IP Library › Granted Patent US 11,325,101
Granted Patent B2
US 11,325,101 · App. 15/556,740 · Granted May 10, 2022

Super absorbent polymer and method for preparing the same

Inventors: Sang Gi Lee (Daejeon, KR); Hye Mi Nam (Daejeon, KR); Min Ho Hwang (Daejeon, KR); Soo Jin Lee (Daejeon, KR); Tae Hwan Jang (Daejeon, KR)
B01J20/267A61L15/60B01J20/103B01J20/265B01J20/28004B01J20/3021B01J20/3064B01J20/3078B01J20/3085C08F2/26C08F6/008C08F20/14C08F20/18C08F220/06C08J3/245C08K3/36C08K5/20B01J2220/68C08J2333/02
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Quick Facts
Patent No.
US 11,325,101
App. No.
15/556,740
Granted
May 10, 2022
Kind
B2
Abstract

The present invention relates to a super absorbent polymer having not only excellent absorption rate and absorbency under load but also excellent rewetting properties, and a method for preparing the same.

Claims (80)

1. A super absorbent polymer comprising:

a base polymer powder containing a first crosslinked polymer of a water-soluble ethylene-based unsaturated monomer having an acidic group in which at least a part thereof is neutralized; and

a surface-crosslinked layer containing a second crosslinked polymer formed on the base polymer powder in which the first crosslinked polymer is additionally crosslinked via a surface crosslinking agent,

wherein the superabsorbent polymer is prepared by:

1) performing thermal polymerization or photopolymerization of a monomer composition comprising the water-soluble ethylene-based unsaturated monomer having the acidic group in which at least the part thereof is neutralized, a carbonate forming agent, an anionic surfactant and a polymerization initiator to form a hydrogel polymer, wherein the anionic surfactant is dioctyl sodium sulfosuccinate,

2) drying the hydrogel polymer,

3) pulverizing the dried polymer, and

4) performing surface cros slinking reaction of the pulverized polymer; and

wherein the super absorbent polymer has:

an average particle diameter of 300 μm to 600 μm,

CRC of 28 g/g to 35 g/g,

AUL (0.9 psi) of 18 g/g to 25 g/g,

10-min WAUL of 15 g/g to 25 g/g,

a gel bed permeability (GBP) for a physiological saline solution of 30 darcy or more,

5-min Gel-Vacuum AUL of 18 g/g to 25 g/g, and

a vortex time of 5 seconds to 50 seconds,

wherein

the WAUL is measured according to the following Equation 1:

WAUL(g/g)=[W 2 (g)−W 1 (g)]/ W 0 (g)   [Equation 1]

in Equation 1,

W 0 (g) is an initial weight(g) of the super absorbent polymer,

W 1 (g) is the total sum of a weight of the super absorbent polymer and a weight of the device capable of providing a load to the super absorbent polymer,

W 2 (g) is the total sum of a weight of the super absorbent polymer and a weight of the device capable of providing a load to the super absorbent polymer, after absorbing a physiological saline solution below 15 cm from the super absorbent polymer under a load (0.7 psi) for 10 minutes,

wherein the vortex time means the amount of time required until the vortex disappears after adding 2 g of a super absorbent polymer to 50 mL of physiological saline solution and then stirring the mixture at 600 rpm, and

wherein

the 5-min Gel-Vacuum AUL is measured according to the following Equation 5:

5-min Gel-Vacuum AUL(g/g)=[W 8 (g)−W 7 (g)]/ W 0 (g)   [Equation 5]

in Equation 5,

W 0 (g) is an initial weight(g) of the super absorbent polymer,

W 7 (g) is the total sum of the weight of the super absorbent polymer and the weight of the device capable of providing a load to the super absorbent polymer, and

W 8 (g) is the total sum of the weight of the super absorbent polymer and the weight of the device capable of providing a load to the super absorbent polymer, after absorbing a physiological saline solution to the super absorbent polymer under a load (0.3 psi) for 5 minutes and removing the remaining liquid with a vacuum device.

2. A super absorbent polymer comprising:

a base polymer powder containing a first crosslinked polymer of a water-soluble ethylene-based unsaturated monomer having an acidic group in which at least a part thereof is neutralized; and

a surface-crosslinked layer containing a second crosslinked polymer formed on the base polymer powder in which the first crosslinked polymer is additionally crosslinked via a surface crosslinking agent,

wherein the first crosslinked polymer is a porous polymer containing a plurality of pores on a micron (μm) scale,

wherein the superabsorbent polymer is prepared by:

1) performing thermal polymerization or photopolymerization of a monomer composition comprising the water-soluble ethylene-based unsaturated monomer having the acidic group in which at least the part thereof is neutralized, a carbonate forming agent, an anionic surfactant and a polymerization initiator to form a hydrogel polymer, wherein the anionic surfactant is dioctyl sodium sulfosuccinate,

2) drying the hydrogel polymer,

3) pulverizing the dried polymer, and

4) performing surface cros slinking reaction of the pulverized polymer;

wherein the super absorbent polymer has an average particle size of 300 μm to 600 μm, CRC of 28 g/g to 35 g/g, AUL (0.9 psi) of 18 g/g to 25 g/g, 5-min Gel-Vacuum AUL of 18 g/g to 25 g/g, and a vortex time of 5 seconds to 50 seconds,

wherein

the WAUL is measured according to the following Equation 1:

