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US4157425A
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Catalytic process for the preparation of phosphazene polymers
Assignee: Armstrong World Industries Inc
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Filing: 1978-04-10
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Granted: 1979-06-05
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Expires: 1998-04-10
Abstract
Abstract A process is disclosed for the catalytically-induced preparation of phosphazene polymers. Cyclic halophosphazenes are polymerized in the presence of a catalytically sufficient amount of a compound having the formula M(OR') x where M is an alkali metal or alkaline earth metal, x is equal to the valence of the metal and R' is C 1 to C 10 linear or branched alkyl, C 1 to C 10 substituted linear or branched alkyl, the substituent selected from the group consisting of nitro, C 1 to C 10 alkyl, C 1 to C 10 alkoxy, C 6 to C 10 aryl and C 6 to C 10 aryloxy, or N 3 P 3 Cl z (OR') 6-z wherein R' is as defined above and z equals 0 to 5.
Inventors
- 👤 Ronald L. Dieck
- 👤 Alan B. Magnusson
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 03:22
CPC Classifications
C; C08; C08J; C08J9/00; C08J9/04; C08J9/06; C08G; C08G79/00; C08G79/02; C08G79/025; C08L; C08L85/00; C08L85/02; C08J2385/00; C08J2385/02; Y; Y10; Y10S; Y10S260/00; Y10S260/24
Claims Analysis
Total Claims: 10
Claim 1
Independent Claim
309 words
A process for producing a phosphazene polymer foam which comprises: (a) thermally polymerizing a cyclic compound of the formula (NPCl 2 ) y wherein y is 3, 4, or mixtures thereof with a catalytically sufficient amount of a compound having the formula M(OR') x , wherein M is an alkali metal or an alkaline earth metal, x is equal to the valence of the metal M, and R' is C 1 to C 10 linear or branched alkyl, C 1 to C 10 substituted linear or branched alkyl, the substituent selected from the group consisting of nitro, C 1 to C 10 alkyl, C 1 to C 10 alkoxy, C 6 to C 10 aryl and C 6 to C 10 aryloxy radicals to form a phosphazene polymer; (b) contacting the resulting phosphazene polymer with a metal compound having the formula M(OC.sub.6 H.sub.4 R.sub.1).sub.x, M(OC.sub.6 H.sub.4 R.sub.2).sub.x, or mixtures thereof wherein M is an alkali metal or alkaline earth metal, x is equal to the valence of said metal M, and R 1 and R 2 are the same or different and are selected from the group consisting of C 1 to C 10 alkyl radical, C 6 to C 10 aryl radical, C 1 to C 10 substituted C 1 to C 10 alkyl radical and substituted C 6 to C 10 aryl radical, the substituent selected from the group consisting of halogen, nitro, cyano, C 1 to C 4 alkyl, C 1 to C 4 alkoxy, C 6 to C 10 aryl and C 6 to C 10 aryloxy radicals, thereby forming a phosphazene polymer which is substantially free of halogen; and (c) mixing the resulting phosphazene polymer which is substantially free of halogen with a chemical blowing agent and heating the resulting mixture to a temperature sufficient to decompose said blowing agent and form a foam.
Claim 2
Dependent Claim
309 words
A process for producing a phosphazene polymer foam which comprises: (a) thermally polymerizing a cyclic compound of the formula (NPCl 2 ) y wherein y is 3, 4, or mixtures thereof with a catalytically sufficient amount of a compound having the formula M(OR') x , wherein M is an alkali metal or an alkaline earth metal, x is equal to the valence of the metal M, and R' is C 1 to C 10 linear or branched alkyl, C 1 to C 10 substituted linear or branched alkyl, the substituent selected from the group consisting of nitro, C 1 to C 10 alkyl, C 1 to C 10 alkoxy, C 6 to C 10 aryl and C 6 to C 10 aryloxy radicals to form a phosphazene polymer; (b) contacting the resulting phosphazene polymer with a metal compound having the formula M(OC.sub.6 H.sub.4 R.sub.1).sub.x, M(OC.sub.6 H.sub.4 R.sub.2).sub.x, or mixtures thereof wherein M is an alkali metal or alkaline earth metal, x is equal to the valence of said metal M, and R 1 and R 2 are the same or different and are selected from the group consisting of C 1 to C 10 alkyl radical, C 6 to C 10 aryl radical, C 1 to C 10 substituted C 1 to C 10 alkyl radical and substituted C 6 to C 10 aryl radical, the substituent selected from the group consisting of halogen, nitro, cyano, C 1 to C 4 alkyl, C 1 to C 4 alkoxy, C 6 to C 10 aryl and C 6 to C 10 aryloxy radicals, thereby forming a phosphazene polymer which is substantially free of halogen; and (c) mixing the resulting phosphazene polymer which is substantially free of halogen with a chemical blowing agent and heating the resulting mixture to a temperature sufficient to decompose said blowing agent and form a foam.
Claim 3
Dependent Claim
13 words
The process in accordance with claim 1 wherein said blowing agent is 1,1'-bisazoformamide.
