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US4600754A
Expired / Lapsed
US
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Phosphate epoxy acrylic copolymers
Assignee: Akzo Nobel Paints LLC
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Filing: 1984-05-10
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Granted: 1986-07-15
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Expires: 2004-05-10
Abstract
Abstract Water dispersed phosphated epoxy-acrylic polymers are produced by first producing an epoxy phosphate followed by in-situ polymerization of ethylenically unsaturated monomers, including carboxyl monomers, in the presence of the epoxy phosphate and utilizing at least 3% peroxide catalyst based on the weight of monomers.
Inventors
- 👤 Peter P. Winner
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 07:45
CPC Classifications
C; C08; C08F; C08F283/00; C08F283/10; C08G; C08G59/00; C08G59/14; C08G59/1405; C08G59/1422
Claims Analysis
Total Claims: 42
Claim 1
Independent Claim
189 words
In a process for polymerizing ethylenically unsaturated monomers in the presence of epoxy resin, the improvement comprising: reacting an epoxy resin having epoxide groups and having a molecular weight between about 350 and 20,000 with a source of phosphoric acid selected from 100% ortho phosphoric acid, aqueous phosphoric acid or polyphosphoric acid to coreact phosphoric acid with the epoxy resin epoxide groups to produce a phosphated epoxy polymer containing by weight between about 0.5% and 5% coreacted phosphoric acid; polymerizing ethylenically unsaturated monomers, at least one being a carboxyl functional monomer, in the presence of said phosphated epoxy polymer and in the presence of at least 3% by weight of benzoyl peroxide based on the weight of ethylenically unsaturated monomers, or under equivalent free radical initiating conditions using a peroxide initiator, at temperatures between about 80° C. and 130° C., to provide an in-situ formed polymerization product comprising on a weight basis between about 10% and 90% phosphated epoxy polymer, and the remaining being carboxyl functional addition polymer of polymerized monomers wherein the acid functionality of the addition polymer is sufficiently high to render the polymerization product water dispersible.
Claim 2
Dependent Claim
189 words
In a process for polymerizing ethylenically unsaturated monomers in the presence of epoxy resin, the improvement comprising: reacting an epoxy resin having epoxide groups and having a molecular weight between about 350 and 20,000 with a source of phosphoric acid selected from 100% ortho phosphoric acid, aqueous phosphoric acid or polyphosphoric acid to coreact phosphoric acid with the epoxy resin epoxide groups to produce a phosphated epoxy polymer containing by weight between about 0.5% and 5% coreacted phosphoric acid; polymerizing ethylenically unsaturated monomers, at least one being a carboxyl functional monomer, in the presence of said phosphated epoxy polymer and in the presence of at least 3% by weight of benzoyl peroxide based on the weight of ethylenically unsaturated monomers, or under equivalent free radical initiating conditions using a peroxide initiator, at temperatures between about 80° C. and 130° C., to provide an in-situ formed polymerization product comprising on a weight basis between about 10% and 90% phosphated epoxy polymer, and the remaining being carboxyl functional addition polymer of polymerized monomers wherein the acid functionality of the addition polymer is sufficiently high to render the polymerization product water dispersible.
Claim 3
Dependent Claim
44 words
The process in claim 1 wherein the phosphated epoxy resin is produced by reacting a non-phosphated epoxy with an epoxy phosphate containing above 5% phosphate for time sufficient whereby the resulting phosphated epoxy resin contains between 0.05% and 5% by weight coreacted phosphoric acid.
Claim 4
Dependent Claim
21 words
The process in claim 1 wherein the phosphated epoxy resin contains between about 0.1% and 3% by weight coreacted phosphoric acid.
Claim 5
Dependent Claim
25 words
The process in claim 1 wherein a base ionizing agent ionizes the acid-functional addition polymer, and said in-situ formed polymerization product is dispersed into water.
Claim 6
Dependent Claim
19 words
The process in claim 1 wherein the ethylenically unsaturated monomers include at least 20% by weight carboxyl functional monomer.
Claim 7
Dependent Claim
14 words
The process in claim 4 wherein the carboxyl functional monomer comprises an acrylic acid.
Claim 8
Dependent Claim
14 words
The process in claim 4 wherein the carboxyl functional monomer comprises a methacrylic acid.
Claim 9
Dependent Claim
17 words
The process in claim 1 wherein the ethylenically unsaturated monomers comprise styrene and acrylic or methacrylic acid.
Claim 10
Dependent Claim
21 words
The process in claim 7 wherein the ethylenically unsaturated monomers further include a lower alkyl ester of acrylic or methacrylic acid.
