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Novel nitration process of 3,5-binitro-4-chlorobenzotrifluoride

A technology of nitrotrifluorotoluene and chlorotrifluorotoluene, which is applied in 3 fields, can solve the problems of low reaction temperature, long reaction period, volatilization of nitric acid, etc., and achieves the effects of less corrosion of equipment, reduction and elimination of pollution, and convenient use.

Inactive Publication Date: 2018-08-10
JIANGSU DAHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has a high conversion rate and yield, but the reaction temperature is low, requiring a large amount of energy for cooling, resulting in energy waste
The reaction cycle is very long, and the nitric acid volatilizes, causing waste

Method used

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  • Novel nitration process of 3,5-binitro-4-chlorobenzotrifluoride
  • Novel nitration process of 3,5-binitro-4-chlorobenzotrifluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a 500mL four-necked flask, 35g of p-chlorotrifluorotoluene, 55g of 68% nitric acid, 10g of N,N-dimethyl-N-dodecyl-N-sulfonic acid propyl ammonium hydrogen sulfate were added successively, and the mixture was added to 50 Mix and stir at ℃ for 4 hours, cool and stand for phase separation, the upper layer of crude product is washed with water and neutralized by vacuum drying to obtain pure product 4-chloro-3-nitrotrifluorotoluene, which is used for the next step of dinitration reaction; the lower layer of waste acid After cyclohexane extraction and drying, it can be recycled for dinitration process.

Embodiment 2

[0021] In a 500mL four-necked flask, 10g of mononitrated product 4-chloro-3-nitrotrifluorotoluene prepared in Example 1, 10g of potassium nitrate, 20g of 30% oleum, 10 g of the treated waste acid was mixed and stirred at 80°C for 5 hours, left to stand for phase separation, and the upper crude product was washed with water, neutralized, purified, and dried in vacuo to obtain pure dinitration product 4-chloro-3,5-dinitrotrifluoro Toluene, the yield is 82%; the semi-waste acid in the lower layer is directly used in the mononitration reaction process.

Embodiment 3

[0023] In a 500mL four-necked flask, 10g of p-chlorotrifluorotoluene and 30g of semi-waste acid produced in Example 2 were added successively, mixed and stirred at 50°C for 3 hours, cooled and left to stand for phase separation, and the upper layer of the crude product was washed with water and neutralized by vacuum. The pure product 4-chloro-3-nitrotrifluorotoluene is obtained by drying, which is used for the next step of dinitration reaction; the lower layer waste acid is extracted with cyclohexane, dried, and filtered to remove the inorganic salt precipitation, which can be recycled for the dinitration process.

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Abstract

The invention discloses a novel nitration process of 3,5-binitro-4-chlorobenzotrifluoride. The novel nitration process comprises the following steps: mixing nitrate, fuming sulfuric acid and a waste acid according to a ratio so as to obtain a mixed acid, performing a dinitration reaction with 4-chlorine-3-nitro trifluorotoluene in a reaction kettle, after the completion of a reaction, performing phase separation so as to obtain a semi-waste acid and a target compound, applying the semi-waste acid to mononitratio reaction on p-chlorobenzotrifluoride, performing phase separation so as to obtaina waste acid and a mononitratio compound, treating the waste acid in a waste acid kettle, performing a dinitration reaction on the treated waste acid, and further recycling the waste acid. Compared with the prior art, the novel nitration process is capable of reducing and eliminating pollution from sources, is an environmental-friendly chemical process and has good industrial application prospects.

Description

a technical field [0001] The invention relates to a novel nitration process of 3,5-dinitro-4-chlorotrifluorotoluene, and belongs to the technical field of chemical material preparation. The method is suitable for the situation where p-chlorotrifluorotoluene and potassium nitrate are used as raw materials, and 3,5-dinitro-4-chlorotrifluorotoluene is synthesized by heating and stirring under normal pressure. Two background technology [0002] 3,5-Dinitro-4-chlorotrifluorotoluene is used as an intermediate in organic synthesis. This product is also an important intermediate in medicine and dyes. It is widely used in pharmaceuticals, pesticides, fine chemical intermediates and other industrial fields. It is an intermediate of the herbicide trifluralin in dry fields. The herbicides such as trifluralin produced by it have the characteristics of safety, high efficiency, low toxicity and low residue. They are widely used in cotton, soybean, sunflower and other dryland crops to cont...

Claims

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Application Information

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IPC IPC(8): C07C205/12C07C201/08C07C201/14
CPCC07C201/08C07C201/14C07C205/12
Inventor 郑龙洲张亮方东李付香
Owner JIANGSU DAHUA CHEM IND
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