US3907863A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for making polyester polyols having a low acid number
Assignee: BASF Corp
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Filing: 1974-03-14
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Granted: 1975-09-23
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Expires: 1994-03-14
Abstract
Abstract Catalyst free polyester polyols for use in polyurethane compositions are prepared by melt-condensation of polyalcohols and polycarboxylic acids. When the resulting polyol obtains an acid number of 480 or less, selected distillable mono- and/or dialcohols are added and the condensation continued until an acid number of less than one is obtained. By the same process out of specification polyester polyols can be regenerated for polyurethane use.
Inventors
- 👤 Harro Voss
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-28 18:45
CPC Classifications
C; C08; C08G; C08G63/00; C08G63/02; C08G63/12; C08G63/46; C08G63/50; C08G18/00; C08G18/06; C08G18/28; C08G18/40; C08G18/42; C08G63/16; C08G63/20
Claims Analysis
Total Claims: 11
Claim 1
Independent Claim
240 words
IN A PROCESS FOR THE PREPARATION OF POLYESTER POLYOLS BY THE MELT-CONDENSATION ESTERIFICATION OF A POLYHYDRIC ALCHOL SELECTED FROM THE GROUP CONSISTING OF POLYETHER DIOLS AND POLYESTER DIOLS AND A POLYCARBOXYLIC ACID AT A TEMPERATURE FROM ABOUT 150* TO ABOUT 300*C WHEREIN RESIDUAL AMOUNTS OF ACTIVE CATALYST IS UNDESIRABLE, THE IMPROVEMENT FOR PRODUCING SUCH POLYOLS HAVING AN ACID NUMBER LESS THAN ONE WHICH COMPRISES, CONTINUING THE ESTERIFICATION UNTIL THE PRODUCT HAS AN ACID NUMBER OF 480 OR LESS AND THEN ADDING TO THE ESTERIFICATION MIXTURE OF REACTANTS AND PRODUCT A DISTILLABLE ALCOHOL IN AN AMOUNT OF 0.1 TO 1.4 MOLES PER MOLE OF CARBOXYLIC ACID CHARGED AND CONTAINING THE ESTERIFICATION WHILE SIMULTANEOUSLY DISTILLING OFF THE EXCESS DISTILLABLE ALCHOL UNTIL THE ESTERIFICATION IS COMPLETED, SAID DISTILLABLE ALCOHOL HOL BEING SELECTED FROM THE GROUP CONSISTING OF (A) MONOHYDROXY NORMAL, BRANCHED OR CYCLO ALKYL, ALKENE OR ALKINE ALCOHOLS CONTAINING FROM 1 TO 6 CARBON ATOMS, (B) AROMATIC MONOHYDROXY ALCOHOLS, (C) DIHYDROXY NORMAL, BRANCHED OR CYCLO ALKYL, ALKENE OR ALKINE ALCOHOLS CONTAINING FROM 2 TO 8 CARBON ATOMS DIALKYL ETHER GYCOLS CONTAINING FROM 2 TO 8 CARBON ATOMS IN EACH ALKYL GROUP AND MIXTURES THEREOF, SAID POLYETHER AND POLYESTER DIOLS HAVING A MOLECULAR WEIGHT FROM 200 TO 4500, SAID DISTILLABLE ALCOHOL BEING SAID MONOHYDROXY ALCOHOLS WHEN SAID ACID NUMBER IS LESS THAN 60 PRIOR TO SAID DISTILLABLE ALCOHOL ADDITION AND DIALCOHOLS OR MIXTURES OF DI-AND MONOALCOHOLS WHEN SAID ACID NUMBER IS GREATER THAN 60.
