Method for preparing salt of hydroxylamine by using 'coupling' technique of reactive extraction

Abstract

This invention provides a method for preparing hydroxylamine salt by reaction-extraction 'coupled' technique. The method utilizes hydroxylamine hydrochloride and HNO3, H2SO4 or H3PO4 as the reactants to prepare hydroxylamine nitrate, hydroxylamine sulfate or hydroxylamine phosphate. During the reaction, a mixture of amide and diluting agent is utilized as the extraction phase to extract byproduct HCl generated during the reaction to obtain high-concentration hydroxylamine salt mother liquor. Then multi-stage cross-flow or vacuum distillation is performed to obtain concentrated hydroxylamine salt solution or crystal. During the reaction, byproduct inorganic acid can be extracted into the organic phase, which can reduce the amount of inorganic acid in aqueous phase, and break the previous thermodynamic equilibrium limit so that the reaction advances toward the positive reaction direction, and the yield is increased. The method has such advantages as simple process, few buproducts and easy operation, and is suitable for industrialization production.

Description

Technical field:

[0001] The invention relates to a method for preparing hydroxylamine salt by using reaction-extraction "coupling" technology, which belongs to the technical field of fine chemical products. Background technique:

[0002] Hydroxylamine salt is a fine chemical product with a wide range of uses. Hydroxylamine sulfate and hydroxylamine phosphate are mainly used in the production of caprolactam, and also have important uses in the production of pesticides and medicines; hydroxylamine nitrate is mainly used in the treatment of spent nuclear materials and liquid propellants.

[0003] At present, the methods for preparing hydroxylamine sulfate mainly include NO reduction method, acetone oximation method, calcium oxide method, hydrolysis method and so on. The methods for preparing hydroxylamine nitrate mainly include catalytic reduction method, ion exchange method, electrodialysis method, precipitation method, neutralization method, electrolysis method, double decom...