IP Library › Granted Patent US 11,370,856
Granted Patent B2
US 11,370,856 · App. 17/041,227 · Granted Jun 28, 2022

Super absorbent polymer and preparation method for the same

Inventors: Dae Woo Nam (Daejeon, KR); Ki Hyun Kim (Daejeon, KR); Jun Kyu Kim (Daejeon, KR); Young Jae Hur (Daejeon, KR)
C08F20/06C08J3/12C08J3/24A61L15/24C08F220/06C08F222/102C08F222/103C08F222/104C08F222/105C08F222/1006C08J2433/08C08K3/36
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Quick Facts
Patent No.
US 11,370,856
App. No.
17/041,227
Granted
Jun 28, 2022
Kind
B2
Abstract

The present invention relates to super absorbent polymer and a method for preparing the same. According to the super absorbent polymer and preparation method for the same of the present invention, super absorbent polymer having improved rewet property and vortex time can be provided.

Claims (38)

1. A super absorbent polymer comprising:

base resin particles in which acrylic acid-based monomers having acid groups, of which at least a part is neutralized, and an internal cross-linking agent are cross-linked in the form of a cross-linked polymer;

a surface modification layer formed on a surface of the base resin particles, in which the cross-linked polymer is additionally cross-linked by an epoxy-based surface cross-linking agent; and

an inorganic filler,

wherein the internal cross-linking agent comprises a poly(meth)acrylate-based first internal cross-linking agent and a polyol polyglycidyl ether-based second internal cross-linking agent at a weight ratio of the first internal cross-linking agent to the second internal cross-linking agent of 1:40 to 1:1200, and

the surface modification layer includes a hydrophobic material having a melting temperature (Tm) of 40 to 80° C., and a water solubility at 25° C. of 70 mg/L or less.

2. The super absorbent polymer according to claim 1 , wherein the first internal cross-linking agent includes one or more of trimethylolpropane tri(meth)acrylate, ethyleneglycol di(meth)acrylate, polyethyleneglycol di(meth)acrylate, propyleneglycol di(meth)acrylate, polypropyleneglycol di(meth)acrylate, butanediol di(meth)acrylate, diethyleneglycol di(meth)acrylate, hexanediol di(meth)acrylate, triethyleneglycol di(meth)acrylate, tripropyleneglycol di(meth)acrylate, tetraethyleneglycol di(meth)acrylate, dipentaerythritol pentaacrylate, glycerin tri(meth)acrylate, or pentaerythritol tetraacrylate.

3. The super absorbent polymer according to claim 1 , wherein the second internal cross-linking agent includes one or more of ethyleneglycol diglycidyl ether, polyethyleneglycol diglycidyl ether, glycerol polyglycidyl ether, propyleneglycol diglycidyl ether, or polypropyleneglycol diglycidyl ether.

4. The super absorbent polymer according to claim 1 , wherein the super absorbent polymer has extractable contents (EC) measured according to EDANA method WSP 270.2 of 9.0 wt % or less.

5. The super absorbent polymer according to claim 1 , wherein the super absorbent polymer has a vortex time of 35 seconds or less.

6. The super absorbent polymer according to claim 1 , wherein the super absorbent polymer has a permeability (unit: seconds) measured according to the following Equation 1, of 40 seconds or less:

Permeability (sec)= T 1− B   [Equation 1]

in the Equation 1,

T1 is a time taken until a height of a liquid level decreases from 40 ml to 20 ml, after putting 0.2±0.0005 g of a sieved (30#˜50#) super absorbent polymer sample in a chromatography column and adding brine to a volume of 50 ml, and then, leaving it for 30 minutes; and B is a time taken until a height of a liquid level decreases from 40 ml to 20 ml in a chromatography column filled with brine.

7. The super absorbent polymer according to claim 1 , wherein the super absorbent polymer has a rewet property (tap water short-term rewet under no pressure) of 1.5 g or less, said rewet property being defined by a weight of water exuding from super absorbent polymer to a filter paper, after 1 g of the super absorbent polymer is soaked in 100 g of tap water to swell for 10 minutes, and then, the swollen super absorbent polymer is left on the filter paper for 1 hour from a first time when it is soaked in the tap water.

8. The super absorbent polymer according to claim 1 , wherein the super absorbent polymer has a rewet property (tap water long-term rewet under pressure) of 1.5 g or less, said rewet property being defined by a weight of water exuding from super absorbent polymer to a filter paper, after 4 g of the super absorbent polymer is soaked in 200 g of tap water to swell for 2 hours, and then, the swollen super absorbent polymer is left on the filter paper for 1 minute under pressure of 0.75 psi.

