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Synthesis technology based on 2-amino-5-nitrobenzonitrile

A technology of nitrobenzonitrile and synthesis process, which is applied in the field of synthesis technology based on 2-amino-5-nitrobenzonitrile, can solve problems such as increasing production cost, and achieves reduction of raw material cost, great benefit, and production saving cost effect

Inactive Publication Date: 2019-07-19
SHAOXING JIANG HUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Synthesis technology based on 2-amino-5-nitrobenzonitrile
  • Synthesis technology based on 2-amino-5-nitrobenzonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Such as figure 1 Shown, based on the synthetic technique of 2-amino-5-nitrobenzonitrile, the step of this technique is as follows:

[0027] a. The o-chlorobenzonitrile is heated to a liquid by a water bath heating tank, and the liquid o-chlorobenzonitrile and dichloroethane are delivered to the reactor together;

[0028] b. Cool the liquid o-chlorobenzonitrile to 0°C, then slowly drop the mixed acid into the reactor, and control the temperature in the reactor by adjusting the titration speed to ensure that the temperature of the reaction system is at 0°C; 98% nitric acid and 98% sulfuric acid are composed, and n(o-chlorobenzonitrile):n(98%HNO3):n(98%H2SO4):n(dichloroethane)=1:1.15:1.4:3.43 ;

[0029] c. After the dropwise addition of the mixed acid is completed, keep the inside of the reactor warm for 5 hours;

[0030] d. Add water to dilute the remaining sulfuric acid after the reaction of mixed acid and o-chlorobenzonitrile;

[0031] e. Solvent and reaction produc...

Embodiment 2

[0039] Such as figure 1 Shown, based on the synthetic technique of 2-amino-5-nitrobenzonitrile, the step of this technique is as follows:

[0040] a. The o-chlorobenzonitrile is heated to a liquid by a water bath heating tank, and the liquid o-chlorobenzonitrile and dichloroethane are delivered to the reactor together;

[0041] b. Cool the liquid o-chlorobenzonitrile to 10°C, then slowly drop the mixed acid into the reactor, and control the temperature in the reactor by adjusting the titration speed to ensure that the temperature of the reaction system is at 10°C; 98% nitric acid and 98% sulfuric acid are composed, and n(o-chlorobenzonitrile):n(98%HNO3):n(98%H2SO4):n(dichloroethane)=1:1.15:1.4:3.43 ;

[0042] c. After the dropwise addition of the mixed acid is completed, keep the inside of the reactor warm for 5 hours;

[0043] d. Add water to dilute the remaining sulfuric acid after the reaction of mixed acid and o-chlorobenzonitrile;

[0044] e. Solvent and reaction prod...

Embodiment 3

[0052] Such as figure 1 Shown, based on the synthetic technique of 2-amino-5-nitrobenzonitrile, the step of this technique is as follows:

[0053] a. The o-chlorobenzonitrile is heated to a liquid by a water bath heating tank, and the liquid o-chlorobenzonitrile and dichloroethane are delivered to the reactor together;

[0054] b. Cool the liquid o-chlorobenzonitrile to 10°C, then slowly drop the mixed acid into the reactor, and control the temperature in the reactor by adjusting the titration speed to ensure that the temperature of the reaction system is at 18°C; 98% nitric acid and 98% sulfuric acid are composed, and n(o-chlorobenzonitrile):n(98%HNO3):n(98%H2SO4):n(dichloroethane)=1:1.15:1.4:3.43 ;

[0055] c. After the dropwise addition of the mixed acid is completed, keep the inside of the reactor warm for 5 hours;

[0056] d. Add water to dilute the remaining sulfuric acid after the reaction of mixed acid and o-chlorobenzonitrile;

[0057] e. Solvent and reaction prod...

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Abstract

The invention discloses a synthesis technology based on 2-amino-5-nitrobenzonitrile. The technology comprises the following steps: a, heating chlorobenzonitrile to form liquid in a water bath heatingtrough and conveying liquid chlorobenzonitrile and dichloroethane into a reactor, B, cooling liquid chlorobenzonitrile to 0-10 DEG C, slowly dropwise adding mixed acid into a reaction kettle, c, afterdropwise adding mixed acid, holding the temperature in the reaction kettle for 4h, d, adding water to dilute residual sulfuric acid after a reaction between mixed acid and chlorobenzonitrile finishes, e, separating a solvent and a reaction product by distillation, f, extracting 2-chlorine-5-nitrobenzonitrile by taking chlorobenzene as a solvent, g, conveying a 2-chlorine-5-nitrobenzonitrile solvent into a high-pressure reaction kettle, h, conveying liquid ammonia into the high-pressure reaction kettle through a compression pump for reaction for a certain time, i, after the reaction finishes,releasing pressure of the high-pressure reaction kettle, collecting excess liquid ammonia, separating chlorobenzene and a reaction product, and j, washing and drying the reaction product.

Description

technical field [0001] The invention belongs to the technical field, in particular to a synthesis process based on 2-amino-5-nitrobenzonitrile. 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 amount 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. [0003] In the nitrification process, enterprises current...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/58
CPCC07C253/30C07C255/50C07C255/58
Inventor 李江华谢小生马海明聂易球
Owner SHAOXING JIANG HUA CHEM
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