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Pretreatment method of hydroxylammonium chloride mother solution recovery process

A hydroxylamine hydrochloride mother and pretreatment technology, applied in the directions of oxime preparation, organic chemistry, etc., can solve the problems of difficult handling, difficult preservation of hydroxylamine hydrochloride mother liquor, etc., and achieves the effect of solving environmental pollution problems and reducing waste discharge.

Inactive Publication Date: 2016-02-03
SHANDONG XINGHUI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a pretreatment method for the recovery process of hydroxylamine hydrochloride mother liquor, which solves the problems that hydroxylamine hydrochloride mother liquor is not easy to store and handle, and has the characteristics of simple process route, high product purity and no environmental pollution

Method used

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  • Pretreatment method of hydroxylammonium chloride mother solution recovery process

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Effect test

Embodiment 1

[0023] The composition of the hydroxylamine hydrochloride mother liquor is: hydroxylamine hydrochloride accounts for 61.5wt%, hydrochloric acid accounts for 5.25wt%, ammonium chloride accounts for 19.3wt%, hydrazine salt accounts for 8.75wt%, and water accounts for 5.2wt%. The pretreatment method of hydroxylamine hydrochloride mother liquor recovery process is as follows:

[0024] (1) Oximation:

[0025] According to the mass ratio of methyl ethyl ketone, hydroxylamine hydrochloride mother liquor is the ratio of 1:1.8, 320kg butanone and 576kg hydroxylamine hydrochloride mother liquor are joined in the reaction kettle that has added water in advance and stir, heat up, drip concentration is the ammoniacal liquor of 25wt% at 45 The reaction is carried out at ℃, and the pH value at the end of the reaction is controlled to be 3.0, and then the heat preservation reaction is continued for 1 hour to obtain a reaction solution containing butanone oxime, hydrazone and ammonium chloride...

Embodiment 2

[0030] The composition of the hydroxylamine hydrochloride mother liquor is: hydroxylamine hydrochloride accounts for 61.5wt%, hydrochloric acid accounts for 5.25wt%, ammonium chloride accounts for 19.3wt%, hydrazine salt accounts for 8.75wt%, and water accounts for 5.2wt%. The pretreatment method of hydroxylamine hydrochloride mother liquor recovery process is as follows:

[0031] (1) Oximation:

[0032] According to the mass ratio of methyl ethyl ketone, hydroxylamine hydrochloride mother liquor is the ratio of 1:1.6, 320kg methyl ethyl ketone and 512kg hydroxylamine hydrochloride mother liquor are joined in the reaction kettle that has added water in advance and stir, heat up, drip concentration is the ammoniacal liquor of 25wt% at 50 The reaction was carried out at ℃, and the pH value at the end of the reaction was controlled to be 3.5, and then the heat preservation reaction was continued for 1.2 hours to obtain a reaction solution containing butanone oxime, hydrazone and ...

Embodiment 3

[0037] The composition of the hydroxylamine hydrochloride mother liquor is: hydroxylamine hydrochloride accounts for 61.5wt%, hydrochloric acid accounts for 5.25wt%, ammonium chloride accounts for 19.3wt%, hydrazine salt accounts for 8.75wt%, and water accounts for 5.2wt%. The pretreatment method of hydroxylamine hydrochloride mother liquor recovery process is as follows:

[0038] (1) Oximation:

[0039] According to the mass ratio of methyl ethyl ketone, hydroxylamine hydrochloride mother liquor is the ratio of 1:1.9, 320kg methyl ethyl ketone and 608kg hydroxylamine hydrochloride mother liquor are joined in the reaction kettle that has added water in advance and stir, heat up, drip concentration is the ammoniacal liquor of 25wt% at 55 The reaction was carried out at ℃, and the pH value at the end of the reaction was controlled to be 4.5, and then the reaction was continued for 1.5 hours to obtain a reaction solution containing butanone oxime, hydrazone and ammonium chloride;...

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Abstract

Belonging to the technical field of chemical waste liquid treatment, the invention relates to a pretreatment method of a hydroxylammonium chloride mother solution recovery process. The pretreatment method includes: adding a hydroxylammonium chloride mother solution, ketone and water into an oximation reaction kettle, then adding ammonia water dropwise to carry out oximation reaction so as to obtain oxime, hydrazone and ammonium salt, carrying out static layering to obtain an organic phase containing oxime and hydrazone, then performing acidification washing on the organic phase with acid liquid, performing static layering, then separating the hydrazine salt, and subjecting the separated product to distillation so as to obtain oxime. The method provided by the invention solves the problems of difficult storage and difficult treatment of hydroxylammonium chloride mother solution, conducts conversion recycling of the hydroxylammonium chloride mother solution, and realizes turning waste into treasure, the process has no discharge of three wastes, and has the characteristics of environmental protection and safety.

Description

technical field [0001] The invention relates to a pretreatment method of a hydroxylamine hydrochloride mother liquor recovery process, belonging to the technical field of chemical waste liquid treatment. Background technique [0002] The production processes of hydroxylamine hydrochloride mainly include Raschig oxidation, nitromethane hydrolysis and nitric oxide reduction. Domestically, nitromethane and hydrochloric acid hydrolysis are generally used to produce hydroxylamine hydrochloride. When the product is concentrated and purified, a large amount of hydroxylamine hydrochloride mother liquor will be accumulated. At the same time, a large amount of hydroxylamine hydrochloride mother liquor will be discharged during the decolorization process. This production process will produce 1000 About tons of hydroxylamine hydrochloride mother liquor. [0003] The color of hydroxylamine hydrochloride mother liquor is brown, and composition is more complicated, wherein hydroxylamine h...

Claims

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Application Information

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IPC IPC(8): C07C249/04C07C249/14C07C251/38
Inventor 韩己强高源候诗东张纪军
Owner SHANDONG XINGHUI CHEM
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