Patent US4525527A successfully refreshed from Google Patents.
US4525527A
Expired / Lapsed
US
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Production process for highly water absorbable polymer
Assignee: BASF SE
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Filing: 1983-01-21
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Granted: 1985-06-25
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Expires: 2003-01-21
Abstract
Abstract Disclosed is a process for preparing water absorbing, cross-linked acrylate resins by aqueous polymerization of (A) acrylic acid neutralized 70 to 100 mole percent for example with ammonia, and/or caustic alkali and/or an amine; with (B) acrylamide in a mole ratio of 70 to 100 mole percent (A) to 30:0 mole percent (B); and (C) a water miscible or a water soluble polyvinyl monomer in an amount of 0.001 to 0.3 weight percent based on the total weight of (A) and (B). In accordance with one embodiment of the invention, the concentration of monomers (A) plus (B) should be at least 70 percent by weight of the polymerization mixture of (A) plus (B) plus (C) to achieve a substantially dry polymer (less than 15 weight percent water) when polymerization is completed by utilizing the exothermic heat of polymerization and cross-linking to drive off water without the need for additional heating to obtain a dry solid. The addition of polystyrene and/or methylcellulose substantially increases the water absorbing capacity of these polymers.
Inventors
- 👤 Hisao Takeda
- 👤 Yasunori Taniguchi
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 18:47
CPC Classifications
C; C08; C08F; C08F220/00; C08F220/02; C08F220/04; C08F220/06; A; A61; A61L; A61L15/00; A61L15/16; A61L15/42; A61L15/60; Y; Y10; Y10S; Y10S521/00; Y10S521/905; Y10T; Y10T428/00; Y10T428/31504; Y10T428/31855
Claims Analysis
Total Claims: 30
Claim 1
Independent Claim
157 words
A method of manufacturing a composition comprising mixing a monomer solution of (A) acrylic acid, neutralized 70 to 100 mole percent, (B) acrylamide in a mole ratio of (A):(B) in the range of 70:30 to 90:10; (C) a water soluble or water miscible polyvinyl monomer cross-linking agent in an amount of 0.001 to 0.3 percent by weight of (A) plus (B); and water to form a mixed monomer solution, wherein the monomers of the mixed monomer solution consist essentially of (A), (B) and (C) and the monomer concentration is at least 70 percent by weight of the monomer solution prior to polymerization initiation; and initiating polymerization of monomers (A) and (B) such that during polymerization, the exothermic heat of reaction is substantially the only heat energy used to accomplish polymerization, cross-linking and to drive off sufficient water to form a water absorbing cross-linked polyacrylate resin composition having a water content of 15 percent by weight or less.
Claim 2
Independent Claim
157 words
A method of manufacturing a composition comprising mixing a monomer solution of (A) acrylic acid, neutralized 70 to 100 mole percent, (B) acrylamide in a mole ratio of (A):(B) in the range of 70:30 to 90:10; (C) a water soluble or water miscible polyvinyl monomer cross-linking agent in an amount of 0.001 to 0.3 percent by weight of (A) plus (B); and water to form a mixed monomer solution, wherein the monomers of the mixed monomer solution consist essentially of (A), (B) and (C) and the monomer concentration is at least 70 percent by weight of the monomer solution prior to polymerization initiation; and initiating polymerization of monomers (A) and (B) such that during polymerization, the exothermic heat of reaction is substantially the only heat energy used to accomplish polymerization, cross-linking and to drive off sufficient water to form a water absorbing cross-linked polyacrylate resin composition having a water content of 15 percent by weight or less.
Claim 3
Independent Claim
169 words
A method of manufacturing a composition comprising mixing a monomer solution of (A) acrylic acid, neutralized 70 to 100 mole percent, (B) acrylamide in a mole ratio of (A):(B) in the range of 70:30 to 100:0; (C) a water soluble or water miscible polyvinyl monomer cross-linking agent in an amount of 0.001 to 0.3 percent by weight of (A) plus (B); and water to form a mixed monomer solution, wherein the monomers of the mixed monomer solution consist essentially of (A), (B) and (C) and the monomer concentration is at least 70 percent by weight of the monomer solution prior to polymerization initiation; and initiating polymerization of monomers (A) and (B) such that during polymerization, the exothermic heat of reaction is substantially the only heat energy used to accomplish polymerization, cross-linking and to drive off sufficient water to form a water absorbing cross-linked polyacrylate resin composition having a water content of 15 percent by weight or less, and wherein said neutralized acrylic acid is one other than potassium acrylate.
