Method for preparing hydroxylammonium salt

Abstract

The invention discloses a method for preparing hydroxylamine salts. Ketoxime is subjected to hydrolysis reaction in an acid solution in a rectification tower to generate the hydroxylamine salts and ketone, and the ketone generated from the top of the rectification tower is discharged in time. The method comprises the following preparation steps: firstly, taking the ketoxime and inorganic acid respectively according to the mol ratio of the ketoxime to the inorganic acid of 1:0.4-3; secondly, feeding the ketoxime and an inorganic acid aqueous solution in the first step from the middle part of the rectification tower, and controlling at reduced pressure the temperature in the tower to between 40 and 100 DEG C and the top reflux ratio to between 1 and 6; and thirdly, cooling and crystallizingthe liquor in the tower when no ketone is distilled, and filtering, washing and drying the liquor crystals to obtain hydroxylamine salt solid. The method adopts rectification technology, simplifies and shortens the technological flow, has a simple technological line and post treatment, can evaporate the ketone generated by reaction in time because the reaction and rectification are performed simultaneously, breaks through the reaction balance, is favorable for complete reaction, improves the conversion rate and the yield of the hydroxylamine salts, and guarantees the stability of the product quality because the purity of products is high.

Description

The preparation method of hydroxylamine salt technical field The invention relates to the field of preparation of hydroxylamine salts, in particular to a preparation method of hydroxylamine salts. Background technique Hydroxylamine salt is a chemical product with a wide range of uses. The main hydroxylamine salts include hydroxylamine sulfate, hydroxylamine hydrochloride, hydroxylamine nitrate, and hydroxylamine phosphate. Hydroxylamine hydrochloride is mainly used as a raw material for synthetic industries such as pharmaceuticals, spices, rubber chemicals, and dyes; hydroxylammonium sulfate and hydroxylamine phosphate are mainly used for the production of caprolactam, pesticides, and pharmaceutical industries; hydroxylamine nitrate is mainly used for the extraction of radioactive elements and the extraction of nuclear raw materials. Handling and preparation of liquid propellants. At present, the method for preparing hydroxylamine hydrochloride mainly contains nitrometha...

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Problems solved by technology

Hydroxylamine phosphate is prepared by reducing nitrate with hydrogen under the action of platinum / palladium / carbon catalyst and using phosphoric acid as a buffer. The platinum / palladium / carbon catalyst used in this process is expensive, so the production cost is high

The application document with the publication number CN101100293A "One-step preparation of hydroxylamine salt by coupling technology of oxime hydrolysis reaction and pervaporation membrane separation" describes the preparation of hydroxylamine salt by one-step method of coupling technology of oxime hydrolysis reaction and pervaporation membrane separation. The hydrolysis conversion rate can be increased to more than 80%, but the pervaporation membrane module is complex, the cost is high, and the post-treatment uses relatively toxic toluene, which is far from the actual production application

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