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Purification method of acetone oxime

A purification method and technology of acetone oxime, which are applied in the field of organic compound purification, can solve the problems of unsuitability for industrial production, easy decomposition of acetone oxime, complicated process, etc., and achieve the effects of easy separation, reduced decomposition and simple process

Inactive Publication Date: 2017-03-08
定州旭阳科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This purification method has high energy consumption, long steps, complicated process, acetone oxime is easy to decompose, and there is a danger of peroxide in the separation process, so it is not suitable for industrial production

Method used

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  • Purification method of acetone oxime

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] a. Extraction experiment of acetone oxime

[0021] Acetone oxime reaction solution generated by acetone ammoximation (contact acetone, ammonia gas or ammonia water, hydrogen peroxide, solvent (tert-butanol and water) and catalyst TS-1 titanium silicon molecular sieve, heat, and react under normal pressure to obtain acetone oxime reaction solution) Filtrate, the filtrate is rectified under normal pressure, the reflux ratio is 2:1, the tert-butanol distillate is 70°C~85°C, the aqueous solution in the tower is a water oxime mixture, and the oxime content is 90g / L. Extract three times with ethyl acetate of 0.5 times the volume of the water oxime mixture, the upper layer is the ethyl acetate layer, and the lower layer is the water layer. Ethyl acetate once extracted, the recovery rate of acetone oxime was 58%, the recovery rate of acetone oxime was 80% in the second extraction, and the recovery rate of acetone oxime was 90% in three extractions.

[0022] b. Rectification an...

Embodiment 2

[0025] a. Extraction experiment of acetone oxime

[0026] Acetone oxime reaction solution generated by acetone ammoximation (contact acetone, ammonia gas or ammonia water, hydrogen peroxide, solvent (tert-butanol and water) and catalyst TS-1 titanium silicon molecular sieve, heat, and react under normal pressure to obtain acetone oxime reaction solution) Filtrate, the filtrate is rectified under normal pressure, the reflux ratio is 2:1, the tert-butanol distillate is 70°C~85°C, the aqueous solution in the tower is a water oxime mixture, and the oxime content is 90g / L. Extract three times with ethyl acetate of 1.0 times the volume of the water oxime mixture, the upper layer is the ethyl acetate layer, and the lower layer is the water layer. Ethyl acetate once extracted, the recovery rate of acetone oxime was 68%, the second extraction, the recovery rate of acetone oxime was 90%, and the recovery rate of acetone oxime was 93% after three extractions.

[0027] b. Rectification a...

Embodiment 3

[0030] a. Extraction experiment of acetone oxime

[0031] The reaction of acetone oxime generated by acetone ammoximation (contacting acetone, ammonia gas or ammonia water, hydrogen peroxide, solvent (tert-butanol and water) and catalyst TS-1 titanium silicon molecular sieve, heating, and reacting at normal pressure to obtain acetone oxime reaction liquid) Liquid filtration, the filtrate is rectified under normal pressure, the reflux ratio is 2:1, the tert-butanol distillate is 70°C~85°C, the aqueous solution in the tower is a water oxime mixture, and the oxime content is 90g / L. Extract three times with ethyl acetate of 0.25 times the volume of the water oxime mixture, the upper layer is the ethyl acetate layer, and the lower layer is the water layer. Ethyl acetate once extracted, the acetone oxime recovery rate was 40%, the second extraction, the acetone oxime recovery rate was 65%, and the three extractions, the acetone oxime recovery rate was 80%.

[0032] b. Rectification...

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Abstract

The invention discloses a purification method of acetone oxime, and relates to the technical field of organic compound purification. The method comprises the steps that acetone, ammonia gas or ammonia water, hydrogen peroxide, a solvent and a catalyst make contact with one another, and an acetone ammoximation reaction is conducted to obtain an acetone oxime reaction solution, wherein the solvent is a mixture of water and an organic solvent; for the purification process, the acetone oxime reaction solution is filtered at first, a filtrate is subjected to rectification to remove the organic solvent, tower kettle water and oxime mixed liquid is extracted with an extraction agent to obtain extraction liquid, the extraction liquid is subjected to rectification, the extraction agent is rectified out, and then pure acetone oxime is rectified out, wherein the extraction agent is ethyl acetate or dichloromethane or trichloromethane or methylbenzene. The method has the advantages of being capable of obtaining the extraction agent easily, high in extraction rate, capable of separating the extraction agent easily, simple in process, low in energy consumption, mild in separation condition, high in product purity and the like.

Description

technical field [0001] The invention relates to the technical field of organic compound purification. Background technique [0002] Acetone oxime can be used as an oxygen scavenger for boilers, and has excellent characteristics such as less usage, high oxygen scavenging efficiency, no toxicity, and no environmental pollution. Acetone oxime is the best drug for subcritical boiler shutdown protection and passivation treatment, and it is also the most ideal product for replacing traditional feed water chemical oxygen scavengers such as hydrazine in medium and high pressure boiler feed water. [0003] Existing technology "Process for Oxidation of Acetone or Butanone to Produce Acetone Oxime or Butanone Oxime" (invention patent, CN200410018607.9) investigates the ammoxidation of acetone (butanone) to acetone oxime ( butanone oxime) reaction conditions. There is no purification method for acetone oxime. [0004] Patent "Acetone Ammoxidation to Acetone Oxime Process Combined wit...

Claims

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Application Information

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IPC IPC(8): C07C249/14C07C251/38
CPCC07C249/14C07C251/38
Inventor 王英其孟祥杨克明曹亚林王峰王立平张鹏
Owner 定州旭阳科技有限公司
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