9. A method for preparing super absorbent polymer comprising:

preparing a base resin in which acrylic acid-based monomers having acid groups, of which at least a part are neutralized, and an internal cross-linking agent are cross-linked;

mixing a hydrophobic material having a melting temperature (Tm) of 40 to 80° C., and a water solubility at 25° C. of 70 mg/L or less, and an epoxy-based surface cross-linking agent with the base resin to prepare a mixture; and

increasing a temperature of the mixture to conduct surface modification of the base resin,

wherein the internal cross-linking agent comprises a poly(meth)acrylate-based first internal cross-linking agent and a polyol polyglycidyl ether-based second internal cross-linking agent at a weight ratio of the first internal cross-linking agent to the second internal cross-linking agent of 1:40 to 1:1200, and

an inorganic filler is additionally mixed with the base resin in the mixture, or the inorganic filler is mixed with the super absorbent polymer as the temperature of the mixture is increased to conduct surface modification.

10. The method for preparing super absorbent polymer according to claim 9 , wherein while preparing the mixture, the hydrophobic material is dry-mixed with the base resin, and then, the epoxy-based surface cross-linking agent is dissolved in water and mixed in a state of a surface cross-linking solution.

11. The method for preparing super absorbent polymer according to claim 9 , wherein the hydrophobic material includes one or more of lauric acid, myristic acid, cetyl alcohol, stearic acid, glycol stearate, glycerol monostearate, glycol distearate, stearin, pentaerythrityl distearate, or oleamide.

12. The method for preparing super absorbent polymer according to claim 9 , wherein the hydrophobic material is mixed in a content of 0.02 to 0.5 parts by weight, based on 100 parts by weight of the base resin.

13. The method for preparing super absorbent polymer according to claim 9 , wherein the first internal cross-linking agent includes one or more of trimethylolpropane tri(meth)acrylate, ethyleneglycol di(meth)acrylate, polyethyleneglycol di(meth)acrylate, propyleneglycol di(meth)acrylate, polypropyleneglycol di(meth)acrylate, butanediol di(meth)acrylate, diethyleneglycol di(meth)acrylate, hexanediol di(meth)acrylate, triethyleneglycol di(meth)acrylate, tripropyleneglycol di(meth)acrylate, tetraethyleneglycol di(meth)acrylate, dipentaerythritol pentaacrylate, glycerin tri(meth)acrylate, or pentaerythritol tetraacrylate.

14. The method for preparing super absorbent polymer according to claim 9 , wherein the second internal cross-linking agent includes one or more of ethyleneglycol diglycidyl ether, polyethyleneglycol diglycidyl ether, glycerol polyglycidyl ether, propyleneglycol diglycidyl ether, or polypropyleneglycol diglycidyl ether.

15. The method for preparing super absorbent polymer according to claim 9 , wherein the epoxy-based surface cross-linking agent includes one or more of ethyleneglycol diglycidyl ether, diethyleneglycol diglycidyl ether, triethyleneglycol diglycidyl ether, tetraethyleneglycol diglycidyl ether, glycerin polyglycidyl ether, or sorbitol polyglycidyl ether.

16. The method for preparing super absorbent polymer according to claim 9 , wherein the epoxy-based surface cross-linking agent is mixed in a content of 0.005 to 0.5 parts by weight, based on 100 parts by weight of the base resin.

17. The method for preparing super absorbent polymer according to claim 9 , wherein the temperature of the mixture is increased to 100 to 170° C.

18. The method for preparing super absorbent polymer according to claim 9 , wherein the inorganic filler includes one or more of fumed silica or precipitated silica, and

the inorganic filler is mixed in a content of 0.01 to 0.5 parts by weight, based on 100 parts by weight of the base resin or super absorbent polymer.

19. The method for preparing super absorbent polymer according to claim 9 , wherein the preparing the base resin comprises:

polymerizing a monomer composition comprising acrylic acid-based monomers having acid groups, of which at least a part is neutralized, an internal crosslinking agent, and a polymerization initiator to form hydrogel polymer;

drying the hydrogel polymer;

grinding the dried polymer; and

sieving the ground polymer.

20. The method for preparing super absorbent polymer according to claim 19 , wherein the monomer composition further comprises colloidal silica included in a content of 0.01 to 1.0 parts by weight, based on 100 parts by weight of the acrylic acid-based monomers.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 29, 2020
From: NAM, DAE WOO; KIM, KI HYUN; KIM, JUN KYU; HUR, YOUNG JAE
To: LG CHEM, LTD.
Reel/Frame 053917/0274 →
Priority Claims (2)
KR 10-2018-0037268 · Mar 30, 2018 · national
KR 10-2019-0031083 · Mar 19, 2019 · national
Continuity (1)
Related Publication 20210009725A1 · Jan 14, 2021