Polyacrylic acid (salt)-based water absorbent resin powder and method for producing the same

Patent metadata

Field	Value
Publication number	US-9044525-B2
Application number	US-201214129792-A
Country	US
Kind code	B2
Filing date	Jun 29, 2012
Priority date	Jun 29, 2011
Publication date	Jun 2, 2015
Grant date	Jun 2, 2015

Abstract

Provided is a water absorbent resin having excellent liquid permeability, water absorbent speed, anti-impact stability, and weather resistance. Provided is a polyacrylic acid (salt)-based water absorbent resin powder in which the water absorption capacity without load (CRC) is 30 to 45 [g/g], the water absorption capacity under load (AAP 0.3) is 20 to 35 [g/g], the water absorption capacity under load (AAP 0.7) is 10 to 28 [g/g], and the weight average particle diameter (D50) is 300 to 500 μm, characterized by including p-methoxyphenol; having a degradable soluble component (0.05% L-A (saline) for 2 hours/60° C., one hour extraction rinse/room temperature) of 40% by weight or less; and having a internal gas bubbles ratio of 0.1 to 2.5%, as specified by the following equation.

(Internal gas bubbles ratio)[%]={(True density)−(Apparent density)}/(True density)×100

First claim

The invention claimed is:

1. A polyacrylic acid (salt)-based water absorbent resin powder in which the water absorption capacity without load (CRC) is 30 to 45 [g/g], the water absorption capacity under load (AAP 0.3) is 20 to 35 [g/g], the water absorption capacity under load (AAP 0.7) is 10 to 28 [g/g], and the weight average particle diameter (D50) is 300 to 500 μm, wherein the water absorbent resin powder comprises p-methoxyphenol, has a degradable soluble component (0.05% L-A (saline) for 2 hours/60° C., one hour extraction rinse/room temperature) of 40% by weight or less, and an internal gas bubbles ratio of 0.1 to 2.5%, as specified by the following equation
(Internal gas bubbles ratio)[%]={(True density)−(Apparent density)}/(True density)×100.

2. The water absorbent resin powder according to claim 1 , further comprising water-insoluble inorganic microparticles, a water soluble polyvalent metal salt (with the proviso that, iron salt is excluded), an inorganic or organic reducing agent, or a combination thereof.

3. The water absorbent resin powder according to claim 1 , further comprising a metal chelating agent.

4. The water absorbent resin powder according to claim 1 , wherein content of an iron ion is 0.1 to 3 ppm.

5. The water absorbent resin powder according to claim 1 , wherein content of p-methoxyphenol is 5 to 50 ppm.

6. The water absorbent resin powder according to claim 1 , wherein residual monomers are 500 ppm or less.

7. The water absorbent resin powder according to claim 1 , wherein the degradable soluble component (0.05% L-A (saline) for 2 hours/60° C., one hour extraction rinse/room temperature) is 20% by weight or less.

8. The water absorbent resin powder according to claim 1 , wherein powder flowability after moisture absorption test is 70% by weight or more.

9. The water absorbent resin powder according to claim 3 , wherein the metal chelating agent is comprised at 0.001 to 2% by weight relative to the water absorbent resin powder.

10. The water absorbent resin powder according to claim 1 , wherein an increase amount of degradable soluble component (defined as degradable soluble component (%)−16 hour soluble component (%)) is 20% by weight or less.

11. The water absorbent resin powder according to claim 3 , wherein the chelating agent is a water soluble non-polymeric chelating agent selected from amino polyvalent carboxylic acid and amino polyvalent phosphoric acid.

12. A method for producing a water absorbent resin powder which has internal gas bubbles ratio of 0.1 to 2.5% as specified by the following equation, the method comprising:
a polymerization step wherein performing foaming polymerization or boiling polymerization of an aqueous monomer solution containing p-methoxyphenol and also acrylic acid as a main component;
a gel-crushing step wherein kneading and grain refining a water-containing gel-like polymer having gas bubbles obtained from the polymerization;
a drying step wherein heating and drying it at 150 to 250° C. after gel-crushing,
a pulverizing and classification step wherein pulverizing and classifying a dried product to have a weight average particle diameter of 300 to 500 μm; and
surface crosslinking the pulverized and classified product with internal gas bubbles ratio 0.1 to 2.5% to have the water absorption capacity without load (CRC) of 30 to 45 [g/g], the water absorption capacity under load (AAP 0.3) of 20 to 35 [g/g], and the water absorption capacity under load (AAP 0.7) of 10 to 28 [g/g]
(Internal gas bubbles ratio)[%]={(True density)−(Apparent density)}/(True density)×100.