Claim 4
Independent Claim
169 words
A method of manufacturing a composition comprising mixing a monomer solution of (A) acrylic acid, neutralized 70 to 100 mole percent, (B) acrylamide in a mole ratio of (A):(B) in the range of 70:30 to 100:0; (C) a water soluble or water miscible polyvinyl monomer cross-linking agent in an amount of 0.001 to 0.3 percent by weight of (A) plus (B); and water to form a mixed monomer solution, wherein the monomers of the mixed monomer solution consist essentially of (A), (B) and (C) and the monomer concentration is at least 70 percent by weight of the monomer solution prior to polymerization initiation; and initiating polymerization of monomers (A) and (B) such that during polymerization, the exothermic heat of reaction is substantially the only heat energy used to accomplish polymerization, cross-linking and to drive off sufficient water to form a water absorbing cross-linked polyacrylate resin composition having a water content of 15 percent by weight or less, and wherein said neutralized acrylic acid is one other than potassium acrylate.
Claim 5
Dependent Claim
20 words
The method of claim 1 wherein the monomer concentration in the mixed monomer solution is 70 to 90 weight percent.
Claim 6
Dependent Claim
20 words
The method of claim 3 wherein the monomer concentration in the mixed monomer solution is 70 to 80 weight percent.
Claim 7
Dependent Claim
36 words
The method of claim 1 wherein the polyvinyl cross-linking agent is included in the mixed monomer solution in an amount of 0.005 to 0.05 percent by weight based on the combined weight of (A) plus (B).
Claim 8
Dependent Claim
36 words
The method of claim 5 wherein the polyvinyl cross-linking agent is included in the mixed monomer solution in an amount of 0.005 to 0.02 percent by weight based on the combined weight of (A) plus (B).
Claim 9
Dependent Claim
24 words
The method of claim 1 wherein the mixed monomer solution is heated to a temperature of 25° to 85° C. prior to polymerization initiation.
Claim 10
Dependent Claim
19 words
A method of claim 1 wherein the polyvinyl monomer is selected from the group consisting of N,N'-methylenebisacrylamide and N,N'-methylenebismethacrylamide.
Claim 11
Dependent Claim
32 words
A method of claim 1 wherein the polyvinyl monomer is N,N'-methylenebisacrylamide in an amount of 0.005 to 0.02 weight percent based on the total weight of monomers in the mixed monomer solution.
Claim 12
Dependent Claim
27 words
The method of claim 1 wherein acrylic acid is neutralized with a neutralizing agent selected from ammonia, an amine, or a lithium, sodium, rubidium or cesium base.
Claim 13
Dependent Claim
24 words
The method of claim 1 wherein polymerization of said mixed monomer solution is initiated by adding a polymerization initiator to said mixed monomer solution.
Claim 14
Dependent Claim
24 words
The method of claim 11 wherein the monomer mixture has a temperature of 50° to 90° C. immediately prior to adding the polymerization initiator.
Claim 15
Dependent Claim
34 words
The method of claim 11 wherein said polymerization initiator is added in an amount of at least 0.5 percent by total weight of monomers (A) plus (B) plus (C) in the mixed monomer solution.
Claim 16
Dependent Claim
24 words
The method of claim 11 including depositing said monomer mixture including said initiator onto a support surface in sheet form for polymerization and cross-linking.
Claim 17
Independent Claim
182 words
A method of manufacturing a composition comprising mixing a monomer solution of (A) acrylic acid, neutralized 70 to 100 mole percent, (B) acrylamide in a mole ratio of acrylic acid:acrylamide in the range of 70:30 to 90:10; (C) a water soluble or water miscible polyvinyl monomer cross-linking agent in an amount of 0.001 to 0.3 percent by weight of (A) plus (B) and water to form a mixed monomer solution wherein the monomer concentration of (A) plus (B) is at least 70 percent by weight of (A) plus (B) plus (C) and wherein the reactant monomers (A), (B) and (C) of the mixed monomer solution comprise at least 70% by weight of the mixed monomer solution; initiating polymerization of monomers (A) and (B) and polymerizing said monomers without substantial external heating such that during polymerization, the exothermic heat of reaction is substantially the only heat energy used to accomplish polymerization, cross-linking and to drive off sufficient water to form a water absorbing cross-linked polyacrylate resin composition having a water content of 15 percent or less as recovered from the mixed monomer solution.