Claim 2
Dependent Claim
240 words
IN A PROCESS FOR THE PREPARATION OF POLYESTER POLYOLS BY THE MELT-CONDENSATION ESTERIFICATION OF A POLYHYDRIC ALCHOL SELECTED FROM THE GROUP CONSISTING OF POLYETHER DIOLS AND POLYESTER DIOLS AND A POLYCARBOXYLIC ACID AT A TEMPERATURE FROM ABOUT 150* TO ABOUT 300*C WHEREIN RESIDUAL AMOUNTS OF ACTIVE CATALYST IS UNDESIRABLE, THE IMPROVEMENT FOR PRODUCING SUCH POLYOLS HAVING AN ACID NUMBER LESS THAN ONE WHICH COMPRISES, CONTINUING THE ESTERIFICATION UNTIL THE PRODUCT HAS AN ACID NUMBER OF 480 OR LESS AND THEN ADDING TO THE ESTERIFICATION MIXTURE OF REACTANTS AND PRODUCT A DISTILLABLE ALCOHOL IN AN AMOUNT OF 0.1 TO 1.4 MOLES PER MOLE OF CARBOXYLIC ACID CHARGED AND CONTAINING THE ESTERIFICATION WHILE SIMULTANEOUSLY DISTILLING OFF THE EXCESS DISTILLABLE ALCHOL UNTIL THE ESTERIFICATION IS COMPLETED, SAID DISTILLABLE ALCOHOL HOL BEING SELECTED FROM THE GROUP CONSISTING OF (A) MONOHYDROXY NORMAL, BRANCHED OR CYCLO ALKYL, ALKENE OR ALKINE ALCOHOLS CONTAINING FROM 1 TO 6 CARBON ATOMS, (B) AROMATIC MONOHYDROXY ALCOHOLS, (C) DIHYDROXY NORMAL, BRANCHED OR CYCLO ALKYL, ALKENE OR ALKINE ALCOHOLS CONTAINING FROM 2 TO 8 CARBON ATOMS DIALKYL ETHER GYCOLS CONTAINING FROM 2 TO 8 CARBON ATOMS IN EACH ALKYL GROUP AND MIXTURES THEREOF, SAID POLYETHER AND POLYESTER DIOLS HAVING A MOLECULAR WEIGHT FROM 200 TO 4500, SAID DISTILLABLE ALCOHOL BEING SAID MONOHYDROXY ALCOHOLS WHEN SAID ACID NUMBER IS LESS THAN 60 PRIOR TO SAID DISTILLABLE ALCOHOL ADDITION AND DIALCOHOLS OR MIXTURES OF DI-AND MONOALCOHOLS WHEN SAID ACID NUMBER IS GREATER THAN 60.
Claim 3
Dependent Claim
32 words
The process of claim 1 wherein the polyhydric alcohol is a poly(alkylether) diol wherein each alkyl group contains from 2 to 4 carbon atoms and a molecular weight up to about 4500.
Claim 4
Dependent Claim
21 words
The process of claim 1 wherein the acid number is 270 or less and the distillable alcohol is a dihydroxy alcohol.
Claim 5
Dependent Claim
25 words
The process of claim 1 wherein the acid number is 270 or less and the distillable alcohol is a mixture of mono- and dihydroxy alcohols.
Claim 6
Dependent Claim
22 words
The process according to claim 1 wherein the acid number is 60 or less and the distillable alcohol is a monohydroxy alcohol.
Claim 7
Dependent Claim
14 words
The process according to claim 5 wherein the acid number is 25 or less.
Claim 8
Dependent Claim
24 words
The process according to claim 1 wherein the esterification is continued after the addition of distillable alcohol at a temperature from 150* to 250*C.
Claim 9
Dependent Claim
14 words
The process according to claim 7 wherein the temperature is from 160* to 220*C.
Claim 10
Dependent Claim
18 words
The process according to claim 1 wherein the amount of distillable alcohol added is 0.3 to 1.2 moles.
Claim 11
Dependent Claim
44 words
A process for the regeneration of partially hydrolized polyester polyols which have an acid number of less than 60 are no longer suitable for use in polyurethane formulations by using said hydrolized polyester polyol as the esterification mixture in the process of claim 1.
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) | 1978-09-22 | 1979-03-24 | 1979-09-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-09-22 | 1983-03-24 | 1983-09-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-09-22 | 1987-03-24 | 1987-09-23 | $7700.00 | Window Closed / Lapsed |