13. A method for producing a water absorbent resin powder which has internal gas bubbles ratio of 0.1 to 2.5% as specified by the following equation, the method comprising steps of:
performing foaming polymerization or boiling polymerization of an aqueous monomer solution containing p-methoxyphenol and also acrylic acid as a main component;
adding a chelating agent during the polymerization or after the polymerization step; and
surface crosslinking a water absorbent resin containing p-methoxyphenol and having internal gas bubbles ratio of 0.1 to 2.5% to have the water absorption capacity without load (CRC) of 30 to 45 [g/g], the water absorption capacity under load (AAP 0.3) of 20 to 35 [g/g] and the water absorption capacity under load (AAP 0.7) of 10 to 28 [g/g]
(Internal gas bubbles ratio)[%]={(True density)−(Apparent density)}/(True density)×100.

14. The method according to claim 12 , wherein, for the gel-crushing step, the water-containing gel-like crosslinked polymer with resin solid content of 10 to 80% by weight is subjected to gel-crushing which satisfies at least one of the following (1) to (4):
(1) the gel-crushing is carried out with gel grinding energy (GGE) of 18 to 60 [J/g];
(2) the gel-crushing is carried out with gel grinding energy (2) (GGE (2)) of 9 to 40 [J/g];
(3) the weight average molecular weight of water soluble component of the water-containing gel-like crosslinked polymer is increased by 10,000 to 500,000 [Da]; and
(4) the gel-crushing is carried out until the water-containing gel-like crosslinked polymer has a weight average particle diameter (D50) of 350 to 2,000 μm, and logarithmic standard deviation (σζ) of particle size distribution of 0.2 to 1.0.

15. The method according to claim 12 , wherein water-insoluble inorganic microparticles, a water soluble polyvalent metal salt (with the proviso that, iron salt is excluded), an inorganic or organic reducing agent, or a combination thereof are additionally mixed after the drying step.

16. The method according to claim 12 , wherein a metal chelating agent is additionally mixed after the polymerization step.

17. The method according to claim 12 , wherein content of iron ion in monomer is 0.1 to 3 ppm.

18. The method according to claim 12 , wherein content of p-methoxyphenol in monomer is 5 to 200 ppm (relative to monomer solid content).

19. The method according to claim 12 , further comprising a step of neutralizing whole or part of acrylic acid with a base having a Fe content of 0 to 7 ppm before the polymerization step,
wherein the polymerization step is a step of performing, under condition including maximum temperature of 130° C. or less and polymerization time of between 0.5 minutes to 3 hours, aqueous solution polymerization or reverse-phase suspension polymerization of an aqueous monomer solution with monomer concentration of 30 to 55% by weight, in which acrylic acid (salt) is contained at 90 to 100% by mol in the monomer, by using 0.001 to 1% by mol of a polymerization initiator (relative to the monomer),
the drying step is a step of drying the water-containing gel-like crosslinked polymer, which has been obtained in particle form by polymerization, to have a moisture content of 20% by weight or less with drying temperature of 100 to 250° C. and drying time of 10 to 120 minutes, and
the surface crosslinking is a step of mixing 0.001 to 10 parts by weight of a surface crosslinking agent relative to 100 parts by weight of the water absorbent resin powder after completion of the pulverizing and classification step and performing a heating treatment for 1 minute to 2 hours at 70 to 300° C.

20. An absorbent article comprising the water absorbent resin powder defined claim 1 , wherein core concentration as defined by weight ratio of the water absorbent resin relative to total weight of the water absorbent resin and a hydrophilic fiber material is 30 to 100% by weight.

Assignees

• Torii Kazushi
• Nakatsuru Reiko
• Nakashima Yasuhisa
• Wada Katsuyuki
• Ishizaki Kunihiko
• Nippon Catalytic Chem Ind

Inventors

• Torii Kazushi
• Nakatsuru Reiko
• Nakashima Yasuhisa
• Wada Katsuyuki
• Ishizaki Kunihiko

Classifications

• C08K5/175

  containing COOH-groups; Esters or salts thereof · CPC title

• Y10T428/2982

  Particulate matter [e.g., sphere, flake, etc.] · CPC title

• A61L15/60

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

• C08K5/0091

  Complexes with metal-heteroatom-bonds · CPC title

• C08F220/06

  Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof · CPC title