US4293658A
Expired / Lapsed
US
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Process for rigid foams of improved friability
Assignee: Air Products and Chemicals Inc
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Filing: 1980-05-12
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Granted: 1981-10-06
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Expires: 2000-05-12
Abstract
Abstract Polyurethanes based on a resole-type polyol can be significantly improved in their friability when the urethane catalyst is a fully neutralized tertiary amine salt and butyl benzyl phthalate is used as the plasticizer. The polyol is prepared by reacting a phenol and formaldehyde under substantially anhydrous conditions with continuous removal of water, and has a water content of no more than about 5%.
Inventors
- 👤 Daniel S. Raden
- 👤 Francis W. Arbir
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 18:52
CPC Classifications
C; C08; C08J; C08J9/00; C08J9/0014; C08J9/0023; C08G; C08G18/00; C08G18/06; C08G18/08; C08G18/16; C08G18/18; C08G18/1875; C08G18/28; C08G18/40; C08G18/54; C08G18/542; C08G2110/00; C08G2110/0025; C08J2375/00; C08J2375/04
Claims Analysis
Total Claims: 24
Claim 1
Independent Claim
85 words
The process of making a rigid, cellular polyurethane with improved friability, comprising reacting a polyisocyanate with a polyol in the presence of a fully neutralized salt of a tertiary amine, a surfactant, a blowing agent, and at least a minor proportion of butyl benzyl phthalate, said polyol being prepared by reacting a phenol and formaldehyde under substantially anhydrous conditions with continuous removal of water, said polyol having a water content of no more than about 5% and having at least four phenyl groups per mole.
Claim 2
Dependent Claim
85 words
The process of making a rigid, cellular polyurethane with improved friability, comprising reacting a polyisocyanate with a polyol in the presence of a fully neutralized salt of a tertiary amine, a surfactant, a blowing agent, and at least a minor proportion of butyl benzyl phthalate, said polyol being prepared by reacting a phenol and formaldehyde under substantially anhydrous conditions with continuous removal of water, said polyol having a water content of no more than about 5% and having at least four phenyl groups per mole.
Claim 3
Dependent Claim
29 words
The process of claim 1 wherein said tertiary amine salt is present in an amount of between 0.001 and 0.05 molar equivalents based on the amount of said polyol.
Claim 4
Dependent Claim
21 words
The process of claim 2 wherein said salt contains as the acid portion an organic acid with a pKa of >3.0.
Claim 5
Dependent Claim
13 words
The process of claim 1 wherein said tertiary amine is a bicyclic amidine.
Claim 6
Dependent Claim
10 words
The process of claim 4 wherein said amidine is 1,5-diaza-bicyclo[5.4.0]-undec-5-ene.
Claim 7
Dependent Claim
19 words
The process of claim 1 wherein said tertiary amine is [Me 2 N(CH 2 ) 3 ] 3 N.
Claim 8
Dependent Claim
19 words
The process of claim 1 wherein said tertiary amine is [Me 2 N(CH 2 ) 3 ] 2 NMe.
Claim 9
Dependent Claim
20 words
The process of claim 1 wherein said tertiary amine salt is [Me 2 N(CH 2 ) 3 ] 2 NMe.formate.
Claim 10
Dependent Claim
21 words
The process of claim 1 wherein said tertiary amine salt is [Me 2 N(CH 2 ) 3 ] 2 NMe phenolate.
Claim 11
Dependent Claim
27 words
The process of claim 1 wherein an optional tin catalyst is added to the reaction mixture at a level of 10-50 weight percent of said amine salt.
Claim 12
Dependent Claim
106 words
The process of making a rigid cellular polyurethane from one molar equivalent of a polyol which is prepared by reacting a phenol and formaldehyde under substantially anhydrous conditions with continuous removal of water and said polyol having a water content of no more than about 5% and having at least four phenyl groups per mole, and 0.95 to 1.25 molar equivalents of a polyisocyanate, in the presence of 0.001-0.05 molar equivalents of a fully neutralized tertiary amine salt, 0.5-5.0% of benzyl butyl phthalate, 0.5-4.0% of a surfactant and 0.4-40% of a blowing agent, said percentage figures being taken as a weight-by-weight amount based on said polyol.
Claim 13
Dependent Claim
106 words
The process of making a rigid cellular polyurethane from one molar equivalent of a polyol which is prepared by reacting a phenol and formaldehyde under substantially anhydrous conditions with continuous removal of water and said polyol having a water content of no more than about 5% and having at least four phenyl groups per mole, and 0.95 to 1.25 molar equivalents of a polyisocyanate, in the presence of 0.001-0.05 molar equivalents of a fully neutralized tertiary amine salt, 0.5-5.0% of benzyl butyl phthalate, 0.5-4.0% of a surfactant and 0.4-40% of a blowing agent, said percentage figures being taken as a weight-by-weight amount based on said polyol.
Claim 14
Dependent Claim
26 words
The process of claim 11 wherein said tertiary amine salt is present in an amount of between 0.001 and 0.01 molar equivalents based on said polyol.
Claim 15
Dependent Claim
21 words
The process of claim 12 wherein said salt contains as the acid portion an organic acid with a pKa of >3.0.
Claim 16
Dependent Claim
13 words
The process of claim 11 wherein said tertiary amine is a bicyclic amidine.
Claim 17
Dependent Claim
10 words
The process of claim 14 wherein said amidine is 1,5-diaza-bicyclo[5.4.0]-undec-5-ene.
Claim 18
Dependent Claim
19 words
The process of claim 11 wherein said tertiary amine is [Me 2 N(CH 2 ) 3 ] 3 N.
Claim 19
Dependent Claim
19 words
The process of claim 11 wherein said tertiary amine is [Me 2 N(CH 2 ) 3 ] 2 NMe.
Claim 20
Dependent Claim
21 words
The process of claim 11 wherein said tertiary amine salt is [Me 2 N(CH 2 ) 3 ] 2 NMe formate.
Claim 21
Dependent Claim
21 words
The process of claim 11 wherein said tertiary amine salt is [Me 2 N(CH 2 ) 3 ] 2 NMe phenolate.
Claim 22
Dependent Claim
27 words
The process of claim 11 wherein an optional tin catalyst is added to the reaction mixture at a level of 10-50 weight percent of said amine salt.
Claim 23
Dependent Claim
52 words
A composition for use in the manufacture of cellular, rigid polyurethane foams containing 10-30 parts of a tertiary amine salt wherein for each tertiary amine site there is a molar equivalent of an organic acid present with a pKa>3.0, 90-70 parts of butyl benzyl phthalate and 0-10 parts of a tin catalyst.
Claim 24
Dependent Claim
52 words
A composition for use in the manufacture of cellular, rigid polyurethane foams containing 10-30 parts of a tertiary amine salt wherein for each tertiary amine site there is a molar equivalent of an organic acid present with a pKa>3.0, 90-70 parts of butyl benzyl phthalate and 0-10 parts of a tin catalyst.
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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) | 1984-10-05 | 1985-04-06 | 1985-10-06 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-10-05 | 1989-04-06 | 1989-10-06 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-10-05 | 1993-04-06 | 1993-10-06 | $7700.00 | Window Closed / Lapsed |