Patent US4049635A successfully refreshed from Google Patents.
US4049635A
Expired / Lapsed
US
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Production of tetramethylene terephthalate polymers using 225° to 248° C. polycondensation temperature
Assignee: Phillips Petroleum Co
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Filing: 1976-01-19
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Granted: 1977-09-20
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Expires: 1996-01-19
Abstract
Abstract 1,4-Butanediol and a dialkyl benzenedicarboxylate such as dimethyl terephthalate are subjected to transesterification conditions and thereafter to polycondensation in the presence of a tetraalkyl titanate catalyst at a temperature within the range of 225° to 248° C.
Inventors
- 👤 James W. Cleary
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-27 14:15
CPC Classifications
C; C08; C08G; C08G63/00; C08G63/78
Claims Analysis
Total Claims: 9
Claim 1
Independent Claim
174 words
A process for preparing a polyester comprising; transesterifying 1,4-butanediol and at least one dialkyl benzenedicarboxylate consisting of 80 to 100 mole percent of at least one dialkyl terephthalate and 0- 20 mole percent of at least one ester selected from dialkyl phthalates and dialkyl isophthalates, each of said alkyls of said dialkyl benzenedicarboxylate being selected from alkyl groups having 1 to 4 carbon atoms, by contacting said 1,4-butanediol and said at least one dialkyl benzenedicarboxylate with a transesterification and polycondensation catalyst consisting essentially of a tetraalkyl titanate of the formula Ti(OR) 4 wherein R is an alkyl group having 1 to 6 carbon atoms, said contacting being carried out at a temperature within a range of 130° C. to 248° C. at substantially atmospheric pressure; and thereafter subjecting the resulting mixture in a melt state to a temperature within the range of 225° to 248° C. and reduced pressure for a time within the range of 2 to 8 hours to effect polycondensation, said temperature during said polycondensation at no time exceeding 248° C.
Claim 2
Dependent Claim
174 words
A process for preparing a polyester comprising; transesterifying 1,4-butanediol and at least one dialkyl benzenedicarboxylate consisting of 80 to 100 mole percent of at least one dialkyl terephthalate and 0- 20 mole percent of at least one ester selected from dialkyl phthalates and dialkyl isophthalates, each of said alkyls of said dialkyl benzenedicarboxylate being selected from alkyl groups having 1 to 4 carbon atoms, by contacting said 1,4-butanediol and said at least one dialkyl benzenedicarboxylate with a transesterification and polycondensation catalyst consisting essentially of a tetraalkyl titanate of the formula Ti(OR) 4 wherein R is an alkyl group having 1 to 6 carbon atoms, said contacting being carried out at a temperature within a range of 130° C. to 248° C. at substantially atmospheric pressure; and thereafter subjecting the resulting mixture in a melt state to a temperature within the range of 225° to 248° C. and reduced pressure for a time within the range of 2 to 8 hours to effect polycondensation, said temperature during said polycondensation at no time exceeding 248° C.
Claim 3
Dependent Claim
17 words
The method according to claim 1 wherein said alkyl groups of said dialkyl benzenedicarboxylate are methyl groups.
Claim 4
Dependent Claim
18 words
The method according to claim 1 wherein said at least one dialkyl benzenedicarboxylate consists essentially of dimethyl terephthalate.
Claim 5
Dependent Claim
25 words
The method according to claim 1 wherein the mole ratio of said 1,4-butanediol to said dialkyl benzenedicarboxylate is within the range of 1.3:1 to 3:1.
Claim 6
Dependent Claim
13 words
The method according to claim 1 wherein said tetraalkyl titanate is tetraisopropyl titanate.
Claim 7
Dependent Claim
28 words
The method according to claim 1 wherein said catalyst is present in an amount within the range of 0.2 to 2 millimoles per mole of total dialkyl benzenedicarboxylate.
Claim 8
Dependent Claim
30 words
The method according to claim 1 wherein the temperature is raised during said transesterification, said transesterification taking place over a time period within the range of 3/4 to 3 hours.
Claim 9
Dependent Claim
63 words
The method according to claim 7 wherein said at least one dialkyl benzenedicarboxylate consists essentially of dimethyl terephthalate, the mole ratio of said 1,4-butanediol to said dimethyl terephthalate is within the range of 1.3:1 to 3:1, said catalyst is tetraisopropyl titanate, and said catalyst is present in an amount within the range of 0.2 to 2 millimoles per mole of said dimethyl terephthalate.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-09-19 | 1981-03-21 | 1981-09-20 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-09-19 | 1985-03-21 | 1985-09-20 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-09-19 | 1989-03-21 | 1989-09-20 | $7700.00 | Window Closed / Lapsed |