IP Library Granted Patent US 6,987,151
Granted Patent B2
US 6,987,151 · App. 10/486,777 · Granted Jan 17, 2006

Continuous polymerization process for the manufacture of superabsorbent polymers

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Quick Facts
Patent No.
US 6,987,151
App. No.
10/486,777
Granted
Jan 17, 2006
Kind
B2
Abstract

A continuous process for producing water-insoluble, water-swellable polymers comprises subjecting a monomer and initiator to polymerization conditions in a reactor system having at least 3 zones.

Claims (36)

1. A process for the preparation of water-absorbent, water-insoluble polymers, the process comprising:

continuously polymerizing a monomer in a reactor system comprising at least 3 zones;

wherein the first zone is an initiation zone to which there is continuously fed a monomer, an initiator and water under conditions such that the polymerization of the monomer is initiated;

wherein the second zone is a gel-phase zone;

wherein the third zone is a granulation zone;

wherein the reactor system has at least two rotating shafts in each of the second and third zones;

wherein the peak temperature in the second and third zones is from 50° C. to 100° C.; and

wherein at least a portion of the water fed to the first zone optionally is in the form of steam.

2. The process of claim 1 wherein the monomer comprises from 25–50 weight percent partially neutralized acrylic acid having a degree of neutralization in the range of 50–80 mole percent.

3. The process of claim 1 wherein the temperature of the initiation zone is from 40° C. to 85° C.

4. The process of claim 1 wherein the peak-temperature in the reactor is maintained in a temperature range of 60 to 85° C. by reducing the pressure, evaporating water, and condensing the water under reflux conditions such that the condensate is sent back to the third zone.

5. The process of claim 1 wherein the combined average residence time in the three zones is from 4 to 80 minutes.

6. The process of claim 3 wherein 50 to 90 percent of the total energy input into the first zone is supplied by the heat of the polymerization reaction, 10 to 40 percent is supplied by injected steam, and 0 to 15 percent is supplied by heating the walls of the reaction vessel.

7. The process of claim 1 wherein the polymer discharged from the reactor has a weight average particle size of from 0.2 to 50 mm.

8. The process of claim 1 wherein the feed rate to the first zone is from 0.5 to 5 kg per liter of reactor volume per hour.

9. The process of claim 1 wherein the feed rate to the first zone is from 1.3 to 3.3 kg per liter of reactor volume per hour.

10. The process of claim 1 wherein a persulfate is introduced into the third zone, the discharge stream, or both.

11. The process of claim 1 wherein the monomer is in an aqueous mixture, and wherein the mixture is deoxygenated by countercurrent flow an inert gas prior to being fed to the first zone.

12. The process of claim 1 wherein the combined residence time in the three zones is from 7 to 20 minutes.

13. The process of claim 1 wherein the three zones are contained in one reactor vessel.

14. The process of claim 1 wherein at least the second and third zone are contained in one reactor vessel.

15. The process of claim 1 wherein the first zone is in a vessel separate from the second and third zones.

16. The process of claim 1 wherein the monomer concentration in the feed to the first zone is at least 45 weight percent based on the weight of the feed.

17. The process of claim 1 wherein the wherein at least 2 of the shafts in the reactor system have overlapping radii and rotate in opposite directions.

18. The process of claim 17 wherein at least 2 shafts rotate at different speeds.

19. The process of claim 1 wherein the feed to the first zone comprises a solution of monomer, initiator, and water.

20. The process of claim 1 wherein the monomer comprises acrylic acid.

21. The process of claim 1 wherein polymer fines are recycled.

22. A process for the preparation of water-absorbent, water-insoluble polymers, the process comprising:

continuously polymerizing a monomer in a reactor system comprising at least 3 zones;

wherein the first zone is an initiation zone to which there is continuously fed a monomer, an initiator and water under conditions such that the polymerization of the monomer is initiated;

wherein the second zone is a highly viscous gel-phase zone;

wherein the third zone is a granulation zone;

wherein the reactor system has at least two rotating shafts in each of the second and third zones;

wherein the pressure in at least the second and third zones of the reactor system is subatmospheric; and

wherein at least a portion of the water fed to the first zone optionally is in the form of steam.

Assignments (6)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 20, 2021
From: EVONIK OPERATIONS GMBH
To: EVONIK SUPERABSORBER GMBH
Reel/Frame 057880/0801 →
CHANGE OF NAME Recorded Dec 9, 2019
From: EVONIK DEGUSSA GMBH
To: EVONIK OPERATIONS GMBH
Reel/Frame 051228/0488 →
CHANGE OF NAME Recorded May 15, 2013
From: STOCKHAUSEN GMBH
To: EVONIK STOCKHAUSEN GMBH
Reel/Frame 030416/0806 →
MERGER Recorded May 15, 2013
From: EVONIK STOCKHAUSEN GMBH
To: EVONIK DEGUSSA GMBH
Reel/Frame 030417/0037 →
CORRECTIVE ASSIGNMENT TO CORRECT THE NAME OF THE ASSIGNEE AND ADD MISSING PAGE TO THE DOCUMENT PREVIOUSLY RECORDED ON REEL 018099 FRAME 0354. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Oct 2, 2006
From: THE DOW CHEMICAL COMPANY; DOW GLOBAL TECHNOLOGIES INC.
To: STOCKHAUSEN GMBH
Reel/Frame 018323/0683 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 14, 2006
From: THE DOW CHEMICAL COMPANY; DOW GLOBAL TECHNOLOGIES INC.
To: STOCKHAUSE GMBH
Reel/Frame 018099/0354 →