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Method for preparing benzylamine through continuous hydrogenation of cyanobenzene

A technology for the preparation of benzonitrile and hydrogen, which is applied to the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds. Simple preparation and stable performance

Inactive Publication Date: 2019-12-20
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems of high energy consumption, harsh reaction conditions, easy deactivation of catalyst, poor selectivity and need for additives in the prior art, the purpose of the present invention is to provide a method with simple process, low energy consumption, low cost, high yield and environmental protection. Method for the continuous catalytic hydrogenation of friendly benzonitrile to synthesize benzylamine

Method used

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  • Method for preparing benzylamine through continuous hydrogenation of cyanobenzene
  • Method for preparing benzylamine through continuous hydrogenation of cyanobenzene
  • Method for preparing benzylamine through continuous hydrogenation of cyanobenzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 80mg of nanoporous palladium catalyst into the fixed bed reactor, continuously add anhydrous methanol to the fixed bed reactor with a pump, raise the temperature to 60°C, adjust the hydrogen pressure to 0.5MPa, and the hydrogen flow rate to 100mL / min, until the temperature and pressure are stable Finally, the mass fraction 3% benzonitrile and 97% methanol are continuously added to the fixed-bed reactor with a pump, and the flow rate of the benzonitrile solution is adjusted to be 0.40mL / min. The reaction material is regularly sampled and analyzed, and the conversion rate of the raw material is 94.9%. The selectivity was 97.3%. Materials can be obtained by distillation benzylamine products. Run time 100h.

Embodiment 2

[0029] Add 80mg of nanoporous palladium catalyst into the fixed bed reactor, continuously add absolute ethanol to the fixed bed reactor with a pump, raise the temperature to 30°C, adjust the hydrogen pressure to 0.5MPa, and the hydrogen flow rate to 100mL / min, until the temperature and pressure are stable Finally, the mass fraction 5% benzonitrile and 95% ethanol are continuously added to the fixed-bed reactor with a pump, and the flow rate of the benzonitrile solution is adjusted to be 0.40mL / min. The reaction material is regularly sampled and analyzed, and the conversion rate of the raw material is 60%. The selectivity 98%. Materials can be obtained by distillation benzylamine products. Run time 100h.

Embodiment 3

[0031] Add 80mg of nanoporous palladium catalyst to the fixed bed reactor, continuously add absolute ethanol to the fixed bed reactor with a pump, raise the temperature to 80°C, adjust the hydrogen pressure to 1.0MPa, and the hydrogen flow rate to 100mL / min, until the temperature and pressure are stable Finally, the mass fraction 5% benzonitrile and 95% ethanol are continuously added to the fixed-bed reactor with a pump, and the flow rate of the benzonitrile solution is adjusted to be 0.30mL / min. The reaction material is regularly sampled and analyzed. The conversion rate of the raw material is 100%. was 72%. Materials can be obtained by distillation benzylamine products. Run time 100h.

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Abstract

The invention relates to a method for preparing benzylamine through continuous hydrogenation of cyanobenzene and belongs to the technical field of heterogeneous catalysis. According to the method, thebenzylamine is synthesized by taking the cyanobenzene as a raw material, nanoporous palladium as a catalyst and hydrogen as a hydrogen source and by a fixed bed liquid phase catalyst hydrogenation process. The method is mild in reaction condition, high in reaction selectivity, additive-free, friendly in operation, high in stability and convenient in industrialized production.

Description

technical field [0001] The invention relates to a method for preparing benzylamine through continuous hydrogenation of benzonitrile, belonging to the technical field of heterogeneous catalysis. Background technique [0002] Benzylamine compounds are organic chemical products and raw materials with a wide range of uses. They are widely used in perfumery, medicine, dyestuff and polyester industries, and have broad prospects for development and utilization. [0003] At present, the production methods of benzylamine compounds are roughly divided into four types. The benzyl chloride addition method is based on benzyl chloride and urotropine (hexamethylenetetramine) as raw materials, through steps such as hydrolysis, acidification, separation, and neutralization. Obtain benzylamine; benzylchloramine hydrolysis method uses benzyl chloride and ammonia water as raw materials to obtain benzylamine through amination, neutralization and other steps. These two methods have all been appl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/48C07C211/27B01J23/44B01J35/10B82Y40/00
CPCC07C209/48B01J23/44B82Y40/00B01J35/643B01J35/647C07C211/27
Inventor 包明修迪冯秀娟方定桥
Owner DALIAN UNIV OF TECH