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Clean preparation method of 2, 4-dichloro-3, 5-dinitrobenzotrifluoride

A technology of dinitrotrifluorotoluene and dichlorotrifluorotoluene is applied in the field of clean preparation of 2,4-dichloro-3,5-dinitrotrifluorotoluene, and can solve the problems of strong corrosiveness, tail gas pollution, There are many problems such as by-products, so as to achieve the effects of less equipment corrosion, less waste acid discharge, and convenient use.

Inactive Publication Date: 2013-09-18
JIANGSU DAHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Not only the emission pollution is serious, but also highly corrosive, with many by-products, and the exhaust pollution is also very serious

Method used

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  • Clean preparation method of 2, 4-dichloro-3, 5-dinitrobenzotrifluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 500mL four-neck flask, add 35 g of 2,4-dichlorobenzotrifluoride, 30 g of 95% nitric acid, and 45 g of 98% concentrated sulfuric acid in sequence, mix and stir at 40°C for 2 hours, cool and stand still. Separation, the crude product in the upper layer is washed with water, neutralized and dried in vacuum to obtain the pure product 2,4-dichloro-3-nitrobenzotrifluoride, which is used for the next dinitration reaction; the waste acid in the lower layer can be recovered by extracting and drying with cyclohexane For dinitration process.

Embodiment 2

[0020] In a 500mL four-neck flask, add 35 g of 2,4-dichlorobenzotrifluoride, 55 g of 68% nitric acid, and N,N-dimethyl-N-dodecyl-N-sulfonic acid propyl sulfuric acid in sequence Ammonium hydrogen 10 g, mixed and stirred at 50°C for 4 hours, cooled, allowed to stand and phase separated, the crude product in the upper layer was washed with water and dried in vacuum to obtain the pure product 2,4-dichloro-3-nitrotrifluorotoluene, which was used for The next step of the dinitration reaction; the waste acid in the lower layer can be recovered for the dinitration process by extracting and drying with cyclohexane.

Embodiment 3

[0022] In a 500mL four-necked flask, add the mononitrated product 2,4-dichloro-3-nitrobenzotrifluoride 10 g, ammonium nitrate 10 g, and 20% oleum 10 g successively, which were prepared in Example 1, and implement 10 g of the treated waste acid produced in Example 1 was mixed and stirred for 4 hours at 100° C., cooled to 70° C., left to stand for phase separation, and the crude product in the upper layer was cooled to normal temperature for washing, neutralization, refining, and vacuum drying. The pure dinitration product 2,4-dichloro-3,5-dinitrobenzotrifluoride was obtained with a yield of 80%; the semi-waste acid in the lower layer was directly used in the mononitration reaction process.

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Abstract

The invention discloses a clean preparation method of 2, 4-dichloro-3, 5-dinitrobenzotrifluoride. The clean preparation method comprises the following steps of: firstly taking 2, 4-dichlorobenzotrifluoride as a raw material for performing primary nitration reaction, and separating into a waste acid and a primary nitration intermediate after the reaction; and further mixing ammonium nitrate and fuming sulfuric acid with the waste acid after concentration treatment into a mixed acid, further performing secondary nitration reaction with the primary nitration intermediate, and separating into a semi-waste acid and a secondary nitration target compound, namely the 2, 4-dichloro-3, 5-dinitrobenzotrifluoride after the reaction, wherein the semi-waste acid after the secondary nitration separation can be directly recycled in the primary nitration reaction for mixing with the 2, 4-dichlorobenzotrifluoride so as to perform the new round of the primary nitration reaction. The clean preparation method has the advantages that the ammonium nitrate is adopted for replacing the nitric acid, raw materials are extensive in sources, the use is convenient, and the corrosion to the environment and equipment is smaller; and the waste acid produced by primary nitration can be used for secondary nitration reaction after treatment, and the semi-waste acid after secondary nitration can also be directly used for primary nitration reaction, so that circular economy is realized and the emission of the waste acid is also reduced.

Description

technical field [0001] The invention relates to a new method for the clean preparation of 2,4-dichloro-3,5-dinitrobenzotrifluoride, belonging to the technical field of chemical material preparation. The method is applicable to the occasion of synthesizing 2,4-dichloro-3,5-dinitrobenzotrifluoride by heating and stirring under normal pressure with 2,4-dichloro-benzotrifluoride and ammonium nitrate as raw materials. Background technique [0002] 2,4-dichloro-3,5-dinitrobenzotrifluoride is used as an intermediate in fine organic synthesis, and many important pharmaceutical products, agricultural chemicals, dyes, etc. can be synthesized from it. It is widely used in important industrial fields such as pharmaceuticals, pesticides, and fine chemical intermediates. The existing process often uses 2,4-dichloro-trifluoromethylbenzene as raw material, and prepares mononitride 2,4 by reacting 2,4-dichloro-trifluorotoluene with semi-waste acid (dinitration reaction waste acid) -dichlor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/08C07C205/12
Inventor 郑龙洲方东李付香
Owner JIANGSU DAHUA CHEM IND
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