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Method for preparing benzoyl cyanide through catalytic synthesis of catalyst

A technology of benzoyl cyanide and catalyst, which is applied in the field of catalyst-catalyzed synthesis of benzoyl cyanide, can solve the problems of many by-products and low yield, and achieve the effect of less by-products, high purity and good selectivity

Pending Publication Date: 2022-01-04
HANDAN RUITIAN PESTICIDES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the prior art, there are multiple methods for the synthesis of benzoyl cyanide, but there are generally low yields and many by-products. Therefore, we have proposed a catalyst-catalyzed synthesis of benzoyl cyanide preparation method for solving the above problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In embodiment 1, the catalyst catalyzed synthetic benzoyl cyanide preparation method comprises the following steps:

[0026] S1. First put xylene into the reaction kettle, start stirring, then put in sodium cyanide and catalyst, and heat the reaction kettle to a reflux state through steam;

[0027] S2, azeotropic dehydration, check whether the moisture content of the material in the kettle is less than 250ppm, open the feed valve of the xylene receiving cylinder after passing the test, steam out 30% xylene for recycling, and cool down after steaming;

[0028] S3. When the reactor is lowered to 88°C, put the phase transfer catalyst into the reactor, open the steam valve, and continue to heat up to the reflux state;

[0029] S4, the temperature is raised to 93° C., and in the reflux state, the measured benzoyl chloride is added dropwise to the reactor, and the temperature of the reactor is raised to 120° C. while adding dropwise, and kept for 4 hours under this condition ...

Embodiment 2

[0039] In embodiment 2, catalyst catalyzes the synthetic benzoyl cyanide preparation method, comprises the following steps:

[0040] S1. First put xylene into the reaction kettle, start stirring, then put in sodium cyanide and catalyst, and heat the reaction kettle to a reflux state through steam;

[0041] S2, azeotropic dehydration, check whether the moisture content of the material in the kettle is less than 250ppm, open the feed valve of the xylene receiving cylinder after passing the test, steam out 30% xylene for recycling, and cool down after steaming;

[0042] S3. When the reactor is lowered to 90°C, put the phase transfer catalyst into the reactor, open the steam valve, and continue to heat up to the reflux state;

[0043] S4, the temperature is raised to 95°C, and under reflux, the measured benzoyl chloride is added dropwise to the reactor, and the temperature of the reactor is raised to 125°C while adding dropwise, and the temperature of the reactor is kept for 5 hou...

Embodiment 3

[0053] In embodiment 3, catalyst catalyzes the synthesis method of benzoyl cyanide preparation, comprises the following steps:

[0054] S1. First put xylene into the reaction kettle, start stirring, then put in sodium cyanide and catalyst, and heat the reaction kettle to a reflux state through steam;

[0055] S2, azeotropic dehydration, check whether the moisture content of the material in the kettle is less than 250ppm, open the feed valve of the xylene receiving cylinder after passing the test, steam out 30% xylene for recycling, and cool down after steaming;

[0056] S3. When the reactor is lowered to 92°C, put the phase transfer catalyst into the reactor, open the steam valve, and continue to heat up to the reflux state;

[0057] S4, the temperature is raised to 96° C., and in the reflux state, the measured benzoyl chloride is added dropwise to the reactor, and the temperature of the reactor is raised to 130° C. while adding dropwise, and the temperature is kept for 6 hour...

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PUM

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Abstract

The invention relates to the technical field of benzoyl cyanide preparation, in particular to a method for preparing benzoyl cyanide through catalytic synthesis of a catalyst. The method comprises the steps of S1, putting xylene into a reaction kettle, starting stirring, adding sodium cyanide and the catalyst, and heating the reaction kettle to a reflux state through steam; S2, conducting azeotropic dehydration, specifically, detecting whether the water content of the material in the kettle is less than 250ppm or not, opening a feed valve of a xylene receiving cylinder after the water content is qualified, steaming out 30% of xylene, recovering the xylene for later use, and cooling after steaming; S3, cooling the reaction kettle to 88-92 DEG C, adding a phase transfer catalyst into the reaction kettle, opening a steam valve, and continuously heating to a reflux state; and S4, raising the temperature to 93-96 DEG C, and dropwise adding metered benzoyl chloride into the reaction kettle in a reflux state. The preparation method provided by the invention has the advantages of mild reaction conditions, short reaction time, conversion rate of benzoyl chloride greater than 99.5%, few by-products generated by the reaction and high purity of benzoyl cyanide.

Description

technical field [0001] The invention relates to the technical field of benzoyl cyanide preparation, in particular to a preparation method for catalytic synthesis of benzoyl cyanide by a catalyst. Background technique [0002] The chemical name of methazinone is 4-amino-3-methyl-6-benzyl-1,2,3-triazin-5(4H)one, which is a triazinone developed by Bayer in 1975 Herbicides are widely used in the field of sugar beet herbicides, and are highly efficient and safe herbicides with considerable scale. [0003] Benzoyl cyanide is an important intermediate for the synthesis of benzoyl cyanide. In the existing production technology, benzoyl cyanide is mostly prepared by using benzoyl chloride and alkali metal cyanide as raw materials under the action of a catalyst. The catalyst used Most of them are phase transfer catalysts. [0004] In the prior art, there are many methods for synthesizing benzoyl cyanide, but generally there are low yields and many by-products. Therefore, we propose ...

Claims

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Application Information

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IPC IPC(8): C07C255/40C07C253/04
CPCC07C253/04C07C255/40
Inventor 王学铭张艳敏王哲君
Owner HANDAN RUITIAN PESTICIDES CO LTD