Method for recycling wastes of trifluoromethyl phenylamine kettle residue

A technology for trifluoromethylaniline and waste, applied in the direction of amino compound purification/separation, etc., can solve problems such as polymerization reaction, achieve the effects of simple operation process, comprehensive utilization of resources, and reduction of pollutant discharge

Inactive Publication Date: 2015-03-25
JIANGSU FENGHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mixture can firstly obtain pure products of o-trifluoromethylaniline and m-trifluoromethylaniline with lower boiling points through conventional rectification, but when the remaining trifluoromethylaniline is less than 10% in the still residue, continue the rectification Violent polymerization is prone to occur, so how to separate useful m-trifluoromethylaniline and p-trifluoromethylaniline from the still residue is of great significance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 800g of trifluoromethylaniline residue and 24g of sodium carbonate to a 3L reactor, control the temperature at 140°C, and distill under reduced pressure (system internal pressure is 10mmHg) to obtain 480g of m-trifluoromethylaniline and p-trifluoromethylaniline The light components are collected for the next step of rectification.

[0020] Add 3000g of light components of m-trifluoromethylaniline and p-trifluoromethylaniline obtained in the previous step to a 5L rectification device, 90g of sodium carbonate, control the temperature at 140°C, and carry out rectification under reduced pressure (10mmHg in the system) , to obtain 702g of m-trifluoromethylaniline, with a purity of 98.5%, to obtain 63g of transition fractions (35.1% of m-trifluoromethylaniline, and 64.2% of p-trifluoromethylaniline), to obtain 2003g of p-trifluoromethylaniline, with a purity of 98.1% . Example 2

Embodiment 2

[0021] Add 800g of trifluoromethylaniline residue, 16g of potassium hydroxide to a 3L reactor, control the temperature at 80°C, and distill under reduced pressure (5mmHg in the system) to obtain 482g of m-trifluoromethylaniline and p-trifluoromethylaniline. Light components are collected for the next step of rectification.

[0022] Add 3000g of light components of m-trifluoromethylaniline and p-trifluoromethylaniline obtained in the previous step to a 5L rectification device, 60g of potassium hydroxide, control the temperature at 80°C, and carry out refining under reduced pressure (5mmHg in the system). Distillation, to obtain 702g m-trifluoromethylaniline, purity 98.5%, to obtain 61g of transition fraction (m-trifluoromethylaniline 35.1%, p-trifluoromethylaniline 64.2%), to obtain 2005g p-trifluoromethylaniline, purity 98.1 %.

Embodiment 3

[0024] Add 800g of trifluoromethylaniline residue and 20g of sodium hydroxide to the 3L reactor, control the temperature at 90°C, and distill under reduced pressure (6mmHg in the system) to obtain 481g of m-trifluoromethylaniline and p-trifluoromethylaniline. Light components are collected for the next step of rectification.

[0025] Add 3000g light components of m-trifluoromethylaniline and p-trifluoromethylaniline obtained in the previous step to a 5L rectification device, 80g of sodium hydroxide, control the temperature at 90°C, and carry out refining under reduced pressure (6mmHg in the system). Distillation, to obtain 702g m-trifluoromethylaniline, purity 98.5%, to obtain 62g transition fraction (m-trifluoromethylaniline 35.1%, p-trifluoromethylaniline 64.2%), to obtain 2004g p-trifluoromethylaniline, purity 98.1 %.

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Abstract

The invention discloses a method for recycling wastes of trifluoromethyl phenylamine kettle residues. The method comprises the steps of 1) vacuum distillation: by taking the trifluoromethyl phenylamine kettle residues as raw materials, adding inorganic alkali according to the proportion of 2-3% of the mass of the trifluoromethyl phenylamine kettle residues, performing vacuum distillation to obtain a light-component mixture containing m-trifluoromethyl phenylamine and p-trifluoromethyl phenylamine; and 2) vacuum rectification: adding the inorganic alkali into the light-component mixture obtained in the step 1), and performing rectification to obtain m-trifluoromethyl phenylamine and p-trifluoromethyl phenylamine respectively. According to the method disclosed by the invention, a polymerization phenomenon during the process of distillation and rectification is effectively prevented by adopting the inorganic alkali; the method is simple in operation process and easy in industrial production; and by adopting the technical scheme of the method, the discharge of pollutants of the production process is reduced, and the comprehensive recycling of the solid wastes is realized.

Description

technical field [0001] The present invention relates to a method for separation and purification of pesticide chemical products, in particular to a method for separation and purification of trifluoromethylaniline residue, in particular to the further separation of effective components of waste from trifluoromethylaniline residue to obtain m-trifluoro Methylaniline and p-trifluoromethylaniline. Background technique [0002] Trifluoromethylaniline has three isomers, which are o-, m-, and p-trifluoromethylaniline. It is an important fluorine-containing organic intermediate and is widely used in the fields of medicine, pesticides, dyes, etc., especially in the synthesis of multi- A new type of high-efficiency, low-toxic fluorine-containing pesticide has attracted much attention from the pesticide industry at home and abroad. [0003] m-trifluoromethylaniline and p-trifluoromethylaniline are important medicines, pesticides, dyes and material intermediates, and are two important ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/86
Inventor 李琦郑龙生方东
Owner JIANGSU FENGHUA CHEM IND
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