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The method of continuous method synthetic benzyl nitrile

A phenylacetonitrile, continuous process technology, applied in the preparation of cyanide reaction, organic chemistry and other directions, can solve the problems of large floor space, many equipment, long reaction time, etc., to achieve high production efficiency, reduce side reactions, and shorten the reaction time. Effect

Active Publication Date: 2017-08-11
HEBEI CHENGXIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This kind of continuous reaction device makes the cyanidation reaction continue, but the reaction time is still long, the equipment used is more, and the floor area is large.

Method used

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  • The method of continuous method synthetic benzyl nitrile

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] First adjust the temperature of the microreactor to be controlled at 180°C. Under the plunger pump action, mix 12kmol mass concentration of 13% sodium cyanide aqueous solution and phase transfer catalyst benzyl diethyl ammonium chloride (the consumption of phase transfer catalyst is 1‰ of benzyl chloride mass) mixed solution and 10kmol benzyl chloride liquid were continuously injected into the microreactor respectively, and the residence time was controlled at 150s to directly obtain the aqueous solution of benzyl nitrile. The quality of benzyl chloride was monitored by GC, and the purity of the crude product was 98.5%. . Under the action of the continuous extraction and separation equipment (extraction centrifuge), the obtained aqueous solution of benzylnitrile is centrifuged to separate the obtained aqueous solution of benzylnitrile, and the crude product of benzylnitrile is separated from the light phase port, and the yield of the crude product of benzylnitrile is 97....

Embodiment 2

[0024] First adjust the temperature of the microreactor to be controlled at 250°C. Under the plunger pump action, mix 12kmol 13% sodium cyanide aqueous solution and phase transfer catalyst benzyl diethyl ammonium chloride (the consumption of phase transfer catalyst is chlorination 0.5‰ of the mass of benzyl), and 10kmol benzyl chloride liquid were continuously injected into the microreactor, the residence time was controlled at 100s, and the aqueous solution of benzyl nitrile was obtained directly. The quality of benzyl nitrile was monitored by GC, and the purity of the crude product was 98.6%. Under the action of the continuous extraction and separation equipment (extraction centrifuge), the obtained phenylacetonitrile feed liquid is subjected to centrifugal separation, and what is separated from the light phase port is the crude product of phenylacetonitrile, and the yield of the crude product of phenylacetonitrile is 97.7% %, what is separated from the heavy phase is waste s...

Embodiment 3

[0026] First adjust the temperature of the microreactor to be controlled at 400°C. Under the plunger pump effect, mix 12kmol 13% sodium cyanide aqueous solution and phase transfer catalyst benzyl triethyl ammonium chloride (the consumption of phase transfer catalyst is chlorination 0.8‰ of the mass of benzyl), and 10kmol benzyl chloride liquid were continuously injected into the microreactor, the residence time was controlled at 20s, and the aqueous solution of benzyl nitrile was obtained directly. The quality of benzyl nitrile was monitored by GC, and the purity of the crude product was 98.5%. Under the action of the continuous extraction and separation equipment (extraction centrifuge), the obtained phenylacetonitrile feed liquid was subjected to centrifugal separation, and what was separated from the light phase port was the crude product of phenylacetonitrile, and the yield of the crude product of phenylacetonitrile was 97.6% %, what is separated from the heavy phase is was...

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Abstract

The invention discloses a method for synthesizing phenylacetonitrile by performing continuous reaction, and relates to the field of preparing a compound containing six-membered aromatic ring connected with cyano group by saturated carbon chain. The method comprises the following steps: adjusting the temperature of a micro-reactor to 80-400 DEG C; adding a mixture of a sodium cyanide aqueous solution and phase-transfer catalyst, and benzyl chloride in the micro-reactor continuously; reacting in the micro-reactor for 20-300 s to get a phenylacetonitrile aqueous solution. The method has rapid reaction speed, high production efficiency, low cost, good product quality, is easy to realize automatic control, is beneficial to subsequent post-treatment, and can raise the phenylacetonitrile yield, reduce the side reaction, and save labour.

Description

technical field [0001] The invention relates to the technical field of compound preparation in which a cyano group is connected to a six-membered aromatic ring by a saturated carbon chain. Background technique [0002] Phenylacetonitrile is a very important intermediate, and the downstream product, phenylacetic acid, is an important precursor for the synthesis of penicillin, and can also be used in the flavor and fragrance industry. The method for synthesizing phenylacetonitrile generally adopts kettle reaction, which is carried out intermittently. The impurities generated by the reaction are more, and the production efficiency is low. Especially, phenylacetonitrile has a special pungent smell, and the shortcoming of batch production is particularly prominent. . The patent CN201942626U of Shandong Liaocheng Zhongsheng Lanrui Chemical Co., Ltd. published a patent titled "Continuous Cyanide Reaction Device and Method in the Production of Phenylacetonitrile", using multiple re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/33C07C253/14
Inventor 贾荣荣李燕张艳章李兴波刘旭王金花彭艳丽程丽华
Owner HEBEI CHENGXIN
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