IP Library › Granted Patent US 9,598,521
Granted Patent B2
US 9,598,521 · App. 14/422,975 · Granted Mar 21, 2017

Method for manufacturing hydrophilic polymer particle

Inventors: Kazuki Naito (Wakayama, JP); Shuichi Kaku (Wakayama, JP)
Assignee: KAO CORPORATION
C08F220/56A61K8/0241A61K8/8158A61Q5/02A61Q19/10C08F2/32C08F220/54
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Quick Facts
Patent No.
US 9,598,521
App. No.
14/422,975
Granted
Mar 21, 2017
Kind
B2
Abstract

In a method for producing hydrophilic polymer particles, a dispersion in which an aqueous-phase component including hydrophilic monomers and a polymerization initiator is dispersed in an oil-phase component including a hydrophobic solvent is prepared. Thereafter, the hydrophilic monomers are polymerized in the aqueous phase by supplying oxygen to a reaction vessel and, while oxygen is being supplied, heating the dispersion having a reduced dissolved oxygen concentration in the reaction vessel so that the temperature of the dispersion is increases. The time from the start of reduction of the dissolved oxygen concentration of the dispersion to the start of the heating is 0.1 hour or more and 3.5 hours or less. The amount of oxygen supplied to the reaction vessel is greater than or equal to 0.02 volume %/h and less than or equal to 0.9 volume %/h with respect to the volume of the dispersion under standard conditions.

Claims (32)

1. A method for producing hydrophilic polymer particles, the method comprising:

step 1: preparing a dispersion in which an aqueous-phase component including hydrophilic monomers and a polymerization initiator is dispersed in an oil-phase component including a hydrophobic solvent having a solubility of 1 mass % or less in water at 25° C.;

step 2: reducing a dissolved oxygen concentration of the dispersion prepared in step 1; and

step 3: polymerizing the hydrophilic monomers in the aqueous phase by supplying oxygen to a reaction vessel and, while oxygen is being supplied, heating the dispersion whose dissolved oxygen concentration was reduced in step 2 in the reaction vessel so that a temperature of the dispersion increases, wherein

a time from a start of reduction of the dissolved oxygen concentration of the dispersion in step 2 to a start of heating of the dispersion in step 3 is greater than or equal to 0.1 hour and less than or equal to 3.5 hours, and

an amount of oxygen supplied to the reaction vessel in step 3 is greater than or equal to 0.02 volume % per hour and less than or equal to 0.9 volume % per hour with respect to a volume of the dispersion, under standard conditions of a temperature of 25° C. and an absolute pressure of 101.3 kPa.

2. The method of claim 1 , wherein

in step 3, a rate of temperature increase of the dispersion is greater than or equal to 5° C. per hour and less than or equal to 100° C. per hour.

3. The method of claim 1 , wherein

in step 2, a reduction ratio of the dissolved oxygen concentration of the dispersion is 40% or more, relative to a dissolved oxygen concentration of the dispersion at the start of reduction of the dissolved oxygen concentration.

4. The method of claim 1 , wherein

in step 2, the dissolved oxygen concentration of the dispersion is reduced by reducing an internal pressure of the reaction vessel storing the dispersion prepared in step 1 and then introducing an inert gas into the reaction vessel so that the internal pressure returns to a normal pressure.

5. The method of claim 1 , wherein

in step 1, the dispersion is prepared by dispersing the aqueous-phase component including the polymerization initiator in advance together with hydrophilic monomers in the oil-phase component including the hydrophobic solvent.

6. The method of claim 1 , wherein

in step 2, the temperature of the dispersion is greater than or equal to 0° C. and less than or equal to 50° C.

7. The method of claim 1 , wherein

in step 1, the oil-phase component includes a dispersing agent.

8. The method of claim 1 , wherein

in step 3, oxygen is supplied by using an oxygen-containing gas.

9. The method of claim 8 , wherein

an oxygen content of the oxygen-containing gas used in step 3 is greater than or equal to 1 volume % and less than or equal to 50 volume %, relative to the oxygen-containing gas.

10. The method of claim 1 , wherein

the hydrophilic polymer includes copolymer of vinyl monomers having cationic groups and/or a salt thereof, vinyl monomers having hydrophilic nonionic groups, and crosslinkable vinyl monomers having at least two reactive unsaturated groups in a molecule.

11. The method of claim 1 , further comprising

step 4: reducing a content of water by dehydrating the dispersion of hydrophilic polymer particles obtained in step 3.

12. The method of claim 11 , further comprising

step 5: substituting, by a substitution solvent, the hydrophobic solvent included in the dispersion of hydrophilic polymer particles dehydrated in step 4.

13. The method of claim 1 , wherein

the amount of oxygen supplied to the reaction vessel in step 3 is greater than or equal to 0.1 volume % per hour and less than or equal to 0.7 volume % per hour with respect to the volume of the dispersion, under standard conditions of a temperature of 25° C. and an absolute pressure of 101.3 kPa.

14. The method of claim 1 , wherein

the time from the start of reduction of the dissolved oxygen concentration of the dispersion in step 2 to the start of heating of the dispersion in step 3 is greater than or equal to 0.3 hour and less than or equal to 2.0 hours.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 10, 2015
From: NAITO, KAZUKI; KAKU, SHUICHI
To: KAO CORPORATION
Reel/Frame 035128/0208 →
Priority Claims (1)
JP 2012-183137 · Aug 22, 2012 · national
Continuity (1)
Related Publication 20150218297A1 · Aug 6, 2015