US3965071A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Polyester catalysts
Assignee: Imperial Chemical Industries Ltd
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Filing: 1974-07-01
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Granted: 1976-06-22
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Expires: 1994-07-01
Abstract
Abstract Manufacture of polyesters and copolyesters by reaction of at least one aromatic dicarboxylic acid with at least one glycol in presence of titanium compound, deactivation of catalyst by reaction with phosphoric acid or ester and polycondensation in presence of antimony compound.
Inventors
- 👤 Euan McClelland
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 20:05
CPC Classifications
C; C08; C08G; C08G63/00; C08G63/78; C08G63/82; C08G63/85; C08G63/83
Claims Analysis
Total Claims: 22
Claim 1
Independent Claim
161 words
A process for preparing a fiber-forming polymeric polyester or copolyester which comprises first forming an ester by esterification reaction between an aromatic dicarboxylic acid and a diol in the presence of a titanium compound as esterification catalyst, deactivating the catalytic titanium compound after the esterification is substantially complete by reacting said compound with phosphoric acid or a phosphate ester and thereafter polycondensing said ester in the presence of a polycondensation catalyst which is a compound selected from the group consisting of antimony and germanium compounds which are soluble in the reaction mixture to form said polyester or copolyester, the diol being a diol of the formula HO(CH 2 ) n OH wherein n is not less than 2 and not greater than 10 and the titanium compound being a tetraalkyl titanate wherein alkyl is of 1 to 4 carbon atoms, a titanate of ethylene glycol, hexylene glycol or octylene glycol, or isopropyl triethanolamine titanate, sodium or lithium titanate or a titanosiloxane.
Claim 2
Dependent Claim
161 words
A process for preparing a fiber-forming polymeric polyester or copolyester which comprises first forming an ester by esterification reaction between an aromatic dicarboxylic acid and a diol in the presence of a titanium compound as esterification catalyst, deactivating the catalytic titanium compound after the esterification is substantially complete by reacting said compound with phosphoric acid or a phosphate ester and thereafter polycondensing said ester in the presence of a polycondensation catalyst which is a compound selected from the group consisting of antimony and germanium compounds which are soluble in the reaction mixture to form said polyester or copolyester, the diol being a diol of the formula HO(CH 2 ) n OH wherein n is not less than 2 and not greater than 10 and the titanium compound being a tetraalkyl titanate wherein alkyl is of 1 to 4 carbon atoms, a titanate of ethylene glycol, hexylene glycol or octylene glycol, or isopropyl triethanolamine titanate, sodium or lithium titanate or a titanosiloxane.
Claim 3
Dependent Claim
21 words
A process according to claim 1 wherein the esterification reactants comprise terephthalic acid, naphthalene-2:6-dicarboxylic acid, 1:2-diphenoxyethane-4:4-dicarboxylic acid or biphenyl-4:4' -dicarboxylic acid.
Claim 4
Dependent Claim
13 words
A process according to claim 1 wherein the dicarboxylic acid is terephthalic acid.
Claim 5
Dependent Claim
33 words
A process according to claim 1 wherein the esterification reactants comprise a diol of the formula HO(CH 2 ) n OH wherein n is not less than 2 and not greater than 10.
Claim 6
Dependent Claim
12 words
A process according to claim 4 wherein n is 2 or 4.
Claim 7
Dependent Claim
12 words
A process according to claim 4 wherein the diol is ethylene glycol.
Claim 8
Dependent Claim
12 words
A process according to claim 1 wherein the polyester is poly(ethylene terephthalate.
Claim 9
Dependent Claim
29 words
A process according to claim 1 wherein the manufacture is of a copolyester comprising structural units based on a second dicarboxylic acid which is isophthalic acid or adipic acid.
Claim 10
Dependent Claim
37 words
A process according to claim 1 wherein the titanium compound is a tetraalkyl titanate wherein alkyl is of 1 to 4 carbon atoms, a titanate of ethylene glycol, hexylene glycol or octylene glycol, or isopropyl triethanolamine titanate.
Claim 11
Dependent Claim
15 words
A process according to claim 1 wherein the titanium compound is sodium or lithium titanate.
Claim 12
Dependent Claim
13 words
A process according to claim 1 wherein the titanium compound is a titanosiloxane.
Claim 13
Dependent Claim
43 words
A process according to claim 1 wherein the proportion of titanium compound employed is not less than 0.0005% and not greater than 0.05%, expressed in terms of titanium based on the weight of terephthalic acid equivalent to the dicarboxylic acid or acids reacted.
Claim 14
Dependent Claim
27 words
A process according to claim 1 wherein the quantity of phosphoric acid or phosphate ester added amounts to at least one molecule for each atom of titanium.
Claim 15
Dependent Claim
39 words
A process according to claim 1 wherein the quantity of phosphoric acid or phosphate ester does not exceed 1,160 part per million expressed as phosphoric acid based on the terephthalic acid equivalent of the dicarboxylic acid or acids reacted.
Claim 16
Dependent Claim
16 words
A process according to claim 1 wherein the esterification stage is carried out at superatmospheric pressure.
Claim 17
Dependent Claim
20 words
A process according to claim 1 wherein during the esterification the water vapour produced is purged continuously from the system.
Claim 18
Dependent Claim
25 words
A process according to claim 1 wherein the ratio of diol to dicarboxylic acid is no less than 1.05:1 and not greater than 3:1 molecularly.
Claim 19
Dependent Claim
23 words
A process according to claim 1 wherein the polycondensation catalyst employed is antimony trioxide, antimonic acid, antimony glycoloxide, antimony triacetate or antimony trichloride.
Claim 20
Dependent Claim
35 words
A process according to claim 1 wherein the polycondensation catalyst employed is germanium dioxide in the amorphous form, germanium tetrachloride, a salt of a germanium acid or a compound derived from ethylene glycol and germanium.
Claim 21
Dependent Claim
18 words
A process according to claim 1 wherein the polycondensation catalyst is added after the esterification stage is completed.
Claim 22
Dependent Claim
51 words
A process according to claim 1 wherein during the esterification stage the terephthalate of a base is present in amount not less than 10 and not greater than 500 parts per million, expressed as sodium hydroxide equivalent to the terephthalate, on terephthalic acid equivalent to the dicarboxylic acid or acids reacted.
References Cited (Backward Citations)
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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) | 1979-06-22 | 1979-12-22 | 1980-06-22 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-06-22 | 1983-12-22 | 1984-06-22 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-06-22 | 1987-12-22 | 1988-06-22 | $7700.00 | Window Closed / Lapsed |