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Method of preparing solid hydroxylamine hydrochloride

A technology of hydroxylamine hydrochloride and hydroxylamine sulfate, which is applied in the direction of hydroxylamine, nitrogen and non-metallic compounds, can solve the problems of low yield and purity of solid hydroxylamine hydrochloride, low purity and yield, etc., and is beneficial to industrial production and high product purity , the effect of high yield

Inactive Publication Date: 2006-03-29
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some use the aqueous solution of hydroxylamine sulfate produced in the production of caprolactam as a raw material, use dilute ammonia water to neutralize to obtain free hydroxylamine, then add methanol to crystallize ammonium sulfate, and add hydrochloric acid to the separated free hydroxylamine methanol aqueous solution to evaporate and crystallize to obtain the product solid Hydroxylamine hydrochloride, but the purity and yield are all low; some adopt the hydroxylamine sulfate aqueous solution produced in the production of caprolactam as raw material, and the hydroxylamine sulfate is extracted with common extraction methods, and the solid hydroxylamine hydrochloride yield and purity obtained are also low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) The raw materials of hydroxylamine sulfate aqueous solution and ammonia water were reacted at 30°C for 30 minutes, and the pH value was adjusted to 5.4, which was used as the aqueous phase of the reaction liquid;

[0035] 2) 20ml of bis(2-ethylhexyl)phosphoric acid, 55ml of kerosene, 0.02ml of trioctylphosphine oxide, and 4ml of ammonia water with a mass concentration of 33% were reacted at 30°C for 30min to make the organic phase;

[0036] 3) 45ml of the reaction liquid aqueous phase and 80ml of the organic phase were subjected to reaction extraction at 30°C for 30 minutes, and the reaction extraction was performed 5-15 times;

[0037]4) The organic phase obtained by the reaction extraction was neutralized and reacted at 30° C. for 30 minutes with 150 ml of hydroxylamine sulfate aqueous solution with a mass concentration of 50 percent;

[0038] 5) The organic phase obtained by the neutralization reaction was extracted with 15 ml of dilute hydrochloric acid with a ma...

Embodiment 2

[0040] 1) The raw materials of hydroxylamine sulfate aqueous solution and ammonia water were reacted at 30°C for 30 minutes, and the pH value was adjusted to 5.4, which was used as the aqueous phase of the reaction liquid;

[0041] 2) 20ml of di(2-ethylhexyl)phosphoric acid, 55ml of benzene, 0.02ml of trioctylphosphine oxide, and 4ml of ammonia water with a mass concentration of 33% were reacted at 30°C for 30min to make the organic phase;

[0042] 3) 45ml of the reaction liquid aqueous phase and 80ml of the organic phase were subjected to reaction extraction at 30°C for 30 minutes, and the reaction extraction was performed 5-15 times;

[0043] 4) The organic phase obtained by the reaction extraction was neutralized and reacted at 30° C. for 30 minutes with 150 ml of hydroxylamine sulfate aqueous solution with a mass concentration of 50 percent;

[0044] 5) The organic phase obtained by the neutralization reaction was extracted with 15 ml of dilute hydrochloric acid with a mas...

Embodiment 3

[0046] 1) The raw materials of hydroxylamine sulfate aqueous solution and ammonia water were reacted at 30°C for 30 minutes, and the pH value was adjusted to 5.4, which was used as the aqueous phase of the reaction liquid;

[0047] 2) 20ml of bis(2-ethylhexyl)phosphoric acid, 55ml of carbon tetrachloride, 0.02ml of trioctylphosphine oxide, and 4ml of ammonia water with a mass concentration of 33% were reacted at 30°C for 30min to make the organic phase;

[0048] 3) 45ml of the reaction liquid aqueous phase and 80ml of the organic phase were subjected to reaction extraction at 30°C for 30 minutes, and the reaction extraction was performed 5-15 times;

[0049] 4) The organic phase obtained by the reaction extraction was neutralized and reacted at 30° C. for 30 minutes with 150 ml of hydroxylamine sulfate aqueous solution with a mass concentration of 50 percent;

[0050] 5) The organic phase obtained by the neutralization reaction was extracted with 15 ml of dilute hydrochloric a...

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Abstract

A process for preparing hydroxyamine hydrochloride solid includes such steps as reaction between the aqueous solution of hydroxyamine sulfate and ammonia water, regulating pH=5.3-5.7 to obtain liquid phase, reaction between complexing agent, deluent, cosolvent and ammonia water to obtain organic phase, reaction between said liquid phase and organic phase while extracting 5-15 times to obtain organic phase, neutralizing reaction on the aqueous solution of hydroxyamine sulfate to obtain organic phase, reaction on deluted hydrochloric acid while extracting, concentrating, evaporating and crystallizing.

Description

technical field [0001] The invention relates to a method for preparing solid hydroxylamine hydrochloride. Background technique [0002] There are many methods for preparing solid hydroxylamine hydrochloride. Many large chemical companies in foreign countries use methane, the main component of natural gas, to react with nitric acid to produce nitromethane, and then treat it with hydrochloric acid to obtain hydroxylamine hydrochloride. The yield is low, there are many types of by-products, and the investment in separation equipment is large; Sodium chloroacetate and sodium nitrite are starting materials. With the popularization and use of dimethyl sulfate as a methylating agent, this method is gradually replaced, but the environmental impact is serious; in addition, the production process of the acetone oxime route is mature, but the process It is relatively complicated, and hydroxylamine must be separated in the form of acetone oxime, and there are many kinds of raw material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/14
Inventor 何潮洪刘建青朱明乔谢方友何朝阳
Owner ZHEJIANG UNIV
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