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Method for preparing benzoin in micro-reaction device

A micro-reaction device and benzoin technology, applied in the field of chemical reaction, can solve the problems of long production cycle, large amount of catalyst, environmental pollution and the like of batch reactor type reactor, achieve high-efficiency heat and mass transfer capability, clean reaction, reduce effect of dissolution

Active Publication Date: 2020-04-17
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of safety in the use of cyanide, long production cycle of batch tank reactor, low efficiency, large catalyst consumption and serious environmental pollution, and provide a A kind of method for preparing benzoin

Method used

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  • Method for preparing benzoin in micro-reaction device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: the preparation of benzoin

[0024] Dissolve 100g of benzaldehyde in 40ml of methanol, mix well, pump into the micro-mixer, and at the same time pump 10ml of 5% sodium cyanide aqueous solution into the micro-mixer, adjust the flow rate of benzaldehyde solution to 2ml / min, adjust the flow rate of sodium cyanide aqueous solution The reaction time is 0.13ml / min, stay in the micro-mixer for 6s, enter the micro-reactor for reaction, the reaction time is 10min, heat to 50 degrees, sample for gas phase analysis, the reaction selectivity is 98.9%. The reacted material was cooled and crystallized, filtered and dried to obtain 97 g of the product, and the product yield was 97%. The mother liquor is recovered to the cyanide storage kettle for recycling.

Embodiment 2

[0025] Embodiment 2: the preparation of benzoin

[0026] Dissolve 100g of benzaldehyde in 40ml of methanol, mix well, pump into the micro-mixer, and at the same time pump 20ml of 1% sodium cyanide aqueous solution into the micro-mixer, adjust the flow rate of benzaldehyde solution to 2ml / min, adjust the flow rate of sodium cyanide aqueous solution 0.29ml / min, stay in the micro-mixer for 6s, enter the micro-reactor for reaction, the reaction time is 20min, the reaction temperature is 60 degrees, sampling for gas phase analysis, the reaction selectivity is 98.3%. The reacted material was cooled and crystallized, filtered and dried to obtain 96.5 g of the product, and the product yield was 96.5%.

Embodiment 3

[0027] Embodiment 3: the preparation of benzoin

[0028] Dissolve 100g of benzaldehyde in 50ml of methanol, mix well, pump into the micro-mixer, and at the same time pump 5ml of 10% sodium cyanide aqueous solution into the micro-mixer, adjust the flow rate of benzaldehyde solution to 2ml / min, adjust the flow rate of sodium cyanide aqueous solution 0.06ml / min, stay in the micro-mixer for 5s, enter the micro-reactor for reaction, the reaction time is 20min, the reaction temperature is 45 degrees, sampling for gas phase analysis, the reaction selectivity is 98.9%. The reacted material was cooled and crystallized, filtered and dried to obtain 97.5 g of the product, and the product yield was 97.5%.

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Abstract

The invention relates to a method for preparing benzoin in a microreactor. According to the invention, benzaldehyde and sodium cyanide are used as raw materials, and benzoin is prepared through benzoin condensation. According to the preparation method for benzoin provided by the invention, the consumption of cyanide is greatly reduced, and the whole reaction process is totally closed and is thus relatively safe and reliable; the efficient heat and mass transfer capacity of the micro-channel reactor is used, so reaction temperature is reduced, side reactions such as oxidation, polymerization and self-disproportionation of benzaldehyde are reduced, reaction yield is high, a yield coefficient is high, and industrial production is easy to realize.

Description

technical field [0001] The invention belongs to the technical field of chemical reaction, and in particular relates to a method for preparing benzoin in a micro-reaction device. Background technique [0002] Benzoin, whose chemical name is 1,2-diphenyl oxyethyl ketone, is a white needle-like crystal and is an important chemical raw material, widely used as a photosensitizer for photosensitive resins, dye intermediates and powder coatings It is also an important drug synthesis intermediate, such as the synthesis of antiepileptic drug diphenylhydantoin and the synthesis of diphenyl ketone, diphenyl ketone oxime, and acetic acid benzoin compounds. preparation etc. [0003] Benzoin is usually prepared by the condensation of benzaldehyde itself (commonly known as benzoin condensation). The industrial preparation of benzoin through benzoin condensation uses sodium cyanide or potassium cyanide as a catalyst. Under alkaline conditions, the cyanide anion ( CN - ) to promote the co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/45C07C49/83B01J19/00
CPCC07C45/45B01J19/0093C07C49/83
Inventor 赵国锋任凤霞马小文董子瑞
Owner TIANJIN JIURI NEW MATERIALS CO LTD
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