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Preparation method of hydroxylammonium chloride

A technology of hydroxylamine hydrochloride and hydrochloride, applied in the directions of hydroxylamine, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of increasing production cost and the amount of three wastes, large output, uneconomical, etc., and achieves reduction of costs and the amount of three wastes and costs. Low, good product quality effect

Inactive Publication Date: 2016-07-20
JUHUA GROUP TECH CENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the process of preparing methyl tributylketoxime silane, methyl trichlorosilane and butanone oxime are used as raw materials to react, and butanone oxime hydrochloride will be generated while methyl tributylketoxime silane is produced. , and the output of butanone oxime hydrochloride is relatively large and has no other uses. Treatment and recycling will increase production costs and the amount of three wastes, which is neither economical nor environmentally friendly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Get the by-product butanone oxime hydrochloride 122g of producing methyl tributanone oxime base silane, water 144g (the mol ratio of butanone oxime hydrochloride and water is 1:8), join in belt stirring, thermometer and condensing tube In a 500ml reactor, start stirring, heat up to 70°C for hydrolysis reaction, and after 7 hours of reaction, concentrate and crystallize under reduced pressure to obtain 68.06g of hydroxylamine hydrochloride, with a yield of 97.9%, and a product purity of hydroxylamine hydrochloride of 99.7%.

Embodiment 2

[0022] Get the by-product butanone oxime hydrochloride 122g of producing methyl tributanone oxime base silane, water 270g (the mol ratio of butanone oxime hydrochloride and water is 1:15), join in belt stirring, thermometer and condensing tube In a 500ml reactor, start stirring, heat up to 80°C for hydrolysis reaction, after 4 hours of reaction, concentrate and crystallize under reduced pressure to obtain 67.99g of hydroxylamine hydrochloride with a yield of 97.8%, and a product purity of hydroxylamine hydrochloride of 99.8%.

Embodiment 3

[0024] Get the by-product butanone oxime hydrochloride 122g of producing methyl tributanone oxime base silane, water 198g (the mol ratio of butanone oxime hydrochloride and water is 1:11), join in belt stirring, thermometer and condensing tube In a 500ml reactor, start stirring, heat up to 100°C for hydrolysis reaction, after reaction for 3 hours, concentrate and crystallize under reduced pressure to obtain 68.48g of hydroxylamine hydrochloride, with a yield of 98.5%, and a product purity of hydroxylamine hydrochloride of 99.8%.

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Abstract

The invention discloses a preparation method of hydroxylammonium chloride. The hydroxylammonium chloride is prepared by taking diacetylmonoxime hydrochloride and water as raw materials to react. The preparation method of the hydroxylammonium chloride has the advantages of simple process, moderate reaction conditions, low cost, and environmental friendless.

Description

technical field [0001] The invention relates to a preparation method of hydroxylamine salt, in particular to a preparation method of hydroxylamine hydrochloride. Background technique [0002] Hydroxylamine hydrochloride is an important chemical raw material and an organic synthesis intermediate with a wide range of uses. Hydroxylamine hydrochloride is mainly used as reducing agent and imaging agents, also used as synthetic anticancer drugs, sulfonamides and pesticide raw materials. Hydroxylamine hydrochloride in Organic Synthesis It is used in the preparation of oxime in the pharmaceutical industry, as an intermediate of sulfamethoxazole in the pharmaceutical industry, in the preparation of isatin intermediate in the synthetic dye industry, and in the oil industry as a fatty acid and Soap anti-aging agent, antioxidant. [0003] Patent CN101497433A discloses a preparation method of hydroxylamine salt. In the rectification tower, ketoxime is hydrolyzed in an acid solut...

Claims

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Application Information

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IPC IPC(8): C01B21/14
CPCC01B21/1409C01P2006/80
Inventor 张万宏陈幼坚周强李宏峰王彤
Owner JUHUA GROUP TECH CENT
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