Claim 11
Dependent Claim
20 words
The process in claim 1 wherein the acid no. of the in-situ formed polymerization product is between 30 and 220.
Claim 12
Dependent Claim
30 words
The process in claim 1 wherein the benzoyl peroxide is at least 4% by weight based on monomer weight or under equivalent free radical initiating conditions using a peroxide initiator.
Claim 13
Dependent Claim
18 words
The process in claim 1 wherein the benzoyl peroxide level is at least 6% by weight of monomers.
Claim 14
Dependent Claim
30 words
The process in claim 1 wherein the in-situ formed polymerization product includes a graft-epoxy polymer component formed by grafting between said addition polymer component and said phosphated epoxy polymer component.
Claim 15
Dependent Claim
26 words
The process in claim 13 wherein the epoxy resin has aliphatic backbone carbons and grafting is onto the aliphatic backbone carbon atoms of the epoxy resin.
Claim 16
Dependent Claim
14 words
The process in claim 1 wherein the epoxy resin comprises bisphenol-A reacted with epichlorohydrin.
Claim 17
Dependent Claim
122 words
A phosphated epoxy-acrylic composition comprising the reaction product of: an epoxy polymer having a molecular weight between about 350 and 20,000 coreacted with ethylenically unsaturated monomers, at least one being a carboxyl monomer by in-situ polymerization of the monomers in the presence of phosphated epoxy polymer with at least 3% by weight of benzoyl peroxide based on the weight of monomers, or under equialent free radical initiating conditions using peroxide initiator, at temperatures between about 80° C. and 130° C., said epoxy coreacted with about 0.05% and 5% phosphoric acid selected from 100% ortho phosphoric acid, aqueous phosphoric acid or polyphosphoric acid phosphate based on epoxy resin to provide phosphated epoxy-acrylic reaction product containing by weight between 10% and 90% phosphated epoxy.
Claim 18
Dependent Claim
122 words
A phosphated epoxy-acrylic composition comprising the reaction product of: an epoxy polymer having a molecular weight between about 350 and 20,000 coreacted with ethylenically unsaturated monomers, at least one being a carboxyl monomer by in-situ polymerization of the monomers in the presence of phosphated epoxy polymer with at least 3% by weight of benzoyl peroxide based on the weight of monomers, or under equialent free radical initiating conditions using peroxide initiator, at temperatures between about 80° C. and 130° C., said epoxy coreacted with about 0.05% and 5% phosphoric acid selected from 100% ortho phosphoric acid, aqueous phosphoric acid or polyphosphoric acid phosphate based on epoxy resin to provide phosphated epoxy-acrylic reaction product containing by weight between 10% and 90% phosphated epoxy.
Claim 19
Dependent Claim
17 words
The phosphated epoxy-acrylic composition in claim 16 wherein the reaction product comprises epoxy phosphate and addition copolymer.
Claim 20
Dependent Claim
28 words
The phosphated epoxy-acrylic composition in claim 16 wherein the reaction product comprises epoxy phosphate, addition copolymer, and graft epoxy phosphate of addition polymer grafted to the epoxy phosphate.
Claim 21
Dependent Claim
19 words
The phosphated epoxy-acrylic composition in claim 16 wherein the epoxy phosphate contains 0.1% to 3% by weight coreacted phosphate.
Claim 22
Dependent Claim
15 words
The phosphated epoxy-acrylic composition in claim 16 ionized with ionizing base and dispersed into water.
Claim 23
Dependent Claim
21 words
The phosphated epoxy-acrylic composition in claim 16 wherein the polymerized addition polymerizable monomer comprises by weight 20% of an acrylic acid.
Claim 24
Dependent Claim
19 words
The phosphated epoxy-acrylic composition in claim 21 wherein the acrylic acid is selected from acrylic acid or methacrylic acid.
Claim 25
Dependent Claim
26 words
The phosphated epoxy-acrylic composition of claim 21 wherein the copolymerized polymerizable monomers include a minor amount of a lower alkyl ester of acrylic or methacrylic acid.
Claim 26
Dependent Claim
30 words
The phosphated epoxy-acrylic composition in claim 16 wherein a phosphated epoxy resin is preformed and coreacted with said ethylenically unsaturated monomers by in-situ polymerization to form said phosphated epoxy-acrylic composition.
Claim 27
Dependent Claim
29 words
The phosphated epoxy-acrylic composition in claim 16 wherein a preformed mixture comprising in-situ polymerization of said ethylenically unsaturated monomers in the presence of epoxy resin is coreacted with phosphate.
