Claims
- 1. A process comprising the steps of:
- (a) reacting an alcoholic solution of a base selected from the group consisting of sodium hydroxide, potassium hydroxide, lithium hydroxide, ammonium hydroxide and the corresponding alkoxides of 1-5 carbons with solid hydroxylammonium sulfate, employing an alcohol of 1-3 carbons, a temperature, a pressure and a time sufficient to produce a liquid phase having at least 50% of the hydroxylamine values of the hydroxylammonium sulfate,
- (b) separating the solid phase comprising a sulfate salt corresponding to said base from the liquid phase, and
- (c) reacting the separated liquid phase with an acid other than sulfuric acid to produce an hydroxylammonium salt other than hydroxylammonium sulfate.
- 2. The process of claim 1 wherein said base is sodium hydroxide.
- 3. The process of claim 2 wherein the alcohol is methanol.
- 4. The process of claim 2 wherein the alcohol is ethanol.
- 5. The process of claim 2 wherein the reacting step (a) is conducted at a temperature not greater than about 30.degree. C.
- 6. The process of claim 3 wherein the reacting step (a) is conducted at a temperature not greater than about 20.degree. C.
- 7. The process of claim 6 wherein the reacting step (a) is conducted at a temperature not greater than about 10.degree. C.
- 8. The process of claim 1 wherein said base is potassium hydroxide.
- 9. The process of claim 8 wherein the alcohol is ethanol.
- 10. The process of claim 9 wherein the reacting step (a) is conducted at a temperature between about 10.degree. C. and about 40.degree. C.
- 11. The process of claim 10 wherein the reacting step (a) is conducted at a temperature between about 5.degree. C. and about 25.degree. C.
- 12. The process of claim 1 wherein said base is lithium hydroxide.
- 13. The process of claim 1 wherein said base is an alkoxide.
- 14. The process of claim 13 wherein the base is sodium methoxide and the solvent is methanol.
- 15. The process of claim 13 wherein the base is sodium ethoxide or potassium ethoxide and the solvent is ethanol.
- 16. The process of claim 1 wherein said separating step (b) comprising separating a free hydroxylamine solution in alcohol of pH between about 7 and about 12 from a solid phase comprising said sulfate salt corresponding to said base.
- 17. The process of claim 1 wherein the acid is an alkanecarboxylic or dicarboxylic acid and the product solution is an alcoholic solution of an hydroxylammonium alkanecarboxylate or dihydroxylammonium alkanedicarboxylate.
- 18. The process of claim 17 wherein said other acid is formic acid.
- 19. The process of claim 17 wherein said other acid is acetic acid.
- 20. The process of claim 17 wherein said other acid is oxalic acid.
- 21. The process of claim 1 wherein said other acid is a mineral acid.
- 22. The process of claim 21 wherein the other acid is HCl and the product solution is alcoholic hydroxylammonium chloride.
- 23. The process of claim 21 wherein said other acid is nitric acid and the product solution is an alcoholic solution of hydroxylammonium nitrate.
- 24. The process of claim 21 wherein said other acid is perchloric acid and the product solution is an alcoholic solution of hydroxylammoninum perchlorate.
- 25. A process comprising the steps of:
- (a) reacting an alcoholic solution of a base or basic organic salt selected from the group consisting of sodium hydroxide, potassium hydroxide, lithium hydroxide, ammonium hydroxide, the corresponding alkoxides of 1-5 carbons and the corresponding organic salts with solid hydroxylammonium sulfate and, in the case of base, an organic acid, in the substantial absence of adder water or water introduced with the alcohol; employing an alcohol of 1-3 carbons, a temperature not greater than about 30.degree. C., a pressure and a time sufficient to produce a liquid phase having at least 50% of the hydroxylamine values of the hydroxylammonium sulfate and a solid alkali metal or ammonium sulfate corresponding to the base or basic salt; and
- separating the solid phase comprising sulfate salt from a liquid phase containing an organic hydroxylammonium salt corresponding to said basic organic salt or organic acid, said liquid phase being substantially free of sulfate.
- 26. The process of claim 25 wherein said base is sodium hydroxide or said basic salt is a sodium salt.
- 27. The process of claim 26 wherein said alcohol is methanol.
- 28. The process of claim 27 wherein said temperature is not greater than about 20.degree. C.
- 29. The process of claim 28 wherein said temperature is not greater than about 10.degree. C.
- 30. The process of claim 28 wherein said basic salt is a sodium alkanecarboxylate, a disodium alkanedicarboxylate, sodium benzoate or sodium aryl or alkylaryl sulfonate.
DESCRIPTION
This is a continuation-in-part of U.S. 437,920, filed Nov. 1, 1982.
US Referenced Citations (7)
Foreign Referenced Citations (1)
Number |
Date |
Country |
1247284 |
Aug 1967 |
DEX |
Non-Patent Literature Citations (2)
Entry |
Feiser, Introduction to Organic Chemistry, (1957), D. C. Heath and Co., pp. 96, 97. |
Kirk-Othmer, Encyclopedia of Chemical Technology, Second Edition, (1967), Interscience Publishers, pp. 494-496, vol. 11. |
Continuation in Parts (1)
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Number |
Date |
Country |
Parent |
437920 |
Nov 1982 |
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