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Process for preparing hydroxylamine hydrochloride by adopting oxime acidolysis method

A technology for hydroxylamine hydrochloride and oximic acid is applied in the directions of oxime preparation, hydrolysis to prepare carbonyl compounds and hydroxylamine, etc., can solve problems such as high cost, harm the environment, uneconomical and the like, achieve less pollution, improve product yield and quality, and reduce production cost effect

Inactive Publication Date: 2017-12-29
临沭县华盛化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current industrial production methods of hydroxylamine salts all have deficiencies: either the cost is high, or the environment is seriously endangered
For a long time, cyclohexanone oxime and methyl ethyl ketone oxime have been prepared from hydroxylamine salt in industry, so the process of preparing hydroxylamine salt from cyclohexanone oxime and methyl ethyl ketone oxime through reverse reaction is easy to be taken for granted as uneconomical

Method used

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  • Process for preparing hydroxylamine hydrochloride by adopting oxime acidolysis method
  • Process for preparing hydroxylamine hydrochloride by adopting oxime acidolysis method

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Experimental program
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Effect test

Embodiment 1

[0030] Adopt the technology of oxime hydrolysis method to prepare hydroxylamine hydrochloride, it may further comprise the steps:

[0031] The process uses methyl ethyl ketone oxime and hydrochloric acid as raw materials, applies pervaporation-reaction coupling technology, and adopts oxime hydrolysis process to prepare hydroxylamine hydrochloride. It mainly includes raw material buffer configuration process, acid hydrolysis reaction process, ketoxime rectification process, dehydration and drying process, Ethanol recovery process, acetaldehyde oximation process and other sections.

[0032] Step a) Raw material buffer preparation process

[0033] The hydrochloric acid flows out from the storage tank and is pressurized by the pump, then enters the preparation tank, and is mixed with the recovered acid water to make a certain proportion of hydrochloric acid; after being heated by the heat exchanger through the pump, it enters the acidolysis kettle; Methyl ethyl ketone oxime enters...

Embodiment 2

[0046] The present invention investigates the effects of factors such as ketoxime type, feeding method, material ratio, material concentration, reaction temperature, and reaction time on the preparation of hydroxylamine hydrochloride by hydrolysis of ketoxime under normal pressure.

[0047] 1. Data analysis of the experimental process of the reaction behavior of hydroxylamine hydrochloride prepared by hydrolysis of oxime

[0048] ① Ketoxime selection

[0049] Hydrochloric acid with a mass concentration of 15% was prepared, and a certain amount of methyl ethyl ketone oxime and cyclohexanone oxime were weighed and reacted with hydrochloric acid at 80° C. at normal pressure for 1 hour. h + The molar ratio to ketoxime is 1.5. After the reaction, the conversion rate of ketoxime and the selectivity of hydroxylamine hydrochloride were analyzed and calculated, and the results are shown in Table 1 below.

[0050] Table 1 The reaction results of different ketoximes and hydrochloric a...

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Abstract

The invention belongs to the technical field of hydroxylamine hydrochloride, and discloses a process for preparing hydroxylamine hydrochloride by adopting an oxime acidolysis method. The method comprises the following steps: a) a raw material cache configuration process; b) an acidolysis reaction process; c) a ketoxime rectification process; d) a dehydration and drying process; e) an alcohol recycling process; and f) an acetaldehyde oximation process. By adopting the process, the process route and technical parameters of hydroxylamine hydrochloride production by methyl ethyl ketone acidolysis are optimized, a pervaporation coupling technology is applied, the product yield and quality can be improved, further improvement of the industrial technology is promoted, related industries can be driven to develop, and resource reasonable utilization can be realized.

Description

technical field [0001] The invention belongs to the technical field of preparing hydroxylamine hydrochloride, and in particular relates to a process for preparing hydroxylamine hydrochloride by adopting an oxime hydrolysis method. Background technique [0002] Hydroxylamine hydrochloride, white needle-like crystal, melting point 152°C (decomposition), specific gravity 1.67. Soluble in water, soluble in ethanol, glycerol, insoluble in ether. It is easy to absorb moisture, decomposes gradually after being exposed to moisture, and is corrosive. It is an important intermediate in organic synthesis, used as an analytical reagent and reducing agent, also used in organic synthesis and color film printing, and used as a raw material for medicine and organic synthesis. , Used as a reducing agent and developer, etc. and used for color photography and film printing. In the pharmaceutical industry, it is used as an intermediate for the production of sulfamethoxazole and as a raw mater...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/14C07C45/42C07C49/10C07C251/38C07C249/04C07C31/08C07C29/80
CPCC01B21/1454C07C29/80C07C45/42C07C249/04C07C49/10C07C251/38C07C31/08
Inventor 孙承权刘厚华袁永清
Owner 临沭县华盛化工有限公司
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