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Patent US4535145A successfully refreshed from Google Patents.
US4535145A
Expired / Lapsed
US
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Process for the preparation of polyesters from aliphatic dicarboxylic acids and polyalkylpiperidyl diols
Assignee: BASF Corp
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Filing: 1984-06-29
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Granted: 1985-08-13
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Expires: 2004-06-29
Abstract
Abstract The invention relates to a novel process for the preparation of compounds of the formula I ##STR1## by polycondensation of a diol of the formula II ##STR2## with a dicarboxylic acid ester of the formula III ##STR3## In the above formulae, the substituents and symbols R 1 , R 2 , R 3 and n are as defined in claim 1. The process comprises stirring the reaction medium which contains an excess of 2 to 50 mol. %, based on the diol of formula II, of the dicarboxylic acid ester of the formula III, in the presence of at least 0.03 mol. % of a suitable catalyst, until the bulk of the alkanol of the formula R 3 OH formed during the reaction is distilled off, under a pressure of 0.7 to 1.3 bar, and thereafter stirring under a pressure of less than 5 mbar, in the temperature range from 100° to 170° C., and subsequently working up the resultant melt in conventional manner.
Inventors
- 👤 Eduard Troxler
- 👤 Thomas Kainmuller
- 👤 Rudolf Maul
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 11:23
CPC Classifications
C; C08; C08G; C08G63/00; C08G63/68; C08G63/685; C08G63/6854; C08G63/6856; C08G63/78; C08G63/82; C08G63/85
Claims Analysis
Total Claims: 6
Claim 1
Independent Claim
230 words
A process for the preparation of a compound of the formula I ##STR8## wherein n is a value from 8 to 25, preferably from 10 to 20, R 1 and R 2 , each independently of the other, are C 1 -C 18 alkylene, C 2 -C 18 alkylene which is interrupted by --O--, --S-- or --N(R)--, in which R is hydrogen or C 1 -C 4 alkyl, or are C 4 -C 8 alkenylene, and R 3 is C 1 -C 4 alkyl, by polycondensation of a diol of the formula II ##STR9## with a dicarboxylic acid ester of the formula III ##STR10## which process comprises stirring the reaction medium which contains an excess of 2 to 50 mol.%, based on the diol of the formula II, of the dicarboxylic acid ester of the formula III, in the presence of at least 0.03 mol.%, of an oxide or of an organometal compound of a metal of the 4th main group or of the 4th auxiliary group of the Periodic Table, until the bulk of the alkanol of the formula R 3 OH which forms during the reaction is distilled off, under a pressure of 0.7 to 1.3 bar, and thereafter stirring under a pressure of less than 10 mbar, in the temperature range from 100° to 170° C., and then working up the melt so obtained in conventional manner.
Claim 2
Dependent Claim
230 words
A process for the preparation of a compound of the formula I ##STR8## wherein n is a value from 8 to 25, preferably from 10 to 20, R 1 and R 2 , each independently of the other, are C 1 -C 18 alkylene, C 2 -C 18 alkylene which is interrupted by --O--, --S-- or --N(R)--, in which R is hydrogen or C 1 -C 4 alkyl, or are C 4 -C 8 alkenylene, and R 3 is C 1 -C 4 alkyl, by polycondensation of a diol of the formula II ##STR9## with a dicarboxylic acid ester of the formula III ##STR10## which process comprises stirring the reaction medium which contains an excess of 2 to 50 mol.%, based on the diol of the formula II, of the dicarboxylic acid ester of the formula III, in the presence of at least 0.03 mol.%, of an oxide or of an organometal compound of a metal of the 4th main group or of the 4th auxiliary group of the Periodic Table, until the bulk of the alkanol of the formula R 3 OH which forms during the reaction is distilled off, under a pressure of 0.7 to 1.3 bar, and thereafter stirring under a pressure of less than 10 mbar, in the temperature range from 100° to 170° C., and then working up the melt so obtained in conventional manner.
Claim 3
Dependent Claim
59 words
A process according to claim 1 for the preparation of a compound of the formula I, wherein n is a value from 10 to 20, R 1 and R 2 are ethylene and R 3 is methyl or ethyl, which comprises reacting 1-(2-hydroxyethyl)-2,2,6,6-tetramethyl-4-hydroxypiperidine with a 5 to 20 mol.% excess of methyl or ethyl succinate, based on the diol.
Claim 4
Dependent Claim
60 words
A process according to claim 1, which comprises stirring the reaction medium under a pressure of 0.9 to 1.1 bar until 70 to 80% of the alkanol of the formula R 3 OH formed during the reaction is distilled off, and thereafter stirring under a pressure of less than 5 mbar in the temperature range from 120° to 150° C.
Claim 5
Dependent Claim
27 words
A process according to claim 1, wherein the catalyst is used in an amount from 0.05 to 1.0 mol.%, based on the diol of the formula II.
Claim 6
Dependent Claim
16 words
A process according to claim 4, wherein tetrabutyl orthotitanate or tetraisopropyl orthotitanate is used as catalyst.
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) | 1988-08-12 | 1989-02-11 | 1989-08-13 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-08-12 | 1993-02-11 | 1993-08-13 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-08-12 | 1997-02-11 | 1997-08-13 | $7700.00 | Window Closed / Lapsed |