WAUL(g/g)=[W 2 (g)−W 1 (g)]/ W 0 (g)   [Equation 1]

in Equation 1,

W 0 (g) is an initial weight(g) of the super absorbent polymer,

W 1 (g) is the total sum of a weight of the super absorbent polymer and a weight of the device capable of providing a load to the super absorbent polymer,

W 2 (g) is the total sum of a weight of the super absorbent polymer and a weight of the device capable of providing a load to the super absorbent polymer, after absorbing a physiological saline solution below 15 cm from the super absorbent polymer under a load (0.7 psi) for 10 minutes,

wherein the vortex time means the amount of time required until the vortex disappears after adding 2 g of a super absorbent polymer to 50 mL of physiological saline solution and then stirring the mixture at 600 rpm,

wherein

the 5-min Gel-Vacuum AUL is measured according to the following Equation 5:

5-min Gel-Vacuum AUL(g/g)=[W 8 (g)−W 7 (g)]/ W 0 (g)   [Equation 5]

in Equation 5,

W 0 (g) is an initial weight(g) of the super absorbent polymer,

W 7 (g) is the total sum of the weight of the super absorbent polymer and the weight of the device capable of providing a load to the super absorbent polymer, and

W 8 (g) is the total sum of the weight of the super absorbent polymer and the weight of the device capable of providing a load to the super absorbent polymer, after absorbing a physiological saline solution to the super absorbent polymer under a load (0.3 psi) for 5 minutes and removing the remaining liquid with a vacuum device.

3. The super absorbent polymer according to claim 1 ,

wherein the super absorbent polymer has a rewetting amount of 0.05 g/g to 1 g/g, which is measured according to the following Equation 6:

Rewetting Amount (g/g)=[W 10 (g)−W 9 (g)]/W 0 (g)   [Equation 6]

in Equation 6,

W 0 (g) is an initial weight(g) of the super absorbent polymer,

W 9 (g) is an initial weight(g) of the second filter paper,

W 10 (g) is a weight(g) of the second filter paper that has absorbed a liquid leaking out from the super absorbent polymer swelled for 2 minutes under a load (0.7 psi), after the super absorbent polymers have absorbed 25 times their weight in a physiological saline solution for a sufficient time under no load condition.

4. A method of preparing a super absorbent polymer according to claim 1 :

1) performing thermal polymerization or photopolymerization of a monomer composition comprising a water-soluble ethylene-based unsaturated monomer having an acidic group in which at least a part thereof is neutralized, a carbonate forming agent, an anionic surfactant and a polymerization initiator to form a hydrogel polymer, wherein the anionic surfactant is dioctyl sodium sulfosuccinate,

2) drying the hydrogel polymer,

3) pulverizing the dried polymer, and

4) performing surface cros slinking reaction of the pulverized polymer.

5. The method of preparing a super absorbent polymer according to claim 4 ,

wherein the carbonate foaming agent is at least one selected from the group consisting of sodium carbonate, sodium hydrogen carbonate, magnesium carbonate, calcium carbonate, potassium carbonate, and potassium hydrogen carbonate.

6. The method of preparing a super absorbent polymer according to claim 4 ,

wherein the carbonate foaming agent is used in an amount of 0.01 to 0.1% by weight relative to the water-soluble ethylene-based unsaturated monomer.

7. The method of preparing a super absorbent polymer according to claim 4 ,

wherein the anionic surfactant is a carboxylic acid salt, a sulfonic acid salt, or a phosphate, containing 6 to 18 carbon atoms.

8. The method of preparing a super absorbent polymer according to claim 4 ,

wherein the anionic surfactant is used in an amount of 0.05 to 3% by weight relative to the water-soluble ethylene-based unsaturated monomer.

9. The method of preparing a super absorbent polymer according to claim 4 ,

wherein the surface crosslinking reaction is carried out by using at least one surface cros slinking agent selected from the group consisting of ethylene glycol diglycidyl ether, polyethylene glycol diglycidyl ether, glycerol polyglycidyl ether, propylene glycol diglycidyl ether, polypropylene glycol diglycidyl ether, ethylene carbonate, ethylene glycol, diethylene glycol, propylene glycol, triethylene glycol, tetraethylene glycol, propanediol, dipropylene glycol, polypropylene glycol, glycerin, polyglycerin, butanediol, heptanediol, hexanediol, trimethylolpropane, pentaerythritol, sorbitol, calcium hydroxide, magnesium hydroxide, aluminum hydroxide, iron hydroxide, calcium chloride, magnesium chloride, aluminum chloride and iron chloride.

10. The method of preparing a super absorbent polymer according to claim 4 ,

wherein the surface crosslinking reaction is carried out by further using silica.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 17, 2021
From: JANG, TAE HWAN
To: LG CHEM, LTD.
Reel/Frame 055297/0528 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 11, 2017
From: LEE, SANG GI; NAM, HYE MI; HWANG, MIN HO; LEE, SOO JIN
To: LG CHEM, LTD.
Reel/Frame 043546/0097 →
Priority Claims (2)
KR 10-2016-0022849 · Feb 25, 2016 · national
KR 10-2016-0103023 · Aug 12, 2016 · national
Continuity (1)
Related Publication 20180050321A1 · Feb 22, 2018