US4522798A
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Halophosphazene polymers
Assignee: Ethyl Corp
•
Filing: 1983-09-08
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Granted: 1985-06-11
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Expires: 2003-09-08
Abstract
Abstract A mixture of compounds of the formulas: [X--(PX.sub.2 ═N).sub.n --PX.sub.3 ].sup.+ [R].sup.- and X--(PX.sub.2 ═N).sub.n --POX.sub.2 wherein X is a halogen atom, R is X or PX 6 or both of them, and n is an integer, usually below about 15, is heated either with no other reactant or with a suitable phosphorus reactant such as PX 5 ; PX 3 +X 2 ; P+X 2 ; or a mixture of two or more such phosphorus reactants so that a halophosphazene having a --PX 3 + end group is formed as one of the co-products of the reaction. This co-product is a substance having the general formula [X--(PX.sub.2 ═N).sub.n --PX.sub.3 ].sup.+ [R].sup.- wherein X, R and n are as defined above. The other co-product is phosphoryl trihalide, POX 3 . In a second stage the resultant reaction product is heated with at least a stoichiometric amount (preferably, an excess) of a nitrogen source (e.g., NH 3 ; NH 4 Cl; etc.) so that hydrogen halide is evolved and halophosphazene polymer of a suitably high molecular weight is formed. By freeing the initial mixture of the --POX 2 end group, the polymer formed in the second stage has greater linearity (less cross-linking) and reduced gel-forming tendencies.
Inventors
- 👤 Genevieve S. Lum
- 👤 Hsueh M. Li
- 👤 F. Alexander Pettigrew
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-05 19:32
CPC Classifications
C; C01; C01B; C01B21/00; C01B21/082; C01B21/097; C01B21/098; C01B21/0986
Claims Analysis
Total Claims: 24
Claim 1
Independent Claim
79 words
In a process wherein halophosphazene polymer is produced by heating halophosphazene composed at least predominantly of linear halophosphazene of lower molecular weight with at least a stoichiometric amount of a nitrogen source so that hydrogen halide is evolved and halophosphazene polymer of higher molecular weight is formed, the improvement in which the halophosphazene of lower molecular weight is substantially freed of --POX 2 end groups (X being a halogen atom) before forming the halophosphazene polymer of higher molecular weight.
Claim 2
Dependent Claim
79 words
In a process wherein halophosphazene polymer is produced by heating halophosphazene composed at least predominantly of linear halophosphazene of lower molecular weight with at least a stoichiometric amount of a nitrogen source so that hydrogen halide is evolved and halophosphazene polymer of higher molecular weight is formed, the improvement in which the halophosphazene of lower molecular weight is substantially freed of --POX 2 end groups (X being a halogen atom) before forming the halophosphazene polymer of higher molecular weight.
Claim 3
Dependent Claim
74 words
The process of claim 1 wherein the halophosphazene of lower molecular weight is composed at least predominantly of oligomer of the formula [X-(PX.sub.2 ═N).sub.n -PX.sub.3 ].sup.+ [R].sup.- wherein X is a halogen atom, R is X or PX 6 or both of them, and n is an integer below about 15, said halophosphazene of lower molecular weight also including oligomer of the formula X-(PX.sub.2 ═N).sub.n -POX.sub.2 wherein X and n are as defined above.
Claim 4
Dependent Claim
79 words
In a process wherein halophosphazene polymer is produced by heating halophosphazene composed at least predominantly of linear halophosphazene of lower molecular weight with at least a stoichiometric amount of a nitrogen source so that hydrogen halide is evolved and halophosphazene polymer of higher molecular weight is formed, the improvement in which the halophosphazene of lower molecular weight is treated to remove --POX 2 end groups (X being a halogen atom) before forming the halophosphazene polymer of higher molecular weight.
Claim 5
Dependent Claim
79 words
In a process wherein halophosphazene polymer is produced by heating halophosphazene composed at least predominantly of linear halophosphazene of lower molecular weight with at least a stoichiometric amount of a nitrogen source so that hydrogen halide is evolved and halophosphazene polymer of higher molecular weight is formed, the improvement in which the halophosphazene of lower molecular weight is treated to remove --POX 2 end groups (X being a halogen atom) before forming the halophosphazene polymer of higher molecular weight.
Claim 6
Dependent Claim
74 words
The process of claim 3 wherein the halophosphazene of lower molecular weight is composed at least predominantly of oligomer of the formula [X-(PX.sub.2 ═N).sub.n -PX.sub.3 ].sup.+ [R].sup.- wherein X is a halogen atom, R is X or PX 6 or both of them, and n is an integer below about 15, said halophosphazene of lower molecular weight also including oligomer of the formula X-(PX.sub.2 ═N).sub.n -POX.sub.2 wherein X and n are as defined above.
Claim 7
Dependent Claim
26 words
The process of claim 3 wherein the treatment to remove the --POX 2 end groups comprises heating the halophosphazene of lower molecular weight with phosphorus pentahalide.
Claim 8
Dependent Claim
47 words
The process of claim 3 wherein the treatment to remove the --POX 2 end groups comprises heating the halophosphazene of lower molecular weight to a temperature high enough to cause such --POX 2 end groups to be transformed in situ to the --PX 3 + end group.
Claim 9
Dependent Claim
74 words
In a process wherein chlorophosphazene polymer is produced by heating chlorophosphazene composed at least predominantly of linear chlorophosphazene of lower molecular weight with at least a stoichiometric amount of a nitrogen source so that hydrogen chloride is evolved and chlorophosphazene polymer of higher molecular weight is formed, the improvement in which the chlorophosphazene of lower molecular weight is substantially freed of --POCl 2 end groups before forming the chlorophosphazene polymer of higher molecular weight.
