Claims
- 1. A process for producing a phosphonitrilate polymer suitable for fire retarding cellulosic materials, said process comprising reacting, in the presence of an amount of an acid acceptor sufficient to complex with at least twice the molar amount of hydrogen halide formed, a phosphonitrilic halide with a hydroxyl compound selected from aliphatic alcohols having from 1 to about 6 carbon atoms and aromatic alcohols having from 6 to about 10 carbon atoms according to the steps of:
- a. contacting a mixture of said phosphonitrilic halide and said acid acceptor with from at least about 85 to about 180 weight percent of the theoretical amount based on said phosphonitrilic halide of said hydroxyl compound at a temperature of not more than about 40.degree.C, whereby a relatively low concentration of said hydroxyl compound is present during the initial 1/2 to about 3 hours of the reaction and whereby condensation occurs between intermediate phosphonitrilate alkoxy or aryloxy ester species and phosphonitrilic halides or partially esterified phosphonitrilates with the evolution of an alkyl or aryl halide compound, and
- b. thereafter, maintaining the reaction mixture at a temperature of from about 20.degree. to about 50.degree.C for a period of from about 1/2 to about 120 hours.
- 2. A phosphonitrilate polymer prepared according to the process of claim 1.
- 3. The process of claim 1 wherein said acid acceptor is a tertiary amine.
- 4. The process of claim 1 wherein said hydroxyl compound is selected from propanol and phenol.
- 5. The process of claim 1 wherein said contacting is effected by adding from about 98 to about 130 weight percent of the theoretical amount of said hydroxyl compound to said phosphonitrilic halide.
- 6. The process of claim 1 wherein said contacting is effected at a temperature of from about 20.degree. to about 30.degree.C.
- 7. The process of clam 1 wherein said acid acceptor is pyridine.
- 8. The process of claim 1 wherein said reaction mixture is maintained in said step (b) at a temperature of from about 20.degree.to about 40.degree.C.
- 9. The process of claim 1 wherein said reaction mixture is maintained in said step (b) at a temperature of from about 20.degree.to about 40.degree.C for a period of from about 1/2 to about 24 hours.
- 10. The process of claim 1 wherein after said step (b), said reaction mixture is further heated to a temperature of from about 40.degree. to about 80.degree.C for a period of about 1/2 to about 81/2hours.
- 11. The process of claim 1 wherein aid acid acceptor is pyridine and said hydroxyl compound is propanol.
- 12. The process of claim 1 wherein said acid acceptor is pyridine and said hydroxyl compound is propanol and the contacting is effected by adding from about 98 to about 130 weight percent of the theoretical amount of said propanol based on the amount of said phosphonitrilic halide to said phosphonitrilic halide.
- 13. The process of claim 1 wherein said acid acceptor is pyridine and said hydroxyl compound is propanol and said phosphonitrilic halide is a phosphonitrilic chloride and said propanol is contacted with said phosphonitrilic chloride by adding from about 98 to about 130 weight percent of the theoretical amount of said propanol to a mixture of said phosphonitrilic chloride and pyridine at a temperature of from about 20.degree. to about 30.degree.C over a period of from about 1 to about 3 hours, maintaining the reaction mixture at a temperature of from about 20.degree. to about 30.degree.C for a period of from about 1 to about 2 hours and then further heating said reaction mixture at a temperature of from about 50.degree. to about 55.degree.C for a period of from about 1/2 to about 8 hours.
- 14. The process of claim 1 wherein said reaction mixture is maintained at a temperature of from about 20.degree. to about 40.degree.C for a period of from about 1/2 to about 24 hours and said acid acceptor is pyridine and said hydroxyl compound is propanol.
- 15. The process of claim 1 wherein said acid acceptor is pyridine and said hydroxyl compound is propanol and said reaction mixture is maintained at a temperature of from about 20.degree. to about 40.degree.C for a period of from about 1/2 to about 24 hours and after said step (b), said reaction mixture is further heated to a temperature of from about 40.degree. to about 80.degree.C for a period of about 1/2to about 81/2 hours.
Parent Case Info
This application is a continuation-in-part of application Ser. No. 369,171, filed June 12, 1973, now abandoned.
US Referenced Citations (2)
Number |
Name |
Date |
Kind |
2214769 |
Lipkin |
Sep 1940 |
|
3845167 |
Franko-Filipasic et al. |
Oct 1974 |
|
Continuation in Parts (1)
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Number |
Date |
Country |
Parent |
369171 |
Jun 1973 |
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