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Separation method of 2,4-dichlorophenol and 2,5-dichlorophenol mixture

A technology of dichlorophenol and its mixture, which is applied in the fields of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc. It can solve the problems of high equipment requirements, difficult post-processing, complicated operation, etc., and achieves improved purity and simple method Ease of use, high purity results

Active Publication Date: 2014-10-08
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above separation methods have the disadvantages of high energy consumption, difficult post-processing, high equipment requirements, relatively large investment, complicated operation, and the use of a large amount of organic reagents and alkalis.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 50g of 2,4 / 2,5-dichlorophenol mixture in a 500ml flask, wherein the content of 2,4-dichlorophenol and 2,5-dichlorophenol is 20% and 80% respectively, then add 10g of morpholine , add 50ml of 95% (v / v) ethanol solution in the flask, stir and heat to make the raw materials fully mixed and dissolved, then place it at -5~0℃ for 7 days, colorless and transparent crystals precipitate out, after filtering , by NMR, UV, MS and other means, the crystal structure is obtained as a complex of 2,5-dichlorophenol and morpholine, while 2,4-dichlorophenol remains in the filtrate.

[0024] Continue to add 8 g of morpholine to the filtrate, then add 30 ml of 95% ethanol solution and stir evenly, and place it at -10 to 0° C. for a long enough time until colorless and transparent crystals are precipitated. After filtering, the obtained crystals are 2,4 - Complexes of dichlorophenol and morpholine.

[0025] The two complexes were vacuum filtered and distilled to obtain relatively pure ...

Embodiment 2

[0027] Add 80g of 2,4 / 2,5-dichlorophenol mixture in a 500ml flask, the content of 2,4-dichlorophenol and 2,5-dichlorophenol in the raw material is 20% and 80% respectively, then add 20g N -Methylmorpholine, add 80ml of anhydrous methanol to the flask, heat to dissolve the raw material, and then place it at 0-10°C for 4 days, a colorless and transparent crystal precipitates, after filtering, pass through NMR, UV, MS, etc. Means, the crystal structure is obtained as a complex of 2,5-dichlorophenol and N-methylmorpholine, while 2,4-dichlorophenol remains in the filtrate.

[0028] Continue to add 16g of N-methylmorpholine to the filtrate, then add 50ml of anhydrous methanol and stir evenly. After placing it at 0-10°C for a long enough time until colorless and transparent crystals precipitate, filter to obtain 2,4- Complexes of dichlorophenol and N-methylmorpholine.

[0029] The two complexes were vacuum filtered and distilled to obtain relatively pure 2,4-dichlorophenol and 2,5-d...

Embodiment 3

[0031] Add 100g 2,4 / 2,5-dichlorophenol mixture raw material in 500ml flask, the content of 2,4-dichlorophenol and 2,5-dichlorophenol in the raw material is respectively 20% and 80%, then add 40g N-ethylmorpholine, add 100ml tetrahydrofuran in the flask, heat to dissolve the raw material, then place it at room temperature for 3 days, there are colorless and transparent crystals precipitated, after filtration, by NMR, UV, MS and other means, it can be obtained The crystal structure is a complex of 2,5-dichlorophenol and N-ethylmorpholine, while 2,4-dichlorophenol remains in the filtrate.

[0032] Continue to add 25g of N-ethylmorpholine to the filtrate, then add 60ml of tetrahydrofuran and stir evenly. After placing it at 10-20°C for a long enough time until colorless and transparent crystals are precipitated, filter to obtain 2,4-dichloro Complexes of phenol and N-ethylmorpholine.

[0033]The two complexes were vacuum filtered and distilled to obtain relatively pure 2,4-dichlo...

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Abstract

The invention provides a method for separating a mixture of 2, 4-dichlorophenol and 2, 5-dichlorophenol. Based on the fundamental principle of supramolecular assembly, the method uses topology match between subjective molecules and objective molecules, and separates 2, 4 / 2, 5-mixed dichlorophenol by identifying molecules. Because of different molecular spatial structures of the 2, 4-dichlorophenol and the 2, 5-dichlorophenol and certain difference on polarities, specific different identifying capability among the subjective molecules exists, while difficulty or ease of intermolecular actions among the subjective molecules and other heterocyclic compound is different, therefore, the aim of separation can be achieved through identifying the molecules. The product obtained from the 2, 4 / 2, 5-mixed dichlorophenol by the method has high purity, and can be directly used after being separated, but does not need to be recrystallized to improve purity; and the method has high yield, is simple and practical, and is easy to industrialize.

Description

(1) Technical field [0001] The invention relates to a method for separating 2,4-dichlorophenol and 2,5-dichlorophenol mixture. (2) Background technology [0002] Dichlorophenol is an important organic intermediate in industry, mainly used in the production of pesticides, pharmaceuticals, and auxiliary products. Most of the dichlorophenols produced are mixed phenols, which can be better used by separating them. And 2,4-dichlorophenol is an important fine chemical product, which is mainly used in pesticides, medicines and auxiliary products. In recent years, the development of downstream products of p-dichlorophenol has been intensified in China, especially the successful development of antifungal agent TCS and pesticide oxadiazone in my country, which has brought excellent opportunities for the development of 2,4-dichlorophenol in my country. [0003] In the pesticide industry, it is mainly used in the production of insecticides phenanophos and herbicides, methyl ester herb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/30C07C37/86
Inventor 金志敏杨振李海燕
Owner ZHEJIANG UNIV OF TECH
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