Claim 4
Dependent Claim
114 words
The process in accordance with claim 1 wherein said phosphazene polymer, substantially free of halogen is mixed with a chemical blowing agent and a mixture of curing agents, at least one of said curing agents having an initiation temperature below the temperature at which said chemical blowing agent decomposes; heating the foamable mass to a temperature below the decomposition temperature of said blowing agent, but above the initiation temperature of at least one of said curing agents, for a sufficient time to partially precure the copolymers; and heating the partially precured mass to a temperature above the decomposition temperature of said blowing agent to foam the copolymers and to effect a further cure thereof.
Claim 5
Dependent Claim
68 words
The process of claim 3, wherein the partial precure is accomplished by heating the foamable mass for about 6 to about 30 minutes at a temperature of from about 200° F. to about 250° F., and the foaming and further curing is accomplished by heating the partially precured mass for about 30 to about 60 minutes at a temperature of from about 300° F. to about 350° F.
Claim 6
Dependent Claim
289 words
A process for producing a phosphazene polymer foam which comprises: (a) thermally polymerizing a cyclic compound of the formula (NPCl 2 ) y where y is 3, 4, or mixtures thereof with a catalytically sufficient amount of a compound having the formula N 3 P 3 Cl z (OR') 6-z wherein R' is C 1 to C 10 linear or branched alkyl, C 1 to C 10 substituted linear or branched alkyl, the substituent selected from the group consisting of halogen, nitro, C 1 to C 10 alkyl, C 1 to C 10 alkoxy, C 6 to C 10 aryl and C 6 to C 10 aryloxy radicals and z equals 0 to 5. (b) contacting the resulting phosphazene polymer with a metal compound having the formula M(OC.sub.6 H.sub.4 R.sub.1).sub.x, M(OC.sub.6 H.sub.4 R.sub.2).sub.x, or mixtures thereof wherein M is an alkali metal or an alkaline earth metal, x is equal to the valence of said metal M, and R 1 and R 2 are the same or different and are selected from the group consisting of C 1 to C 10 alkyl radical, C 6 to C 10 aryl radical, substituted C 1 to C 10 alkyl radical and substituted C 6 to C 10 aryl radical, the substituent selected from the group consisting of halogen, nitro, cyano, C 1 to C 4 alkyl, C 1 to C 4 alkoxy, C 6 to C 10 aryl and C 6 to C 10 aryloxy radicals, thereby forming a phosphazene polymer substantially free of halogen; and (c) mixing the resulting phosphazene polymer which is substantially free of halogen with a chemical blowing agent and heating the resulting mixture to a temperature sufficient to decompose said blowing agent and form a foam.
Claim 7
Dependent Claim
289 words
A process for producing a phosphazene polymer foam which comprises: (a) thermally polymerizing a cyclic compound of the formula (NPCl 2 ) y where y is 3, 4, or mixtures thereof with a catalytically sufficient amount of a compound having the formula N 3 P 3 Cl z (OR') 6-z wherein R' is C 1 to C 10 linear or branched alkyl, C 1 to C 10 substituted linear or branched alkyl, the substituent selected from the group consisting of halogen, nitro, C 1 to C 10 alkyl, C 1 to C 10 alkoxy, C 6 to C 10 aryl and C 6 to C 10 aryloxy radicals and z equals 0 to 5. (b) contacting the resulting phosphazene polymer with a metal compound having the formula M(OC.sub.6 H.sub.4 R.sub.1).sub.x, M(OC.sub.6 H.sub.4 R.sub.2).sub.x, or mixtures thereof wherein M is an alkali metal or an alkaline earth metal, x is equal to the valence of said metal M, and R 1 and R 2 are the same or different and are selected from the group consisting of C 1 to C 10 alkyl radical, C 6 to C 10 aryl radical, substituted C 1 to C 10 alkyl radical and substituted C 6 to C 10 aryl radical, the substituent selected from the group consisting of halogen, nitro, cyano, C 1 to C 4 alkyl, C 1 to C 4 alkoxy, C 6 to C 10 aryl and C 6 to C 10 aryloxy radicals, thereby forming a phosphazene polymer substantially free of halogen; and (c) mixing the resulting phosphazene polymer which is substantially free of halogen with a chemical blowing agent and heating the resulting mixture to a temperature sufficient to decompose said blowing agent and form a foam.
Claim 8
Dependent Claim
13 words
The process in accordance with claim 5 wherein said blowing agent is 1,1'-azobisformamide.
Claim 9
Dependent Claim
114 words
The process in accordance with claim 5 wherein said phosphazene polymer, substantially free of halogen is mixed with a chemical blowing agent and a mixture of curing agents, at least one of said curing agents having an initiation temperature below the temperature at which said chemical blowing agent decomposes; heating the foamable mass to a temperature below the decomposition temperature of said blowing agent, but above the initiation temperature of at least one of said curing agents, for a sufficient time to partially precure the copolymers; and heating the partially precured mass to a temperature above the decomposition temperature of said blowing agent to foam the copolymers and to effect a further cure thereof.
Claim 10
Dependent Claim
68 words
The process of claim 6 wherein the partial precure is accomplished by heating the foamable mass for about 6 to about 30 minutes at a temperature of from about 200° F. to about 250° F., and the foaming and further curing is accomplished by heating the partially precured mass for about 30 to about 60 minutes at a temperature of from about 300° F. to about 350° F.
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) | 1982-06-04 | 1982-12-04 | 1983-06-05 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-06-04 | 1986-12-04 | 1987-06-05 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-06-04 | 1990-12-04 | 1991-06-05 | $7700.00 | Window Closed / Lapsed |