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Recycling and treatment technology for hydroxylamine hydrochloride mother liquor

A technology for the recovery and treatment of hydroxylamine hydrochloride mother liquor, which is applied in the direction of hydroxylamine, nitrogen and non-metallic compounds, etc., can solve the problems of difficult storage and difficult treatment of hydroxylamine hydrochloride mother liquor, and achieve the effect of reducing waste discharge and solving environmental pollution problems

Inactive Publication Date: 2016-01-27
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 recovery treatment process for hydroxylamine hydrochloride mother liquor, which solves the problems of difficult storage and difficult handling of hydroxylamine hydrochloride mother liquor, and has the characteristics of simple process route, high product purity and no environmental pollution

Method used

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  • Recycling and treatment technology for hydroxylamine hydrochloride mother liquor
  • Recycling and treatment technology for hydroxylamine hydrochloride mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 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 recycling process of hydroxylamine hydrochloride mother liquor is as follows:

[0030] (1) Oximation:

[0031] 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;

[0032] (2) Pur...

Embodiment 2

[0039] 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 recycling process of hydroxylamine hydrochloride mother liquor is as follows:

[0040] (1) Oximation:

[0041] 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 reactor that has added water in advance and stir, heat up, drip concentration is the ammoniacal liquor of 25wt%, in Carry out the reaction at 50°C, control the pH value at the end of the reaction to 3.5, and then continue the heat preservation reaction for 1.2h to obtain a reaction solution containing butanone oxime, hydrazone and ammonium chloride;

[0042] (2) Purification:

[0043]...

Embodiment 3

[0049] 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 recycling process of hydroxylamine hydrochloride mother liquor is as follows:

[0050] (1) Oximation:

[0051]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;

[0052] (2) Purif...

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Abstract

The invention relates to a recycling and treatment technology for hydroxylamine hydrochloride mother liquor, and belongs to the technical field of chemical engineering waste liquor treatment. The recycling and treatment technology includes the steps that the hydroxylamine hydrochloride mother liquor, ketone and water are added into an oximation reaction kettle, ammonium hydroxide is dropwise added to conduct an oximation reaction, oxime, hydrazone and ammonium salt are obtained, an organic phase containing oxime and hydrazone is obtained after standing and layering, acidification washing is performed on the organic phase through acid liquor, a hydrazonium salt solution is separated out after standing and layering, the hydrazonium salt solution and the ammonium salt are mixed and subjected to aftertreatment, a product obtained after separation is distilled to remove residual hydrazonium salt and ammonium salt in the product, oxime is obtained, hydrolysis and acidification are performed on oxime finally, and after concentration and purification, solid hydroxylamine salt is obtained. The recycling and treatment technology solves the problem that the hydroxylamine hydrochloride mother liquor is difficult to store and treat, the purpose of making waste profitable is achieved by converting and recycling the hydroxylamine hydrochloride mother liquor, no three waste discharge exists in the technological process, and the recycling and treatment technology has the advantages of environmental friendliness and safety.

Description

technical field [0001] The invention relates to a recovery and treatment process of hydroxylamine hydrochloride mother liquor, belonging to the technical field of chemical waste liquid treatment. Background technique [0002] Hydroxylamine hydrochloride, whose appearance is colorless needle crystal, is an important chemical raw material for organic synthesis, and is mainly used as a pharmaceutical intermediate in the pharmaceutical industry. Present domestic production technology all adopts nitromethane and hydrochloric acid hydrolysis to produce hydroxylamine hydrochloride, when product is carried out concentration and purification, sucking and filtering mother liquor will be applied mechanically repeatedly, and the by-product that produces in the hydrolysis reaction also accumulates thereupon, causes the hydroxylamine hydrochloride The quality is affected, so the mother liquor of hydroxylamine hydrochloride needs to be discharged regularly. At the same time, the product de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/14
Inventor 韩己强高源候诗东张纪军
Owner SHANDONG XINGHUI CHEM
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