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US4049635A Expired / Lapsed US ⏱️ 0.0 years remaining

Production of tetramethylene terephthalate polymers using 225° to 248° C. polycondensation temperature

Assignee: Phillips Petroleum Co
•
Filing: 1976-01-19
•
Granted: 1977-09-20
•
Expires: 1996-01-19
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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 09:27
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.

References Cited (Backward Citations)

US2727881A Cited
DE1900270A1 Cited
DE2213259A1 Cited
US3817935A Cited
DE2315272A1 Cited
JPS4921497A Cited
US3965071A Cited
JPS5038791A Cited
US3907754A Cited

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

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