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Preparation method of hydroxylamine hydrochloride

A technology of hydroxylamine hydrochloride and hydrochloride, which is applied in the field of preparation of hydroxylamine hydrochloride, can solve the problems of environmental pollution, low yield, complex process, etc., and achieve the effects of cost reduction, high yield and simple process conditions

Inactive Publication Date: 2019-04-05
江苏艾科维科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Hydroxylamine hydrochloride is a colorless crystalline, deliquescent, white chemical substance, mainly used as a reducing agent and imaging agent, used to prepare oximes in organic synthesis, and also used to synthesize anticancer drugs, sulfonamides and pesticides, so hydrochloric acid Hydroxylamine is an important chemical raw material. At present, most of the methods for industrially synthesizing hydroxylamine hydrochloride have problems such as complex process, many by-products, low yield, large discharge of three wastes, and serious environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The preparation method of the hydroxylamine hydrochloride of the present embodiment may further comprise the steps:

[0022] 1) Add 122g of butanone oxime hydrochloride and 126g of water into the mixer and keep it warm at 40°C for 1 hour, and mix well to prepare the premix;

[0023] 2) Put 20g of titanium-silicon molecular sieve into the reactor, put the uniformly mixed premix in step 1) into the reactor, raise the temperature to 80°C, the reaction pressure is 50KPa, and react for 8 hours to obtain hydroxylamine hydrochloride and by-product butanone ;

[0024] 3) Transfer the hydroxylamine hydrochloride in step 2) to the crystallization tank, the temperature in the crystallization tank is controlled at 40°C, the reaction pressure is 50KPa, after crystallization for 10 hours, the solid-liquid separation after cooling, pumped into the airtight filter In the container, the solid hydroxylamine hydrochloride is separated, and the separated solid hydroxylamine hydrochloride ...

Embodiment 2

[0030] The preparation method of the hydroxylamine hydrochloride of the present embodiment may further comprise the steps:

[0031] 1) Add 122g of butanone oxime hydrochloride and 180g of water into the mixer and keep warm at 42°C, keep warm for 1.5h, and mix well to prepare the premix;

[0032] 2) Put 25g of titanium-silicon molecular sieves into the reactor, put the premixed solution uniformly mixed in step 1) into the reactor, raise the temperature to 75°C, the reaction pressure is 45KPa, and react for 7 hours to obtain hydroxylamine hydrochloride and by-product butanone ;

[0033] 3) Transfer the hydroxylamine hydrochloride in step 2) to the crystallization tank, the temperature in the crystallization tank is controlled at 38°C, the reaction pressure is 45KPa, after crystallization for 9 hours, the solid-liquid separation after cooling, pumped into the airtight filter In the container, the solid hydroxylamine hydrochloride is separated, and the separated solid hydroxylami...

Embodiment 3

[0039] The preparation method of the hydroxylamine hydrochloride of the present embodiment may further comprise the steps:

[0040] 1) Add 122g of butanone oxime hydrochloride and 288g of water into the mixer and keep warm at 45°C, keep warm for 2 hours, and mix well to prepare the premix;

[0041] 2) Put 28g of titanium-silicon molecular sieves into the reactor, put the premixed solution uniformly mixed in step 1) into the reactor, raise the temperature to 85°C, the reaction pressure is 55KPa, and react for 9 hours to obtain hydroxylamine hydrochloride and by-product butanone ;

[0042] 3) Transfer the hydroxylamine hydrochloride in step 2) to the crystallization cylinder, the temperature in the crystallization cylinder is controlled at 42°C, the reaction pressure is 55KPa, after crystallization for 11 hours, the solid-liquid separation after cooling, and pump into the airtight filter In the container, the solid hydroxylamine hydrochloride is separated, and the separated sol...

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Abstract

The invention relates to the field of preparation of hydroxylamine salt, in particular to a preparation method of hydroxylamine hydrochloride. The preparation method includes hydrolyzing a certain mass of diacetylmonoxime hydrochloride and water before crystallizing and drying, allowing generated butanone and impurities in raw materials to pass through an oil-water separator after condensation, and finally recycling the butanone and diacetylmonoxime materials through alkali wash by an alkali wash separating column and rectification by a rectifying column. The preparation method has the advantages that the diacetylmonoxime hydrochloride and the water are added into a mixer in advance for uniform mixing to facilitate thorough reaction between the diacetylmonoxime hydrochloride and the waterin later period, a catalyst is added during reaction to accelerate the reaction process, and other reaction products are recycled through tertiary condensation, the oil-water separator and the alkaliwash separating column, so that high efficiency and energy conservation are achieved, and the product yield is high.

Description

technical field [0001] The invention relates to the field of preparation of hydroxylamine salts, in particular to a preparation method of hydroxylamine hydrochloride. Background technique [0002] Hydroxylamine hydrochloride is a colorless crystalline, deliquescent, white chemical substance, mainly used as a reducing agent and imaging agent, used to prepare oximes in organic synthesis, and also used to synthesize anticancer drugs, sulfonamides and pesticides, so hydrochloric acid Hydroxylamine is an important chemical raw material. At present, most of the methods for industrially synthesizing hydroxylamine hydrochloride have problems such as complex process, many by-products, low yield, large discharge of three wastes, and serious environmental pollution. Therefore, the market needs a novel synthesis process of hydroxylamine hydrochloride with high efficiency, energy saving, high product yield and environmental friendliness. In the process of preparing methyl tributylketoxi...

Claims

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Application Information

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IPC IPC(8): C01B21/14C07C45/00C07C45/78C07C49/04
CPCC01B21/1409C07C45/00C07C45/78C07C49/04
Inventor 刘建青李鲁祯汪俊杰叶茂伟
Owner 江苏艾科维科技有限公司
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