Claim 18
Independent Claim
182 words
A method of manufacturing a composition comprising mixing a monomer solution of (A) acrylic acid, neutralized 70 to 100 mole percent, (B) acrylamide in a mole ratio of acrylic acid:acrylamide in the range of 70:30 to 90:10; (C) a water soluble or water miscible polyvinyl monomer cross-linking agent in an amount of 0.001 to 0.3 percent by weight of (A) plus (B) and water to form a mixed monomer solution wherein the monomer concentration of (A) plus (B) is at least 70 percent by weight of (A) plus (B) plus (C) and wherein the reactant monomers (A), (B) and (C) of the mixed monomer solution comprise at least 70% by weight of the mixed monomer solution; initiating polymerization of monomers (A) and (B) and polymerizing said monomers without substantial external heating such that during polymerization, the exothermic heat of reaction is substantially the only heat energy used to accomplish polymerization, cross-linking and to drive off sufficient water to form a water absorbing cross-linked polyacrylate resin composition having a water content of 15 percent or less as recovered from the mixed monomer solution.
Claim 19
Dependent Claim
20 words
The method of claim 15 wherein the monomer concentration in the mixed monomer solution is 70 to 90 weight percent.
Claim 20
Dependent Claim
20 words
The method of claim 16 wherein the monomer concentration in the mixed monomer solution is 70 to 80 weight percent.
Claim 21
Dependent Claim
36 words
The method of claim 15 wherein the polyvinyl cross-linking agent is included in the mixed monomer solution in an amount of 0.005 to 0.05 percent by weight based on the combined weight of (A) plus (B).
Claim 22
Dependent Claim
36 words
The method of claim 18 wherein the polyvinyl cross-linking agent is included in the mixed monomer solution in an amount of 0.005 to 0.02 percent by weight based on the combined weight of (A) plus (B).
Claim 23
Dependent Claim
24 words
The method of claim 15 wherein the mixed monomer solution is heated to a temperature of 25° to 85° C. prior to polymerization initiation.
Claim 24
Dependent Claim
19 words
The method of claim 15 wherein the polyvinyl monomer is selected from the group consisting of N,N'-methylenebisacrylamide and N,N'-methylenebismethacrylamide.
Claim 25
Dependent Claim
32 words
The method of claim 15 wherein the polyvinyl monomer is N,N'-methylenebisacrylamide in an amount of 0.005 to 0.02 weight percent based on the total weight of monomers in the mixed monomer solution.
Claim 26
Dependent Claim
31 words
The method of claim 15 wherein acrylic acid is neutralized with a neutralized agent selected from the group consisting of ammonia, an amine, and lithium, sodium, rubidium or a cesium base.
Claim 27
Dependent Claim
24 words
The method of claim 15 wherein polymerization of said mixed monomer solution is initiated by adding a polymerization initiator to said mixed monomer solution.
Claim 28
Dependent Claim
24 words
The method of claim 24 wherein the monomer mixture has a temperature of 50° to 90° C. immediately prior to adding the polymerization initiator.
Claim 29
Dependent Claim
34 words
The method of claim 24 wherein said polymerization initiator is added in an amount of at least 0.5 percent by total weight of monomers (A) plus (B) plus (C) in the mixed monomer solution.
Claim 30
Dependent Claim
36 words
The method of claim 20 wherein the water content of said cross-linked polyacrylate resin is not greater than about 10% by weight as recovered from the mixed monomer solution after polymerization, without an additional drying step.
References Cited (Backward Citations)
GB869333A
Cited
US3251194A
Cited
US4058124A
Cited
US4059552A
Cited
US4057521A
Cited
US4459396A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1988-06-24 | 1988-12-24 | 1989-06-25 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-06-24 | 1992-12-24 | 1993-06-25 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-06-24 | 1996-12-24 | 1997-06-25 | $7700.00 | Window Closed / Lapsed |