Preparation method for hydroxylammonium chloride

A technology for chlorinating hydroxylamine and hydrochloride, applied in the directions of hydroxylamine, nitrogen and non-metallic compounds, can solve the problems of high production cost, unfavorable production system water balance, large sewage discharge, etc., so as to reduce treatment costs and reduce sewage. Emission, acid cost saving effect

Inactive Publication Date: 2016-02-10
余立新
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the raw materials used in the preparation of hydroxylamine chloride are limited to ketoxime, and hydrochloric acid is required for hydrolysis. Due to the limitation of hydrochloric acid concentration, it contains a certain amount of water, which is not conducive to the water balance of the production system.
Therefore, the production cost of this method is relatively high, and the amount of sewage discharge is large

Method used

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  • Preparation method for hydroxylammonium chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 123.5g butanone oxime hydrochloride (1mol) into the mixer, then add 360g (20mol) of desalted water at a certain speed to fully mix, feed the material from the feed port in the rectification tower, and open the valve connected to the vacuum pump port. Vacuum pump, so that the vacuum degree in the tower is controlled at 0.05MPa, the temperature in the rectification tower is controlled at 70-110°C, the reflux ratio in the tower is 4, the liquid in the tank is partially circulated, and the butanone produced is passed through the cooler from the top of the tower in time Drained, part of the still liquid was cooled and crystallized in a crystallization tank, filtered and dried to obtain 65 g of hydroxylamine chloride, the yield was 94%, and the titration content was 99.1%. The reaction formula is as follows:

[0032] CH 3 CH 2 (C=NOH)CH 3 ·HCl+H 2 O→(NH 2 OH)·HCl+CH 3 CH 2 (C=O)CH 3

Embodiment 2

[0034] Add 109.5g of acetone oxime hydrochloride (1mol) to the mixer, then add 360g (20mol) of desalted water and 10g of 35% hydrochloric acid at a certain speed to fully mix, and the others are the same as in Example 1, until 67g of hydroxylamine chloride is obtained. 96%, titration content 99.2%. The reaction formula is as follows:

[0035] CH 3 (C=NOH)CH 3 ·HCl+HCl+H 2 O→(NH 2 OH)·HCl+CH 3 (C=O)CH 3

Embodiment 3

[0037] Add 123.5g butanone oxime hydrochloride (1mol) and 87g butanone oxime (1mol) to the mixer, then add 720g (40mol) of desalted water and 110g of 35% hydrochloric acid at a certain speed to fully mix, and the others are the same as in Example 1 , to hydroxylamine chloride 134g, yield 96%, titration content 99.3%. The reaction formula is as follows:

[0038] CH 3 CH 2 (C=NOH)CH 3 ·HCl+CH 3 CH 2 (C=NOH)CH 3 +HCl+H 2 O→NH 2 OH)·HClCH 3 CH 2 (C=O)CH 3

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Abstract

The invention discloses a preparation method for hydroxylammonium chloride. The method comprises the following steps: in a rectifying column, subjecting a raw material, i.e., ketoxime hydrochloride, to hydrolysis reaction in an aqueous solution so as to generate hydroxylammonium chloride and ketone, discharging the ketone from the top of the rectifying column, and subjecting a hydroxylammonium chloride solution produced from the bottom of the rectifying column to cooling, crystallization and drying so as to obtain a hydroxylammonium chloride product. Compared with the prior art, the preparation method for hydroxylammonium chloride provided by the invention has the following significant advantages: (1) the byproduct ketoxime hydrochloride in the production process of ketoxime type silane is used as a raw material, so cost of treating ketoxime hydrochloride in the production process of ketoxime type silane is reduced, and acid cost of production of hydroxylammonium chloride is saved at the same time; and (2) the use of the byproduct ketoxime hydrochloride in the production process of ketoxime type silane as the raw material is favorable for circulation of process water in a production system and greatly reduces wastewater discharge of production equipment.

Description

technical field [0001] The invention relates to the field of preparation of hydroxylamine chloride, in particular to a preparation method of hydroxylamine chloride. Background technique [0002] Hydroxylamine chloride is a chemical product with a wide range of uses, mainly used as raw materials in synthetic industries such as pesticides, medicines, spices, rubber chemicals, and dyes. [0003] At present, the methods for preparing hydroxylamine chloride mainly include nitromethane hydrolysis method, natural gas (methane) nitration method, acetone oxime method, nitric oxide reduction method, ammonium disulfonate hydrolysis method and the like. [0004] The nitromethane hydrolysis method uses dimethyl sulfate and sodium nitrite as starting materials to first produce nitromethane, and then hydrolyzes nitromethane hydrochloric acid to produce hydroxylamine hydrochloride. It uses highly toxic dimethyl sulfate, and the reaction by-product is highly toxic carbon monoxide. The reac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/14
Inventor 余立新
Owner 余立新
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