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Catalytic system for Beckmann rearrangement of oxime

A Beckmann rearrangement and catalytic system technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, organic chemistry, etc. It can achieve the effect of realizing recycling, simple reaction system and high conversion rate.

Active Publication Date: 2013-01-30
TSINGHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these processes still have problems such as low caprolactam selectivity and easy deactivation of catalysts, which restrict their industrial application.

Method used

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  • Catalytic system for Beckmann rearrangement of oxime
  • Catalytic system for Beckmann rearrangement of oxime

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Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0011] The present invention will be further described below by specific examples.

[0012] The experimental steps for the catalytic system to be used in the Beckmann rearrangement reaction of ketoxime are: add a certain amount of organic acid and 10 mmol of organic solvent into a three-necked flask, then add 2 mmol of ketoxime, control the temperature in an oil bath, and stir with a magnetic force. After a certain period of time, the product was analyzed to obtain the conversion rate of ketoxime and the selectivity of amide.

[0013] Embodiment 1-11 is carried out according to the above-mentioned experimental procedure, wherein the mol ratio of organic acid, organic solvent, organic acid and organic solvent, ketoxime, reaction time, reaction temperature, conversion rate of ketoxime after reaction finishes and amide The options are listed in Table 1.

[0014] Table 1 The raw materials and results of the preparation of amides from ketoximes via Beckmann rearrangement

[0015]...

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Abstract

The invention discloses a catalytic system for Beckmann rearrangement of oxime, characterized in that: the catalytic system is a homogeneous system comprising organic acid and organic solvent; the catalytic system is used as a catalyst in the Beckmann rearrangement of oxime for preparing amide, the reaction temperature is 60-130 DEG C, and the reaction time is 2-240 min; and the molar ratio of the organic acid to the organic solvent is 0.1-50. The catalytic system can efficiently convert oxime into a corresponding amide-type compound under relatively mild reaction conditions. According to the invention, the catalytic system can be recycled and has high conversion rate and selectivity, the reaction system while use is simple, and the reaction conditions are mild; the Beckmann rearrangement of oxime has high conversion rate and good selectivity; the product after the Beckmann rearrangement is easily processed, thus the recycling of the organic solvent and the catalyst can be realized.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysis, and in particular relates to a catalytic system for the Beckmann rearrangement reaction of ketoxime. Background technique [0002] Beckmann rearrangement is a kind of rearrangement reaction that occurs under acid catalysis, and it is mainly used in the conversion of ketoxime to the corresponding amide. Take caprolactam as an example, it is an important organic chemical raw material, mainly used in the production of nylon 6 fiber (nylon 6) and nylon 6 engineering plastics. Among them: nylon 6 fiber is widely used in wool spinning, knitting, weaving, carpet and other industries, and nylon 6 engineering plastics is widely used in electronics, automobiles, packaging films and other industries. In 2010, the apparent consumption of caprolactam in my country reached 1.125 million tons, while the domestic production was only 494,000 tons, and the self-sufficiency rate was only 43.9%. [0003...

Claims

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Application Information

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IPC IPC(8): B01J31/04B01J31/02C07D201/04C07D223/10C07D225/02C07C231/10C07C233/05C07C233/65
CPCY02P20/584
Inventor 张吉松骆广生吕阳成王凯
Owner TSINGHUA UNIV
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