Patent US3839296A successfully refreshed from Google Patents.
US3839296A
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US
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Sequential preparation of tractable polyterephthalamides
Assignee: Phillips Petroleum Co
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Filing: 1972-05-22
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Granted: 1974-10-01
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Expires: 1992-05-22
Abstract
Abstract A salt of dicarboxylic acid and diamine, at least 50 mole percent of the dicarboxylic acid being terephthalic acid, is condensed to form a polyterephthalamide by heating the salt to a temperature in the range of about 200*C. to about 230*C. and maintaining the salt at that temperature for about 1/2 hour to about 6 hours before increasing the temperature of the salt to at least 250*C. In one specific embodiment the salt contains from about 2 to about 8 mole percent excess acid.
Inventors
- 👤 R Campbell
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 07:57
CPC Classifications
C; C08; C08G; C08G69/00; C08G69/02; C08G69/26; C08G69/28
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
192 words
A METHOD OF PRODUCING A TRACTABLE RESINOUS POLYTEREPHTHALAMIDE FROM A SALT OF DICARBOXYLIC ACID AND DIAMINE, AT LEAST 50 MOLE PERCENT OF SAID DICARBOCYLIC ACID BEING TEREPHTHALIC ACID, SAID DIAMINE HAVING THE FORMULA H2N-R-NH2 WHEREIN R IS A DIVALENT HYDROCARBON RADICAL HAVING FROM 6 TO 20 CARBON ATOMS AND WHEREIN EACH -NH2 GROUP IS ATTACHED TO AN ALIPHATIC OR CYCLOALIPHTIC CARBON ATOM OF SAID HYDROCARBON RADICAL, WHICH COMPRISES, IN THE RECITED SEQUENCE, THE STEPS OF HEATING SAID SALT DURING A FIRST PERIOD OF TIME TO A FIRST TEMPER TURE IN THE RANGEOF ABOUT 200*C TO ABOUT 230*C, THEN TREATING THE THUS HEATED MATEIAL BY MAINTAINING SAID THUS HEATED MATERIAL AT LEAST SUBSTANTIALLY AT SAID FIRST TEMPERATURE FOR A SECOND PERIOD OF TIME IN THE RANGE OF ABOUT 1/2 HOUR TO ABOUT 6 HOURS, THEN HEATING THE THUS TREATED MATERIAL DURING A THIRD PERIOD OF TIME TO A SECOND TEMPERATURE OF AT LEAST 295*C, THEN MAINTAINING THE THUS HEATED TREATED MATERIAL AT LEAST SUBSTANTIALLY CONSTANT AT SAID SECOND TEMPERATURE FOR A FOURTH PERIOD OF TIME IN THE RANGE OF ABOUT 1/4 HOUR TO ABOUT 20 HOURS, AND THEN RECOVERING THE THUS PRODUCED POLYTEREPHTHALAMIDE.
Claim 2
Independent Claim
192 words
A METHOD OF PRODUCING A TRACTABLE RESINOUS POLYTEREPHTHALAMIDE FROM A SALT OF DICARBOXYLIC ACID AND DIAMINE, AT LEAST 50 MOLE PERCENT OF SAID DICARBOCYLIC ACID BEING TEREPHTHALIC ACID, SAID DIAMINE HAVING THE FORMULA H2N-R-NH2 WHEREIN R IS A DIVALENT HYDROCARBON RADICAL HAVING FROM 6 TO 20 CARBON ATOMS AND WHEREIN EACH -NH2 GROUP IS ATTACHED TO AN ALIPHATIC OR CYCLOALIPHTIC CARBON ATOM OF SAID HYDROCARBON RADICAL, WHICH COMPRISES, IN THE RECITED SEQUENCE, THE STEPS OF HEATING SAID SALT DURING A FIRST PERIOD OF TIME TO A FIRST TEMPER TURE IN THE RANGEOF ABOUT 200*C TO ABOUT 230*C, THEN TREATING THE THUS HEATED MATEIAL BY MAINTAINING SAID THUS HEATED MATERIAL AT LEAST SUBSTANTIALLY AT SAID FIRST TEMPERATURE FOR A SECOND PERIOD OF TIME IN THE RANGE OF ABOUT 1/2 HOUR TO ABOUT 6 HOURS, THEN HEATING THE THUS TREATED MATERIAL DURING A THIRD PERIOD OF TIME TO A SECOND TEMPERATURE OF AT LEAST 295*C, THEN MAINTAINING THE THUS HEATED TREATED MATERIAL AT LEAST SUBSTANTIALLY CONSTANT AT SAID SECOND TEMPERATURE FOR A FOURTH PERIOD OF TIME IN THE RANGE OF ABOUT 1/4 HOUR TO ABOUT 20 HOURS, AND THEN RECOVERING THE THUS PRODUCED POLYTEREPHTHALAMIDE.
Claim 3
Dependent Claim
18 words
A method in accordance with claim 1 wherein at least 70 mole percent of said diamine is 1,12-dodecanediamine.
Claim 4
Dependent Claim
14 words
A method in accordance with claim 1 wherein said salt is 1, 12-dodecanediammonium terephthalate.
Claim 5
Dependent Claim
44 words
A method in accordance with claim 1 wherein said salt contains from about 2 mole percent of said diamine in excess of the molar amount of said acid up to about 8 mole percent acid in excess of the molar amount of said diamine.
Claim 6
Dependent Claim
28 words
A method in accordance with claim 1 wherein said dicarboxylic acid comprises up to 30 mole percent of a second acid having from 6 to 20 carbon atoms.
Claim 7
Dependent Claim
39 words
A method in accordance with claim 1 wherein said first temperature is in the range of about 200*C to about 220*C, and said seCond period of time is in the range of about 1 hour to about 4 hours.
Claim 8
Dependent Claim
18 words
A method in accordance with claim 6 wherein at least 70 mole percent of said diamine is 1,12-dodecanediamine.
Claim 9
Dependent Claim
14 words
A method in accordance with claim 6 wherein said salt is 1, 12-dodecanediammonium terephthalate.
Claim 10
Dependent Claim
31 words
A method in accordance with claim 6 wherein said salt contains from about 1 to about 5 mole percent of said acid in excess of the molar amount of said diamine.
Claim 11
Dependent Claim
35 words
A method in accordance with claim 6 wherein said fourth period of time is in the range of about 1 hour to about 8 hours, and said diamine has from 8 to 15 carbon atoms.
Claim 12
Dependent Claim
30 words
A method in accordance with claim 10 wherein the temperature of said salt is increased at an at least substantially uniform rate during said first and third periods of time.
Claim 13
Dependent Claim
19 words
A method in accordance with claim 11 wherein at least 70 mole percent of said salt is 1,12-dodecanediammonium terephthalate.
Claim 14
Dependent Claim
31 words
A method in accordance with claim 12 wherein said salt contains from about 1 to about 5 mole percent of said acid in excess of the molar amount of said diamine.
Claim 15
Dependent Claim
29 words
A method in accordance with claim 11 wherein at least 70 mole percent of said salt is the salt of terephthalic acid and an admixture of 4,6-dimethyl-1,3-bis(2-aminoethyl)benzene and 2,4-dimethyl-1,3-bis(2-aminoethyl)benzene.
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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) | 1977-09-30 | 1978-04-01 | 1978-10-01 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1981-09-30 | 1982-04-01 | 1982-10-01 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1985-09-30 | 1986-04-01 | 1986-10-01 | $7700.00 | Window Closed / Lapsed |