Claim 10
Dependent Claim
74 words
In a process wherein chlorophosphazene polymer is produced by heating chlorophosphazene composed at least predominantly of linear chlorophosphazene of lower molecular weight with at least a stoichiometric amount of a nitrogen source so that hydrogen chloride is evolved and chlorophosphazene polymer of higher molecular weight is formed, the improvement in which the chlorophosphazene of lower molecular weight is substantially freed of --POCl 2 end groups before forming the chlorophosphazene polymer of higher molecular weight.
Claim 11
Dependent Claim
67 words
The process of claim 7 wherein the chlorophosphazene of lower molecular weight is composed at least predominantly of oligomer of the formula [Cl-(PCl.sub.2 ═N).sub.n -PCl.sub.3 ].sup.+ [R].sup.- wherein R is Cl or PCl 6 or both of them, and n is an integer below about 15, said chlorophosphazene of lower molecular weight also including oligomer of the formula Cl-(PCl.sub.2 ═N).sub.n -POCl.sub.2 wherein n is as defined above.
Claim 12
Dependent Claim
14 words
The process of claim 8 wherein R is at least predominantly PCl 6 .
Claim 13
Dependent Claim
74 words
In a process wherein chlorophosphazene polymer is produced by heating chlorophosphazene composed at least predominantly of linear chlorophosphazene of lower molecular weight with at least a stoichiometric amount of a nitrogen source so that hydrogen chloride is evolved and chlorophosphazene polymer of higher molecular weight is formed, the improvement in which the chlorophosphazene of lower molecular weight is treated to remove --POCl 2 end groups before forming the chlorophosphazene polymer of higher molecular weight.
Claim 14
Dependent Claim
74 words
In a process wherein chlorophosphazene polymer is produced by heating chlorophosphazene composed at least predominantly of linear chlorophosphazene of lower molecular weight with at least a stoichiometric amount of a nitrogen source so that hydrogen chloride is evolved and chlorophosphazene polymer of higher molecular weight is formed, the improvement in which the chlorophosphazene of lower molecular weight is treated to remove --POCl 2 end groups before forming the chlorophosphazene polymer of higher molecular weight.
Claim 15
Dependent Claim
67 words
The process of claim 10 wherein the chlorophosphazene of lower molecular weight is composed at least predominantly of oligomer of the formula [Cl-(PCl.sub.2 ═N).sub.n -PCl.sub.3 ].sup.+ [R].sup.- wherein R is Cl or PCl 6 or both of them, and n is an integer below about 15, said chlorophosphazene of lower molecular weight also including oligomer of the formula Cl-(PCl.sub.2 ═N).sub.n -POCl.sub.2 wherein n is as defined above.
Claim 16
Dependent Claim
14 words
The process of claim 11 wherein R is at least predominantly PCl 6 .
Claim 17
Dependent Claim
26 words
The process of claim 12 wherein the treatment to remove the --POCl 2 end groups comprises heating the chlorophosphazene of lower molecular weight with phosphorus pentachloride.
Claim 18
Dependent Claim
47 words
The process of claim 12 wherein the treatment to remove the --POCl 2 end groups comprises heating the chlorophosphazene of lower molecular weight to a temperature high enough to cause such --POCl 2 end groups to be transformed in situ to the --PX 3 + end group.
Claim 19
Dependent Claim
57 words
A process for removing the --POX 2 end group from an oligomer of the formula: X-(PX.sub.2 ═N).sub.n -POX.sub.2 wherein X is a halogen atom and n is an integer below about 15 which comprises heating the oligomer with a phosphorus pentahalide to a temperature at which the oligomer is essentially freed of the --POX 2 end group.
Claim 20
Dependent Claim
57 words
A process for removing the --POX 2 end group from an oligomer of the formula: X-(PX.sub.2 ═N).sub.n -POX.sub.2 wherein X is a halogen atom and n is an integer below about 15 which comprises heating the oligomer with a phosphorus pentahalide to a temperature at which the oligomer is essentially freed of the --POX 2 end group.
Claim 21
Dependent Claim
11 words
The process of claim 15 wherein X is a chlorine atom.
Claim 22
Dependent Claim
91 words
A process for removing the --POX 2 end group from an oligomer of the formula: X-(PX.sub.2 ═N).sub.n -POX.sub.2 wherein X is a halogen atom and n is an integer below about 15 which comprises heating the oligomer with at least one phosphorus compound of the formula: [X-(PX.sub.2 ═N).sub.n -PX.sub.3 ].sup.+ [R].sup.- wherein X is a halogen atom, R is X or PX 6 or both of them, and n is an integer below about 15, to a temperature at which the oligomer is essentially freed of the --POX 2 end group.
Claim 23
Dependent Claim
91 words
A process for removing the --POX 2 end group from an oligomer of the formula: X-(PX.sub.2 ═N).sub.n -POX.sub.2 wherein X is a halogen atom and n is an integer below about 15 which comprises heating the oligomer with at least one phosphorus compound of the formula: [X-(PX.sub.2 ═N).sub.n -PX.sub.3 ].sup.+ [R].sup.- wherein X is a halogen atom, R is X or PX 6 or both of them, and n is an integer below about 15, to a temperature at which the oligomer is essentially freed of the --POX 2 end group.
Claim 24
Dependent Claim
11 words
The process of claim 17 wherein X is a chlorine atom.
References Cited (Backward Citations)
CA572951A
Cited
US4374815A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1988-06-10 | 1988-12-10 | 1989-06-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-06-10 | 1992-12-10 | 1993-06-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-06-10 | 1996-12-10 | 1997-06-11 | $7700.00 | Window Closed / Lapsed |