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Method for preparing n-phenylglycinenitrile

A technology of anilinoacetonitrile and hydroxyacetonitrile, which is applied in the preparation of carboxylic acid nitriles, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of large corrosion of equipment and limit the use of microchannel reactors, and achieve fast reaction speed, Prevents decomposition or aggregation and prolongs service life

Active Publication Date: 2015-04-08
内蒙古诚信永安化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Under the traditional process, the method of preparing anilinoacetonitrile by using hydroxyacetonitrile with a mass concentration of 10~60% needs to be carried out under alkaline conditions, and the microchannel reactor is generally a ceramic or glass device, and the alkaline condition will corrode the equipment at high temperature Larger, limiting the use of microchannel reactors in the preparation of anilinoacetonitrile

Method used

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  • Method for preparing n-phenylglycinenitrile
  • Method for preparing n-phenylglycinenitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 1) Use a 30% sodium hydroxide solution to adjust the pH of the hydroxyacetonitrile solution with a mass percentage of 10.0% to 2.5, and then pass it into the G1R*F module through a metering pump;

[0044] 2) Pass aniline with a mass percentage of 99.0% into the G1SHH module for preheating, and the preheating temperature is 130°C;

[0045] 3) Synchronously pump the hydroxyacetonitrile treated in step 1) at a volume flow rate of 35mL / min and the aniline preheated in step 2) at a volume flow rate of 5mL / min into the G1SHH module for mixing, and the temperature of the module is 130°C ;

[0046] 4) The mixed material liquid obtained in step 3) continues to pass through 8 G1SHH modules connected in series, the module temperature is 130°C, and the pressure is 0.3MPa;

[0047] 5) Introduce the feed liquid after step 4) into the G1SHF module to quench the reaction at 70°C;

[0048]6) The feed liquid obtained in step 5) was exported, the feed time was 35 minutes, the temperatur...

Embodiment 2

[0050] 1) Take a hydroxyacetonitrile solution with a mass percentage of 10.0%, and its pH is 1.5, and pass it into the G1SHH module through a metering pump;

[0051] 2) Pass aniline with a mass percentage of 99.14% into the G1R*F module for preheating, and the preheating temperature is 130°C;

[0052] 3) Synchronously pump the hydroxyacetonitrile treated in step 1) at a volume flow rate of 35mL / min and the aniline preheated in step 2) at a volume flow rate of 5mL / min into the G1SHH module for mixing, and the temperature of the module is 130°C ;

[0053] 4) The mixed material liquid obtained in step 3) continues to pass through 12 G1R*H modules connected in series, the module temperature is 130°C, and the pressure is 0.35MPa;

[0054] 5) Introduce the feed liquid after step 4) into the G1SHF module to quench the reaction at 60°C;

[0055] 6) The material liquid obtained in step 5) was exported, and the receiving time was 45 minutes. The temperature in the reaction bottle was ...

Embodiment 3

[0057] 1) Use a 10% sodium hydroxide solution to adjust the pH of the hydroxyacetonitrile solution with a mass percentage of 20.0% to 3.0, and then pass it into the G1R*F module through a metering pump;

[0058] 2) Pass aniline with a mass percentage of 99.25% into the G1R*F module for preheating, and the preheating temperature is 135°C;

[0059] 3) Synchronously pump the hydroxyacetonitrile treated in step 1) at a volume flow rate of 30mL / min and the aniline preheated in step 2) at a volume flow rate of 10mL / min into the G1SHH module for mixing, and the temperature of the module is 135°C ;

[0060] 4) The mixed material liquid obtained in step 3) continues to pass through 5 series-connected G1SHH modules and 5 series-connected G1R*H modules. The temperature of the modules is 135°C and the pressure is 0.44MPa;

[0061] 5) Introduce the feed liquid after step 4) into the G1SHF module to quench the reaction at 65°C;

[0062] 6) The material liquid obtained in step 5) was expor...

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Abstract

The invention relates to a method for preparing n-phenylglycinenitrile. The method is characterized in that condensation reaction is continuously performed for aniline and glycolonitrile by a micro-channel reactor to obtain n-phenylglycinenitrile; the pH of glycolonitrile is pre-regulated to be 1.5 to 7 through a basic catalyst; the molar ratio of aniline to glycolonitrile is 1.00: 1.00-1.30. The method for preparing n-phenylglycinenitrile has the advantages that the process route is simple, and the reaction is fast, so that the working efficiency and production capacity can be ensured, and moreover, the production and operation safety of the process can also be ensured; with the adoption of the process method, the purity of a n-phenylglycinenitrile product exceeds 98.0% and the yield exceeds 99.9%.

Description

technical field [0001] The invention relates to a method for preparing anilinoacetonitrile, in particular to a method for preparing anilinoacetonitrile by utilizing a microchannel reactor. Background technique [0002] Anilinoacetonitrile is not only the main raw material of indigo, but also can be used in the synthesis of other fine chemicals. At present, there are many methods for producing anilinoacetonitrile at home and abroad, among which the "hydroxyacetonitrile" method, that is, aniline and hydroxyacetonitrile with a mass concentration of 10-60% is used as a raw material to prepare anilinoacetonitrile, which is widely used in China, such as Chinese patent CN102627581A, the The method mainly adopts the kettle-type batch-type production process, and synthesizes anilinoacetonitrile through reaction kettle mixing and condensation reaction at a pH of 7~9 and a temperature of 70~110°C. Its disadvantages are mainly long reaction time period, difficult process control, low p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/42C07C253/30
Inventor 刘少华董璞张辰亮陈银霞程丽华彭艳丽杨雪伟王金金
Owner 内蒙古诚信永安化工有限公司
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