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A device for continuously synthesizing benzylamines by heterogeneous hydrogenation in a microreactor

A micro-reactor, benzylamine technology, applied in the field of chemical reactions, can solve the problems of poor control accuracy of process conditions, large catalyst dosage, large reactor volume, etc., to avoid local excessive hydrogenation, reduce by-products, and transmit high quality effect

Active Publication Date: 2021-02-12
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has problems such as cumbersome operation, frequent loading and unloading of catalysts, low reaction efficiency, large catalyst consumption and easy loss, large reactor volume, poor safety, poor control accuracy of process conditions, and low product purity.

Method used

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  • A device for continuously synthesizing benzylamines by heterogeneous hydrogenation in a microreactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Carry out experiment according to this method, configure the ethyl acetate solution of benzaldehyde, concentration is 5wt%, mixes with ammonia gas in inlet film dispersion micro-mixer 1, the molar ratio of control ammonia / benzaldehyde is 15:1, mixes with hydrogen afterwards Mix in the entrance film dispersion micro-mixer 2, the formed gas-liquid mixture passes through the micro-packed bed reactor filled with Raney nickel catalyst, the control reaction temperature is 150°C, the pressure is 5.0MPa, and the control residence time is 0.5min. Gas-liquid phase separation was carried out at the outlet of the packed bed, and the obtained ethyl acetate solution was analyzed. The conversion rate of the reaction was 100%, and the yield of benzylamine was 96%.

Embodiment 2

[0034] Carry out experiment according to this method, configure the methanol solution of benzaldehyde, concentration is 10wt%, mixes with ammonia in inlet micro-sieve micro-mixer 1, the molar ratio of control ammonia / benzaldehyde is 0.5:1, then mixes with hydrogen in Mix in the inlet micro-sieve micro-mixer 2, and the formed gas-liquid mixture passes through the micro-packed bed reactor filled with palladium-carbon catalyst. The reaction temperature is controlled to be 100°C, the pressure is 10.0MPa, and the residence time is controlled to be 2min. The micro-packed bed Gas-liquid phase separation was carried out at the outlet, and the obtained methanol solution was analyzed. The conversion rate of the reaction was 100%, and the yield of dibenzylamine was 90%.

Embodiment 3

[0036] Carry out experiment according to this method, configure the propanol solution of p-tert-butylbenzaldehyde, concentration is 20wt%, add phase-transfer catalyst benzyltriethylammonium chloride, add-on is 0.5% of substrate concentration to be hydrogenated, and Ammonia is mixed in the inlet T-type micro-mixer 1, and the molar ratio of ammonia / benzaldehyde is controlled to be 5:1, and then mixed with hydrogen in the inlet membrane dispersion micro-mixer 2, and the formed gas-liquid mixture passes through the ruthenium alumina The micro-packed bed reactor of the catalyst, the reaction temperature is controlled at 80°C, the pressure is 4.0MPa, and the residence time is controlled at 3min. The gas-liquid phase separation is carried out at the outlet of the micro-packed bed, and the obtained propanol solution is analyzed. The conversion rate of the reaction is 100%, the yield of p-tert-butylbenzylamine is 95%.

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Abstract

Belonging to the technical field of chemical reaction, the invention particularly relates to a device for continuous synthesis of a benzylamine substance through heterogeneous hydrogenation in a micro-reactor. The device comprises: an inlet micro-mixer (1), an inlet micro-mixer (2), a micro-packed bed reactor (3) and an outlet split-phase tank (4). The device utilizes the efficient mixing and excellent mass and heat transfer performance of the micro-reactor to enhance the interphase mass transfer and heat removal capability in the reaction process, and can obviously reduce the volume of the reactor, improve the reaction yield, and enhance the production efficiency and safety. The method can solve the problems of low production efficiency, poor product purity, high device risk and the likein the hydrogenation kettle process, can realize continuous automatic operation of the process, and has the advantages of high yield, high safety and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical reactions, in particular to a method for continuously synthesizing benzylamines through heterogeneous hydrogenation in a microreactor. Background technique [0002] Benzylamines, such as monobenzylamine, dibenzylamine and p-tert-butylbenzylamine, are an important class of organic synthesis intermediates, widely used in medicine, pesticides, dyes and other industries. The commonly used methods for producing such substances are benzyl chloride method, benzonitrile hydrogenation method and benzaldehyde reductive amination method. The benzyl chloride process is simple and mature, but the process yield is low, the product quality is poor, and a large amount of saline wastewater is produced, which does not meet the needs of clean production and has been gradually eliminated. The product quality of benzonitrile method is high, and technological process is simple, but raw material cost is high. Therefo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/26C07C211/27B01J19/00
CPCB01J19/0093C07C209/26C07C211/27
Inventor 张吉松屠佳成桑乐
Owner TSINGHUA UNIV
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