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Method for processing and utilizing trifluoromethyl aniline distillation still residue

A technology of trifluoromethylaniline and distillation pots, which is applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the problems of large environmental hazards, underutilization, high cost of incineration, etc., and achieve high Economic value, less harm, and the effect of reducing waste residue

Active Publication Date: 2009-09-23
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because this kind of kettle residue contains fluorine, the cost of incineration treatment is very high, and it is harmful to the environment, which is a major problem in the treatment of three wastes
The 4-trifluoromethylaniline contained therein is a key pharmaceutical and pesticide intermediate, and has the highest price among the three isomers of trifluoromethylaniline. However, it has not been fully utilized yet.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024]Add 405g of still residue (4-trifluoromethylaniline content 46%) and 6480g of 10% hydrochloric acid into a 10L three-necked flask, stir and dissolve at 30°C, then add 675g of 30% hydrogen peroxide, heat up to 60°C and stir for 4 hours, cool to After standing at room temperature, the layers were separated, and the oil in the lower layer was simply distilled under reduced pressure at 2kPa, and the fraction at 80-120°C was collected to obtain 340g of orange liquid, with a content of 78% in 2,6-dichloro-4-trifluoromethylaniline. Put the crude fraction into the rectification kettle, the theoretical plate of the rectification column is about 50, and rectify under the reduced pressure to 2kPa. At the same time, take samples to track and analyze the content of the fractions, and collect 2,6-dichloro-4-trifluoromethylaniline respectively For fractions with a mass content of less than 90% and greater than or equal to 90%, 100g of fractions with a content of less than 90% and 230g o...

Embodiment 2

[0026] Add 300g of still residue (30% content of 4-trifluoromethylaniline) and 7200g of 5% hydrochloric acid into a 10L three-necked flask, stir and dissolve at 20°C, then add 172g of 70% hydrogen peroxide, heat up to 70°C and stir for 4 hours, cool to After standing at room temperature, the layers were separated, and the oil in the lower layer was simply distilled under reduced pressure at 2kPa, and the fractions at 80-120°C were collected to obtain 235g of orange liquid, with a content of 54%. Put the crude fraction into the rectification kettle, the theoretical plate of the rectification column is about 60, and rectify under reduced pressure to 5kPa. At the same time, take samples to track and analyze the content of the fractions, and collect 2,6-dichloro-4-trifluoromethylaniline respectively For fractions with a mass content of less than 90% and greater than or equal to 90%, 106 g of fractions with a content of less than 90% and 110 g of fractions with a content of more tha...

Embodiment 3

[0028] Add 600g of still residue (4-trifluoromethylaniline content 80%) and 4800g of 15% hydrochloric acid to a 10L three-necked flask, stir and dissolve at 5°C, then add 400g of 50% hydrogen peroxide, heat up to 40°C and stir for 6 hours, cool to After standing at room temperature, the layers were separated, and the oil in the lower layer was simply distilled under reduced pressure at 2kPa, and the fractions at 80-120°C were collected to obtain 810g of orange liquid with a content of 84%. Put the crude fraction into the rectification kettle, the theoretical plate of the rectification column is about 40, and rectify under reduced pressure to 100Pa, and at the same time, take samples to track and analyze the content of the fractions, and collect 2,6-dichloro-4-trifluoromethylaniline respectively For fractions with a content of less than 90% and greater than or equal to 90%, 139g of fractions with a content of less than 90% and 658g of fractions with a content of more than 90% we...

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PUM

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Abstract

The invention discloses a method for processing and utilizing trifluoromethyl aniline distillation still residue, comprising the following steps of: dissolving the trifluoromethyl aniline distillation still residue into hydrochloric acid at the temperature of 5 to 30 DEG C, adding hydrogen peroxide, reacting for 4 to 6 hours at the reaction temperature of 30 to 90 DEG C; after the reaction is finished, resting for delamination, taking the oil layer at the lower layer, carrying out reduced pressure distillation to obtain crude product of 2, 6-dichloro-4-trifluoromethyl aniline; carrying out the reduced pressure distillation again, simultaneously executing sampling and analyzing the content of distillates by tracking, respectively collecting the distillate with the mass content of 2, 6-dichloro-4-trifluoromethyl aniline being lower than 90 percent and the distillate with the mass content of the 2, 6-dichloro-4-trifluoromethyl aniline being more than 90 percent; taking the distillate with the mass content of the 2, 6-dichloro-4-trifluoromethyl aniline being more than 90 percent; and obtaining the 2, 6-dichloro-4-trifluoromethyl aniline with the mass content of more than 99 percent by a melting crystallization method. The method changes waste into valuable, obtains products with higher economic value by converting the distillation still residues which are hard to be processed, reduces the waste residues generated in the production process of trifluoromethyl aniline, and has small harm to the environment in the processing process.

Description

(1) Technical field [0001] The present invention relates to a method for treating and utilizing trifluoromethylaniline still residue, in particular to the waste treatment of trifluoromethylaniline still residue, and at the same time utilizing useful components therein to produce 2,6-dichloro-4-tri Fluoromethylaniline. (2) Background technology [0002] Trifluoromethylaniline is an important medicine, pesticide, dye and material intermediate, and its main industrial production method is to obtain the product through nitration, reduction and rectification of benzotrifluoride. During the above production process, three isomers of trifluoromethylaniline are mainly produced: 2-trifluoromethylaniline, 3-trifluoromethylaniline and 4-trifluoromethylaniline. The ratio of the three isomers varies with the reaction conditions, among which 3-trifluoromethylaniline is the main one. In the rectification process, 2-trifluoromethylaniline is distilled out first, followed by 3-trifluoromet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/74
Inventor 杜晓华李惠跃胡智燕陈静华任旭康吴江伟徐振元
Owner ZHEJIANG UNIV OF TECH