Method for preparing acetaldehyde oxime

A technology for acetaldoxime and ketoxime, which is applied in the field of preparing acetaldoxime, can solve the problems of large amount of hydroxylamine salt, generation of by-products, unfriendly environment and the like, and achieves the effects of high selectivity, high conversion rate and environmental friendliness

Inactive Publication Date: 2015-05-20
BEIJING RISUN TECH CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of this production process are: complex process, long reaction process, large amount of hydroxylamine salt, alkali needs to be added to adjust the pH of the reaction system, and by-products are generated, which is not friendly to the environment

Method used

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  • Method for preparing acetaldehyde oxime
  • Method for preparing acetaldehyde oxime

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Experimental program
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Effect test

Embodiment 1

[0023] a, the synthetic reaction of acetaldehyde oxime

[0024] Butanone oxime (Zhejiang Jinhua New Materials Co., Ltd.), acetaldehyde (Tianjin Kemiou, 40% aqueous solution) and hydrochloric acid (4% aqueous solution) were added to the reactor at a molar ratio of 1:2.0:0.1, Water was added to make the pH of the reaction system 4, and the reaction system was heated to a reaction temperature of 30° C., a reaction time of 8 hours, and a pressure of the reaction system at normal pressure.

[0025] b, the purification of acetaldehyde oxime

[0026] After the above reaction is completed, the product obtained by rectification and purification is acetaldehyde oxime. The detection and analysis results show that the conversion rate of acetaldehyde is 98%, and the selectivity of acetaldehyde oxime is 98%.

[0027] The gas chromatogram of the product is as follows figure 1 as shown in:

[0028] After gas chromatographic comparison with the standard product, the obtained product is acet...

Embodiment 2

[0030] a, the synthetic reaction of acetaldehyde oxime

[0031] Butanone oxime (Zhejiang Jinhua New Materials Co., Ltd.), acetaldehyde (Tianjin Kemiou, 40% aqueous solution) and sulfurous acid were added to the reactor at a molar ratio of 1:2.0:0.3, and water was added to make the reaction system The pH is 4.5, the above reaction system is heated, the reaction temperature is 50° C., the reaction time is 10 hours, and the pressure of the reaction system is normal pressure.

[0032] b, the purification of acetaldehyde oxime

[0033] After the above reaction, the reaction solution was rectified and purified to obtain the product acetaldehyde oxime. The detection and analysis showed that the conversion rate of acetaldehyde was 97.02%, and the selectivity was 98.52%.

[0034] It was confirmed that the product was acetaldehyde oxime through gas chromatography detection.

Embodiment 3

[0036] a, the synthetic reaction of acetaldehyde oxime

[0037] Butanone oxime (Zhejiang Jinhua New Materials Co., Ltd.), acetaldehyde (Tianjin Kemiou, 40% aqueous solution) and acetic acid were added to the reactor at a molar ratio of 1:2.0:0.6, and water was added to make the pH of the reaction system is 5, the above reaction system is heated, the reaction temperature is 50° C., the reaction time is 8 hours, and the pressure of the reaction system is normal pressure.

[0038] b, the purification of acetaldehyde oxime

[0039] After the above reaction is completed, the product obtained by rectification and purification is acetaldehyde oxime. The detection and analysis results show that the conversion rate of acetaldehyde is 99.21%, and the selectivity of acetaldehyde oxime is 99.12%.

[0040] It was confirmed that the product was acetaldehyde oxime through gas chromatography detection.

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Abstract

The invention provides a method for preparing acetaldehyde oxime. The acetaldehyde oxime is prepared by carrying out reaction on acetaldehyde and ketoxime in the presence of an acid which serves as a catalyst to exchange oxime. The method provided by the invention is simple, has the advantages of mild reaction conditions, high acetaldehyde conversion rate and environment-friendly reaction process, is a typical chemical process and is suitable for industrial implementation.

Description

technical field [0001] The invention relates to a method for preparing acetaldehyde oxime. The method of the invention has the advantages of low cost and no pollution. Background technique [0002] Acetaldoxime has the structure described below: It is a reducing agent, a new oxygen scavenger, and an important organic synthesis and analysis reagent, which has the characteristics of low toxicity, less pollution, low price and excellent oxygen scavenging effect. In the 1990s, acetaldehyde oxime replaced the highly toxic hydrazine as a boiler water oxygen scavenger, and its oxygen scavenging effect was much higher than that of hydrazine, so it was widely used. Acetaldoxime is an important intermediate for the synthesis of pesticides methomyl and thiodicarb. This pesticide is a good broad-spectrum insecticide. With the continuous growth of its usage, the market demand for acetaldehyde oxime also increases. [0003] Regarding the synthesis method of acetaldehyde oxime, in the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/04C07C251/38C07C45/00C07C49/10
Inventor 张英伟王英其张敏生曹亚林孟祥魏小林
Owner BEIJING RISUN TECH CO LTD
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