Continuous synthetic method for benzyl cyanide

A synthesis method, technology of benzyl nitrile, applied in the direction of cyanide reaction preparation, organic chemistry, etc., can solve problems such as side reactions, and achieve the effect of solving side reactions

Inactive Publication Date: 2019-01-18
营创三征(营口)精细化工有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of the above problems, the present invention proposes a continuous synthesis method of benzyl nitrile, which adopts multi-temperature section series microreactors, and sets a low temperature microreactor after the synthesis reaction of benzyl nitrile, which solves the problem of side reactions in the reaction process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Polyethylene glycol is added in 30wt.% sodium cyanide aqueous solution, and the mass ratio of polyethylene glycol and 30wt.% sodium cyanide is 0.03:1, and it is standby after dissolving, and the feed pipe 1 of microchannel reactor is inserted into cyanide In the mixed solution of sodium cyanide and tetrabutylammonium bromide, the feed pipe 2 is inserted into the sealed benzyl chloride solution, the molar ratio of sodium cyanide to benzyl chloride is 0.9:1, and the temperature of the high and low temperature circulation device is set at 70°C At the same time, the raw material peristaltic pump is turned on, and the reaction liquid enters the first-stage microchannel reactor at the set flow rate, and the residence time is 50s. Connect the secondary microchannel reactor to the outlet of the primary microchannel reactor, set the secondary microchannel reactor lower than the primary microchannel reactor, the temperature is 50°C, and the residence time is 100s. The two-phase r...

Embodiment 2

[0015] Tetrabutylammonium bromide is added in 30wt.% sodium cyanide aqueous solution, tetrabutylammonium bromide and 30wt.% sodium cyanide mass ratio are 0.05:1, standby after dissolving, the feeding of microchannel reactor Tube 1 is inserted into the mixed solution of sodium cyanide and tetrabutylammonium bromide, and feeding tube 2 is inserted into the sealed benzyl chloride solution. The molar ratio of sodium cyanide to benzyl chloride is 0.98:1, and a high and low temperature circulation device is installed. The temperature is 70°C, and at the same time, the raw material peristaltic pump is turned on, and the reaction solution enters the first-stage microchannel reactor at the set flow rate, and the residence time is 50s. Connect the secondary microchannel reactor to the outlet of the primary microchannel reactor, set the secondary microchannel reactor lower than the primary microchannel reactor, the temperature is 50°C, and the residence time is 100s. The two-phase reacti...

Embodiment 3

[0017] Tetrabutylammonium bromide is added in 30wt.% sodium cyanide aqueous solution, tetrabutylammonium bromide and 30wt.% sodium cyanide mass ratio are 0.04:1, standby after dissolving, the feeding of microchannel reactor Tube 1 is inserted into the mixed solution of sodium cyanide and tetrabutylammonium bromide, and feeding tube 2 is inserted into the sealed benzyl chloride solution. The molar ratio of sodium cyanide to benzyl chloride is 0.95:1, and a high and low temperature circulation device is installed. The temperature is 70°C, and at the same time, the raw material peristaltic pump is turned on, and the reaction solution enters the first-stage microchannel reactor at the set flow rate, and the residence time is 50s. Connect the secondary microchannel reactor to the outlet of the primary microchannel reactor, set the secondary microchannel reactor lower than the primary microchannel reactor, the temperature is at 50°C, and the residence time is 150s. The two-phase rea...

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Abstract

The invention provides a continuous synthetic method for benzyl cyanide. Multi-temperature serially connected micro-reactors are adopted; a low temperature micro-reactor is arranged after the benzyl cyanide synthetic reaction; sodium cyanide, phase transfer catalyst component and benzyl chloride component are respectively introduced into two continuous micro-channel reactors; the temperature of asecond micro-channel reactor is slightly lower than the temperature of a first micro-channel reactor, so that the 'overheat' phenomenon under a microcosmic condition can be solved; side reaction during reaction process is reduced; purity and yield of products are increased.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a continuous synthesis method of benzyl nitrile. Background technique [0002] Phenylacetonitrile, an organic compound. Chemical formula: C8H7N, commonly known as benzonitrile, benzyl cyanide, benzyl cyanide, α-benzyl nitrile. Colorless oily liquid with a pungent smell, insoluble in water, soluble in most organic solvents such as ethanol and ether. for toxic chemicals. Mainly used in organic synthesis and production of pharmaceuticals and pesticide intermediates. [0003] The existing phenylacetonitrile production process mainly adopts benzyl chloride, sodium cyanide aqueous solution and phase transfer catalyst as raw materials, and adopts the intermittent mode of slowly dripping sodium cyanide in the reactor for production. The cyanidation process in the process has problems such as long reaction time, small processing capacity, and many side reactions....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/14C07C255/33
CPCC07C253/14C07C255/33
Inventor 刘至寻梁海齐长亮吴丹张佳兴姜德孜
Owner 营创三征(营口)精细化工有限公司
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