (sec)= T 1 −B   [Equation 1]

in Equation 1, T1 represents a time taken for a liquid level to decrease from 40 ml to 20 ml, when 0.2±0.0005 g of a size-sorted superabsorbent polymer sample (300 μm˜600 μm) is put in a chromatography column, brine is applied thereto at a volume of 50 ml, and then left for 30 minutes, and B represents a time taken for a liquid level in a brine-filled chromatography column to decrease from 40 ml to 20 ml.

13. The superabsorbent polymer of claim 10 , wherein the superabsorbent polymer has a centrifuge retention capacity (CRC) of 25 g/g or more.

14. The superabsorbent polymer of claim 10 , wherein the superabsorbent polymer has a rewetting property (long-term tap water rewetting under pressure) of 1.0 g or less, the rewetting property defined by a weight of water that soaks out from the superabsorbent polymer to a filter paper, when 4 g of the superabsorbent polymer is immersed in 200 g of tap water and allowed to swell for 2 hours, and then the swollen superabsorbent polymer is left on the filter paper under a pressure of 0.75 psi for 1 minute.

Assignees

• Lg Chemical Ltd

Inventors

• Hur Young Jae
• Nam Dae Woo
• Park Bohee
• Kim Sujin

Classifications

• C08K5/1515

  Three-membered rings · CPC title

• A61L15/60

  Liquid-swellable gel-forming materials, e.g. super-absorbents · CPC title

• C08K3/013

  Fillers, pigments or reinforcing additives · CPC title

• C08K3/12

  Hydrides · CPC title

• C08F2810/20

  leading to a crosslinking, either explicitly or inherently · CPC title