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Preparation method for acetoxime

A technology of acetone oxime and ketoxime, which is applied in the field of preparation of acetone oxime, can solve the problems of low selectivity and increased cost, and achieve the effects of high reaction conversion rate, reduced pollution, and simple reaction process

Inactive Publication Date: 2018-05-25
BEIJING RISUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method significantly reduces pollution emissions, the selectivity is not high because the titanium-silicon molecular sieve u

Method used

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  • Preparation method for acetoxime
  • Preparation method for acetoxime

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a, the synthetic reaction of acetone oxime

[0022] Add cyclohexanone oxime (Sinopharm Chemical Reagent Co., Ltd.), acetone (Sinopharm Chemical Reagent Co., Ltd.) and hydrochloric acid into the reactor according to the molar ratio of 1.0:30.0:0.3, and add water so that the pH value of the solution is 1, and the above The reaction system was heated, the reaction temperature was 30° C., the reaction time was 9 hours, and the pressure of the reaction system was normal pressure.

[0023] b, the purification of acetone oxime

[0024] After the above reaction is finished, the product obtained by rectification and purification is acetone oxime. The detection and analysis results show that the conversion rate of cyclohexanone oxime is 97.1%, and the selectivity of acetone oxime is 99.3%.

[0025] The gas chromatogram of the product is as follows figure 1 Shown: the product obtained is acetone oxime through gas chromatographic comparison with the standard product.

Embodiment 2

[0027] a, the synthetic reaction of acetone oxime

[0028] Add cyclohexanone oxime (Sinopharm Chemical Reagent Co., Ltd.), acetone (Sinopharm Chemical Reagent Co., Ltd.) and sulfuric acid into the reactor according to the molar ratio of 1.0:35:0.3, and add water so that the pH value of the solution is 2, and the above The reaction system is heated, the reaction temperature is 80° C., the reaction time is 5 hours, and the pressure of the reaction system is normal pressure.

[0029] b, the purification of acetone oxime

[0030] After the above reaction is finished, the product obtained by rectification and purification is acetone oxime. The detection and analysis results show that the conversion rate of cyclohexanone oxime is 98.2%, and the selectivity of acetone oxime is 99.2%. It was confirmed by gas chromatography that the product was acetone oxime.

Embodiment 3

[0032] a, the synthetic reaction of acetone oxime

[0033] Add cyclohexanone oxime (Sinopharm Chemical Reagent Co., Ltd.), acetone (Sinopharm Chemical Reagent Co., Ltd.) and nitric acid into the reactor according to a molar ratio of 1.0:10:0.6, and add water so that the pH value of the solution is 1, and the above The reaction system is heated, the reaction temperature is 70° C., the reaction time is 8 hours, and the pressure of the reaction system is normal pressure.

[0034] b, the purification of acetone oxime

[0035] After the above reaction is finished, the product obtained by rectification and purification is acetone oxime. The detection and analysis results show that the conversion rate of cyclohexanone oxime is 91.6%, and the selectivity of acetone oxime is 99.3%. It was confirmed by gas chromatography that the product was acetone oxime.

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Abstract

The invention relates to a preparation method for acetoxime. The preparation method comprises the following steps: a) preparation of a reaction system: adding ketoxime and acetone in a molar ratio of1.0: (5.0-35.0) into a reactor, then adding an acid catalyst and a solvent, and carrying out uniform mixing in the reactor under stirring to form the reaction system which has a pH value of 1 to 5; b)a synthetic reaction of acetoxime: heating the reaction system obtained in step a) and carrying out the reaction for 5 to 10 h with reaction temperature controlled to be 5 to 100 DEG C and a pressurecontrolled to be 0 to 2 atm; and c) purification of acetoxime: purifying a product obtained in step b) so as to obtain acetoxime. The method of the invention has the advantages of high reaction conversion rate, high acetoxime selectivity, simple reaction process, environmental friendliness, reduced environmental pollution and easy industrial production.

Description

technical field [0001] The invention relates to a method for preparing acetone oxime, in particular to a method for preparing acetone oxime through an oxime exchange reaction. The method of the invention has the advantages of low cost and no pollution. Background technique [0002] Acetone oxime, also known as dimethyl ketone oxime, is mainly used as an oxygen scavenger for boilers. Compared with traditional boiler chemical oxygen scavenger hydrazine and other substances, it has less usage, high oxygen scavenging efficiency, no toxicity, and no environmental pollution. Excellent features. 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. At the same time, acetone oxime can also be used as an intermediate of silicone crosslinking agent and a capping agent of p...

Claims

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Application Information

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IPC IPC(8): C07C249/04C07C249/14C07C251/38
CPCC07C249/04C07C249/14C07C251/38
Inventor 张英伟张敏生宋艾罗郑云孙长江
Owner BEIJING RISUN TECH CO LTD
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