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Method for extracting effective components from o-nitrochlorobenzene tar

A technology of o-nitrochlorobenzene and o-nitrochlorobenzene, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the need for regular discharge of tar, affecting the effect of rectification, and easy to explode, etc. problems, to achieve the effect of enhancing market competitiveness, improving economic benefits, and avoiding hidden dangers of explosions

Pending Publication Date: 2020-09-22
SINOPEC NANJING RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the rectification process, due to the continuous high-temperature distillation in the tower kettle, tar is produced in the liquid in the kettle. At the same time, after the rectification of o-nitrochlorobenzene, dinitrochlorobenzene is gradually enriched, which affects the rectification effect, and the tar needs to be discharged regularly
In the discharged tar, the content of o-nitrochlorobenzene is about 66%, and the trace amount of dinitrochlorobenzene produced in the reaction process reaches about 22% after being enriched. pose a great security risk

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A 500mL four-neck flask is connected to a speed-adjustable stirring device, a thermometer, a dropping funnel, a condenser tube and a heating device. Add 170 grams of ortho-nitrochlorobenzene distilled tar to the four-necked bottle, then add 150 grams of azeotropic solvent (water), start stirring, start heating, heat the solution to 105°C, boil, and the gas phase temperature is 78°C. According to the amount of gas phase recovery, the azeotropic solvent is continuously added dropwise, the gas phase distilled liquid is separated from the organic phase and the azeotropic solvent through the separatory funnel, and the azeotropic solvent is added to the dropping funnel for recycling. The temperature of the gas phase reaches 98°C, and the distillation ends , 90 grams of organic phase weight, gas chromatography analysis, o-nitrochlorobenzene content 94.3%.

Embodiment 2

[0020] 500mL four-neck flask, the same device as above. Add 100 grams of ortho-nitrochlorobenzene distilled tar to the four-neck flask, then add 200 grams of azeotropic solvent (water), start stirring, start heating, heat the solution to 102°C, boil, and the gas phase temperature is 74°C. According to the amount of gas phase recovery, the azeotropic solvent is continuously added dropwise, the gas phase distilled liquid is separated from the organic phase and the azeotropic solvent through the separatory funnel, and the azeotropic solvent is added to the dropping funnel for recycling. The temperature of the gas phase reaches 98°C, and the distillation ends , organic phase analysis, o-nitrochlorobenzene content of 95.2%.

Embodiment 3

[0022] 500mL four-neck flask, the same device as above. Add 200 grams of ortho-nitrochlorobenzene distilled tar to the four-necked bottle, then add 100 grams of azeotropic solvent (water), start stirring, start heating, heat the solution to 107 ° C, boil, according to the amount of gas phase recovery, continue Add the azeotropic solvent dropwise, the vapor phase distilled liquid is separated through the separatory funnel to separate the organic phase and the azeotropic solvent, and the azeotropic solvent is added to the dropping funnel for recycling. The content of chlorobenzene is 93.8%.

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PUM

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Abstract

According to the invention, an azeotropic distillation method is adopted to extract effective components in tar after ortho-nitrochlorobenzene distillation; the method comprises the following steps: adding a certain amount of tar into a distillation container, adding a certain amount of azeotropic solvent into the container, heating the mixture to boil, cooling the azeotropic solvent and organic components, layering the mixture, separating liquid, returning the azeotropic solvent to a distillation system for circulation, distilling the mixture until no organic phase is evaporated, and dehydrating and rectifying the organic phase to obtain the high-purity o-nitrochlorobenzene. According to the method, the tar content in the o-nitrochlorobenzene can be reduced by half; therefore, on one hand, the recovered o-nitrochlorobenzene is sold as a product, the economic benefit can be improved, the market competitiveness of the product is enhanced, and on the other hand, the tar yield can be reduced, and good social benefits are achieved.

Description

technical field [0001] The invention relates to the field of organic chemical separation, and introduces a method for extracting effective components from o-nitrochlorobenzene distillation tar. Background technique [0002] The production of o-nitrochlorobenzene is to obtain the final product through nitration, washing, neutralization and rectification of chlorinated benzene. While nitrochlorobenzene is nitrated to generate mononitrochlorobenzene, there is also a small amount of dinitrochlorobenzene generate. The nitration solution is obtained by rectification to obtain para-rich finished product and high-purity o-nitrochlorobenzene finished product. During the rectification process, due to the continuous high-temperature distillation in the tower kettle, tar is produced in the liquid in the kettle. At the same time, after the rectification of o-nitrochlorobenzene, dinitrochlorobenzene is gradually enriched, which affects the rectification effect, and the tar needs to be di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/16C07C205/12
CPCC07C201/16C07C205/12
Inventor 王培兰杨怀青李珊
Owner SINOPEC NANJING RES INST OF CHEM IND CO LTD
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