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
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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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