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Micro-reaction based production technology of 2-chloro-5-nitrobenzonitrile

A kind of technology of nitrobenzonitrile and production process, applied in the field of production process based on micro-reaction synthesis of 2-chloro-5-nitrobenzonitrile, can solve problems such as increasing production cost, reduce raw material cost and save production The effect of cost and great benefit

Inactive Publication Date: 2019-08-16
SHAOXING JIANG HUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the nitrification process, enterprises currently use sulfuric acid as a solvent and dehydrating agent in the production process of this product, resulting in the use of a large amount of sulfuric acid, which increases the cost of raw materials in the production process, and needs to treat the wastewater generated by the nitrification process. It will inevitably increase the production cost of the product and bring great pressure to the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a. Heating o-chlorobenzonitrile to a liquid state by a water bath;

[0022] b. adding the liquid o-chlorobenzonitrile in step a to the dichloroethane solvent to obtain o-chlorobenzonitrile-dichloroethane solution, the molar ratio of o-chlorobenzonitrile and dichloroethane is 1:6.3;

[0023] c. Transport the o-chlorobenzonitrile-dichloroethane solution and the mixed acid to the micro-reaction module for 60 seconds, and set the reaction temperature of the micro-reaction module to 55°C through the temperature control system;

[0024] d. washing the reaction product to neutrality by 10% sodium hydroxide solution and distilled water;

[0025] e. reclaim ethylene dichloride solvent by distillation, obtain 2-chloro-5-nitrobenzonitrile; Mixed acid is made up of sulfuric acid and nitric acid, and n(98% H2SO4):n(98%HNO3)=1.4:1, Then the yield in the nitration product reached 92%.

Embodiment 2

[0027] a. Heating o-chlorobenzonitrile to a liquid state by a water bath;

[0028] b. adding the liquid o-chlorobenzonitrile in step a to the dichloroethane solvent to obtain o-chlorobenzonitrile-dichloroethane solution, the molar ratio of o-chlorobenzonitrile and dichloroethane is 1:6.3;

[0029] c. Transport the o-chlorobenzonitrile-dichloroethane solution and the mixed acid to the micro-reaction module for 120 seconds, and set the reaction temperature of the micro-reaction module to 65°C through the temperature control system;

[0030] d. washing the reaction product to neutrality by 10% sodium hydroxide solution and distilled water;

[0031] e. reclaim ethylene dichloride solvent by distillation, obtain 2-chloro-5-nitrobenzonitrile; Mixed acid is made up of sulfuric acid and nitric acid, and n(98% H2SO4):n(98%HNO3)=1.4:1, Then the yield in the nitration product reached 93%.

Embodiment 3

[0033] a. Heating o-chlorobenzonitrile to a liquid state by a water bath;

[0034] b. adding the liquid o-chlorobenzonitrile in step a to the dichloroethane solvent to obtain o-chlorobenzonitrile-dichloroethane solution, the molar ratio of o-chlorobenzonitrile and dichloroethane is 1:6.3;

[0035] c. Transport the o-chlorobenzonitrile-dichloroethane solution and the mixed acid to the micro-reaction module to stay for 150 seconds, and set the reaction temperature of the micro-reaction module to 75°C through the temperature control system;

[0036] d. washing the reaction product to neutrality by 10% sodium hydroxide solution and distilled water;

[0037] e. reclaim ethylene dichloride solvent by distillation, obtain 2-chloro-5-nitrobenzonitrile; Mixed acid is made up of sulfuric acid and nitric acid, and n(98% H2SO4):n(98%HNO3)=1.4:1, Then the yield in the nitration product reached 68%.

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PUM

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Abstract

The invention discloses a micro-reaction based production technology of 2-chloro-5-nitrobenzonitrile. The technology comprises following steps: step a, heating o-chlorobenzonitrile in a water bath until o-chlorobenzonitrile is molten; step b, adding liquid o-chlorobenzonitrile obtained in the step a into an organic inert solvent; step c, delivering the mixed solution composed of o-chlorobenzonitrile and the organic inert solvent and mixed acids to a micro reactor, and carrying out reactions to obtain a reaction product; step d, washing the reaction product by a sodium hydroxide solution and distilled water until the reaction product becomes neutral; and step e, recovering the solvent through distillation to obtain 2-chloro-5-nitrobenzonitrile.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a production process for synthesizing 2-chloro-5-nitrobenzonitrile based on micro-reaction. Background technique [0002] 2-Amino-5-nitrobenzonitrile is an important intermediate of disperse red dye, and its hydrolyzed product 2-amino-5-nitrobenzoic acid is an important raw material for the synthesis of quinazolinone compounds, and it is also an important raw material for the synthesis of other medicines. intermediate. This product is currently in great demand in the market and has a broad market prospect in the future. Through a large number of literature research, it has been found that there are many production processes for this product. At present, the main method used in industry is to first nitrate o-chlorobenzonitrile through nitration reaction. Then the obtained 2-chloro-5-nitrobenzonitrile is subjected to ammonolysis reaction to obtain the final product. [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/50B01J19/00
CPCB01J19/0093C07C253/30C07C255/50
Inventor 李江华谢小生马海明聂易球
Owner SHAOXING JIANG HUA CHEM
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