IP Library Granted Patent US 8,357,766
Granted Patent B2
US 8,357,766 · App. 12/575,071 · Granted Jan 22, 2013

Continuous process for the production of a superabsorbent polymer

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Quick Facts
Patent No.
US 8,357,766
App. No.
12/575,071
Granted
Jan 22, 2013
Kind
B2
Abstract

The present invention relates to a continuous process for the production of a superabsorbent polymer comprising providing an acidic liquid aqueous monomer mixture containing dissolved oxygen; continuously feeding the aqueous monomer mixture to a reactor; introducing a source of carbonate or hydrogen carbonate into the aqueous monomer mixture prior to entry into the reactor thereby forming a gas phase comprising carbon dioxide and at least a part of the dissolved oxygen, the gas phase being dispersed in the liquid phase; subjecting the gas/liquid mixture to at least partial phase separation immediately prior to or after entry into the reactor and at least partially removing the separated gaseous phase; subjecting the liquid phase in the reactor to free-radical polymerization to obtain the superabsorbent polymer, and continuously removing the superabsorbent polymer from the reactor.

Claims (29)

1. A continuous process for the production of a superabsorbent polymer comprising:

(a) providing an acidic liquid aqueous monomer mixture containing dissolved oxygen, whereby the monomers are selected to provide after polymerization a superabsorbent polymer,

(b) continuously feeding said aqueous monomer mixture to a reactor,

(c) introducing a source of carbonate or hydrogen carbonate into said aqueous monomer mixture prior to entry into the reactor thereby forming a dispersed gas phase comprising carbon dioxide and at least a part of said dissolved oxygen, said dispersed gas phase being dispersed in said aqueous monomer mixture wherein the source of carbonate or hydrogen carbonate is introduced in an amount to provide about 1 to about 15% of the total neutralization of the acidic functionality of the resultant superabsorbent polymer wherein the total neutralization is between about 50% and about 85%,

(d) at least partially separating said dispersed gas phase from the aqueous monomer mixture to create a separated gas phase and a liquid phase immediately prior to or after entry into the reactor and at least partially removing the separated gas phase,

(e) subjecting the liquid phase in the reactor to free-radical polymerization to obtain the superabsorbent polymer, and

(f) continuously removing the superabsorbent polymer from the reactor.

2. The process of claim 1 , wherein the aqueous monomer mixture is fed to the reactor via a transfer line and wherein the pressure difference between said transfer line and reactor is about 0.5 to about 5 bar.

3. The process according to claim 1 , wherein the free-radical polymerization is initiated by a redox initiator and wherein the oxidative component of the redox initiator is added to the monomer mixture in step (a) and the reductive component of the redox initiator is added to the monomer mixture after step (c) prior to the monomer mixture entry into the reactor or the reductive component of the redox initiator is added directly to the reactor at a position in proximity to the entry point of the monomer mixture.

4. The process according to claim 1 , wherein the reactor encompasses at least three zones, wherein the first zone is an initiation zone, the second zone is a gel-phase zone and the third zone is a granulation zone.

5. The process according to claim 4 , wherein said aqueous monomer mixture is fed to said initiation zone.

6. The process according to claim 1 , wherein the reactor is selected from continuous kneaders and extruders or belt reactors.

7. The process according to claim 1 , wherein no additional inert gas is introduced at any point of the process.

8. The process according to claim 1 , wherein fines of a superabsorbent polymer having a particle size of less than about 300 μm are added to the aqueous monomer mixture prior to the introduction of the source of carbonate or hydrogen carbonate.

9. The process according to claim 1 , wherein the aqueous monomer mixture comprises at least one ethylenically unsaturated acid and at least one monomer bearing at least two ethylenically unsaturated groups.

10. The process according to claim 9 , wherein the at least one ethylenically unsaturated acid is at least partially neutralized.

11. The process according to claim 1 , wherein at least one carbon dioxide containing off-gas stream withdrawn from the reactor is subjected to scrubbing with a basic aqueous solution in a scrubber prior to venting thereby forming a carbonate or hydrogen carbonate containing aqueous scrubber solution.

12. The process according to claim 1 , wherein said source of carbonate or hydrogen carbonate comprises an aqueous solution of any one of an alkali metal carbonate, hydrogen carbonate, or mixtures thereof.

13. The process according to claim 12 , wherein said source of carbonate or hydrogen carbonate further comprises said aqueous scrubber solution produced in by subjecting the carbon dioxide containing off-gas stream withdrawn from the reactor to scrubbing with a basic aqueous solution in a scrubber prior to venting thereby forming a carbonate or hydrogen carbonate containing aqueous scrubber solution.

14. The process of claim 11 , wherein the source of carbonate or hydrogen carbonate is at least a part of said carbonate or hydrogen carbonate containing aqueous scrubber solution.

15. The process according to claim 1 , further comprising:

(g) withdrawing at least one carbon dioxide containing off-gas stream from the reactor,

(h) subjecting said carbon dioxide containing off-gas stream to scrubbing with a basic aqueous solution in a scrubber prior to venting thereby forming a carbonate or hydrogen carbonate containing aqueous scrubber solution,

(i) drying the superabsorbent polymer,

(j) grinding and classifying the dried superabsorbent polymer thereby removing fines having a particle size of less than about 300 μm, and

(k) recycling said fines to the monomer mixture prior to the introduction of the source of carbonate or hydrogen carbonate, wherein at least a part of the carbonate or hydrogen carbonate containing aqueous scrubber solution obtained in (h) is introduced as source of carbonate or hydrogen carbonate in (c).

16. The process according to claim 1 , wherein the resultant superabsorbent polymer is surface modified by surface post-crosslinking, heat-treatment, by additives, or any combination thereof.

17. The process according to claim 1 , wherein no additional inert gas is introduced in any of steps (a), (b), and (c).

18. The process according to claim 1 , wherein no additional inert gas is introduced into the reactor.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 21, 2021
From: EVONIK OPERATIONS GMBH
To: EVONIK SUPERABSORBER GMBH
Reel/Frame 057885/0071 →
CHANGE OF NAME Recorded Feb 3, 2020
From: EVONIK DEGUSSA GMBH
To: EVONIK OPERATIONS GMBH
Reel/Frame 051781/0167 →
MERGER Recorded May 15, 2013
From: EVONIK STOCKHAUSEN GMBH
To: EVONIK DEGUSSA GMBH
Reel/Frame 030417/0037 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 23, 2009
From: FRICKER, DANIEL; GARTNER, HERBERT; HAGER, MARC; HARREN, JORG; KOHLER, HANS-PETER; PLOCHINGER, HARALD
To: EVONIK STOCKHAUSEN GMBH
Reel/Frame 023693/0505 →