Patent US4071509A successfully refreshed from Google Patents.
US4071509A
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Arylene sulfide polymer purification
Assignee: Phillips Petroleum Co
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Filing: 1976-08-13
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Granted: 1978-01-31
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Expires: 1996-08-13
Abstract
Abstract Arylene sulfide polymers containing ash-forming impurities or materials are purified by heating such polymers with an organic amide and an alkali metal salt selected from carboxylates, carbonates, and selected lithium halides under conditions sufficient to reduce the ash-forming impurities without extensive polymer degradation.
Inventors
- 👤 James T. Edmonds, Jr.
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 15:52
CPC Classifications
C; C08; C08G; C08G75/00; C08G75/02; C08G75/0204; C08G75/0277; C08G75/0281; C08G75/0231; C08G75/025; C08G75/0254
Claims Analysis
Total Claims: 11
Claim 1
Independent Claim
138 words
A process for the reduction of ash-forming impurities contained in arylene sulfide polymers without extensive degradation of the polymer which comprises: a. forming a mixture comprising an arylene sulfide polymer containing at least 0.10 weight percent ash-forming impurities or materials, an organic amide, and at least one alkali metal salt selected from the group consisting of alkali metal carboxylates, alkali metal carbonates, and lithium halides selected from the group consisting of lithium chloride, lithium bromide, and lithium iodide, the amount of alkali metal salt present being sufficient to inhibit degradation of the polymer or to increase the molecular weight of the polymer, and b. heating said mixture formed in (a) at an elevated temperature and for a period of time sufficient to produce an arylene sulfide polymer of appreciably reduced ash content without extensive degradation of said polymer.
Claim 2
Dependent Claim
138 words
A process for the reduction of ash-forming impurities contained in arylene sulfide polymers without extensive degradation of the polymer which comprises: a. forming a mixture comprising an arylene sulfide polymer containing at least 0.10 weight percent ash-forming impurities or materials, an organic amide, and at least one alkali metal salt selected from the group consisting of alkali metal carboxylates, alkali metal carbonates, and lithium halides selected from the group consisting of lithium chloride, lithium bromide, and lithium iodide, the amount of alkali metal salt present being sufficient to inhibit degradation of the polymer or to increase the molecular weight of the polymer, and b. heating said mixture formed in (a) at an elevated temperature and for a period of time sufficient to produce an arylene sulfide polymer of appreciably reduced ash content without extensive degradation of said polymer.
Claim 3
Dependent Claim
38 words
A process according to claim 1 wherein at least the alkali metal salt is heated, prior to forming the mixture in (a), at an elevated temperature sufficient to effect at least partial dehydration of said alkali metal salt.
Claim 4
Dependent Claim
36 words
A process according to claim 1 wherein said organic amide and said alkali metal salt are heated at an elevated temperature sufficient to effect dehydration prior to addition of polymer to form said mixture in (a).
Claim 5
Dependent Claim
20 words
A process according to claim 1 wherein water is added to the mixture of (a) prior to heating in (b).
Claim 6
Dependent Claim
84 words
A process according to claim 1 wherein the temperature in (b) is in the range of about 150° C to about 280° C and said heating is effected under sufficient pressure to maintain the organic amide substantially in the liquid phase, the weight ratio of organic amide to arylene sulfide polymer is within the range of about 1:1 to about 20:1, and the amount of alkali metal salt present ranges from about 0.05 to about 4 g-moles per 100 g of arylene sulfide polymer.
Claim 7
Dependent Claim
36 words
A process according to claim 1 wherein said arylene sulfide polymer is poly(phenylene sulfide), said organic amide is N-methyl-2-pyrrolidone, and said alkali metal salt is lithium chloride, lithium acetate dihydrate, sodium carbonate monohydrate, or sodium acetate.
Claim 8
Dependent Claim
55 words
A process according to claim 3 wherein said arylene sulfide polymer is poly(phenylene sulfide), said organic amide is N-methyl-2-pyrrolidone, and said alkali metal salt is lithium acetate dihydrate, and the mixture of N-methyl-2-pyrrolidone and lithium acetate dihydrate is heated under conditions such that the mixture is substantially dehydrated, cooled, and then mixed with poly(phenylene sulfide).
Claim 9
Dependent Claim
27 words
A process according to claim 4 wherein said arylene sulfide polymer is poly(phenylene sulfide), said organic amide is N-methyl-2-pyrrolidone, and said alkali metal salt is sodium acetate.
Claim 10
Dependent Claim
76 words
A process according to claim 1 wherein the temperature in (b) is in the range of about 200° C to about 270° C, the pressure is sufficient to maintain the organic amide under liquid phase conditions, the weight ratio of organic amide to arylene sulfide polymer ranges from about 3:1 to about 15:1, and the amount of alkali metal salt employed ranges from about 0.1 to about 2 g-moles per 100 g of arylene sulfide polymer.
Claim 11
Dependent Claim
60 words
A process according to claim 1 wherein said organic amide is a cyclic or acyclic amide having from 1 to about 10 carbon atoms per molecule, and said alkali metal carboxylates can be represented by the formula RCO 2 M where R is a hydrocarbyl radical having from 1 to about 20 carbon atoms and M is an alkali metal.
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) | 1981-01-30 | 1981-08-01 | 1982-01-31 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1985-01-30 | 1985-08-01 | 1986-01-31 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1989-01-30 | 1989-08-01 | 1990-01-31 | $7700.00 | Window Closed / Lapsed |