Claim 28
Dependent Claim
171 words
In a process for producing a phosphated epoxy-acrylic cmposition, the process comprising: polymerizing ethylenically unsaturated monomers, at least one being a carboxyl functional monomer, in the presence of epoxy resin having epoxide groups and having a molecular weight between about 350 and 20,000 and in the presence of at least 3% by weight of benzoyl peroxide based on the weight of ethylenically unsaturated monomers, or under equivalent free radical initiating conditions using a peroxide initiator, at temperatures between about 80° C. and 130° C., to provide a preformed in-situ polymerization product comprising on a weight basis between about 10% and 90% epoxy resin, and said preformed polymerization product containing carboxyl functionality sufficiently high to render the preformed polymerization product water dispersible, said preformed polymerization product coreacted with a source of phosphoric acid selected from 100% ortho phosphoric acid, aqueous phosphoric acid, or polyphosphoric acid to coreact phosphoric acid with the epoxy resin epoxy groups to produce a phosphated epoxy polymer containing by weight between about 0.05% and 5% coreacted phosphoric acid.
Claim 29
Dependent Claim
171 words
In a process for producing a phosphated epoxy-acrylic cmposition, the process comprising: polymerizing ethylenically unsaturated monomers, at least one being a carboxyl functional monomer, in the presence of epoxy resin having epoxide groups and having a molecular weight between about 350 and 20,000 and in the presence of at least 3% by weight of benzoyl peroxide based on the weight of ethylenically unsaturated monomers, or under equivalent free radical initiating conditions using a peroxide initiator, at temperatures between about 80° C. and 130° C., to provide a preformed in-situ polymerization product comprising on a weight basis between about 10% and 90% epoxy resin, and said preformed polymerization product containing carboxyl functionality sufficiently high to render the preformed polymerization product water dispersible, said preformed polymerization product coreacted with a source of phosphoric acid selected from 100% ortho phosphoric acid, aqueous phosphoric acid, or polyphosphoric acid to coreact phosphoric acid with the epoxy resin epoxy groups to produce a phosphated epoxy polymer containing by weight between about 0.05% and 5% coreacted phosphoric acid.
Claim 30
Dependent Claim
45 words
The process in claim 26 wherein the phosphated epoxy acrylic composition is produced by reacting a non-phosphated epoxy with an epoxy phosphate containing above 5% phosphate for time sufficient whereby the resulting phosphated epoxy resin contains between 0.05% and 5% by weight coreacted phosphoric acid.
Claim 31
Dependent Claim
22 words
The process in claim 26 wherein the phosphated epoxy acrylic composition contains between about 0.1% and 3% by weight coreacted phosphoric acid.
Claim 32
Dependent Claim
24 words
The process in claim 26 wherein a base ionizing agent ionizes the carboxyl functionality, and said preformed in-situ polymerization product is dispersed into water.
Claim 33
Dependent Claim
19 words
The process in claim 26 wherein the ethylenically unsaturated monomers include at least 20% by weight carboxyl functional monomer.
Claim 34
Dependent Claim
14 words
The process in claim 29 wherein the carboxyl functional monomer comprises an acrylic acid.
Claim 35
Dependent Claim
14 words
The process in claim 29 wherein the carboxyl functional monomer comprises a methacrylic acid.
Claim 36
Dependent Claim
17 words
The process in claim 26 wherein the ethylenically unsaturated monomers comprise styrene and acrylic or methacrylic acid.
Claim 37
Dependent Claim
21 words
The process in claim 32 wherein the ethylenically unsaturated monomers further include a lower alkyl ester of acrylic or methacrylic acid.
Claim 38
Dependent Claim
20 words
The process in claim 29 wherein the acid no. of the in-situ formed polymerization product is between 30 and 220.
Claim 39
Dependent Claim
30 words
The process in claim 26 wherein the benzoyl peroxide is at least 4% by weight based on monomer weight or under equivalent free radical initiating conditions using a peroxide initiator.
Claim 40
Dependent Claim
18 words
The process in claim 26 wherein the benzoyl peroxide level is at least 6% by weight of monomers.
Claim 41
Dependent Claim
29 words
The process in claim 26 wherein the preformed in-situ polymerization product includes a graft-epoxy polymer component formed by grafting between said addition polymer component and said epoxy resin component.
Claim 42
Dependent Claim
26 words
The process in claim 38 wherein the epoxy resin has aliphatic backbone carbons and grafting is onto the aliphatic backbone carbon atoms of the epoxy resin.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1989-07-14 | 1990-01-13 | 1990-07-15 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1993-07-14 | 1994-01-13 | 1994-07-15 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1997-07-14 | 1998-01-13 | 1998-07-15 | $7700.00 | Window Closed / Lapsed |