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Method for separating 2,4-Dichlorophenol and 2,6-Dichlorophenol

A technology of dichlorophenol and mixture, applied in the field of separation 2, can solve the problems of small investment, high equipment requirements, and difficult post-processing, etc., and achieve the effects of industrial scale-up, rapid separation, and low implementation cost

Active Publication Date: 2010-07-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The small difference in properties makes it difficult to achieve the expected separation effect by traditional distillation methods
Also, rectification is energy-intensive and not ideal
[0009] (2) Hermann A et al. have reported utilizing zeolite to adsorb and separate 2,4-dichlorophenol, and using zeolite as an adsorbent to separate chlorophenols can contain 2,4-dichlorophenol and 2,6-dichlorophenol 2,4-dichlorophenol is isolated from the mixture, but the method is complicated to operate and has low efficiency, which is not suitable for industrialization
This method has less investment than simple dissociation extraction equipment, and is simple to operate, but it still cannot avoid the use of a large amount of organic solvents, and the purity of its products is not ideal.
[0013] The above separation methods have the disadvantages of high energy consumption, difficult post-processing, high requirements for equipment conditions, correspondingly large investment, and complicated operation.

Method used

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  • Method for separating 2,4-Dichlorophenol and 2,6-Dichlorophenol

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0039]In a 200ml beaker, add 150ml ethanol and 50g 2,4 dichlorophenol, 2,6-dichlorophenol mixture, detect through high performance liquid chromatography (the same below) wherein 2,4-dichlorophenol and 2,6-dichlorophenol The content of phenol was 50% and 50% respectively, then 16g of morpholine was added, stirred and heated at 70° C. for 2 minutes until the solution was clear. Placed under the greenhouse for 7 days, colorless and transparent crystals were precipitated, and filtered under reduced pressure to obtain 31.5 g of filter cake crystals and filtrate. compound, and 2,4-dichlorophenol is left in the filtrate, and then high-purity 2,4-dichlorophenol 22.8g can be obtained by distillation, the yield is 91%, and the purity is 96% (high performance liquid Phase chromatography detection, the same below). Use 100ml of ethanol to recrystallize the crude 2,6-dichlorophenol once, add it to 60ml of 10% dilute hydrochloric acid solution for a full reaction at room temperature, then ...

example 2

[0041] In a 500ml beaker, add 200ml methyl alcohol and 50g 2,4 dichlorophenol, 2,6-dichlorophenol mixture, wherein the content of 2,4-dichlorophenol and 2,6-dichlorophenol is respectively 60% and 40%, then add 16g of triethylenediamine, stir and heat at 60°C for 2 minutes until the solution is clear. Placed under the greenhouse for 6 days, colorless and transparent crystals precipitated, and filtered under reduced pressure to obtain 30.8 g of filter cake crystals and filtrate. The crystals were 2,6-dichlorophenol crude product, which was 2,6-dichlorophenol and triethylene The compound of diamine, while 2,4-dichlorophenol is left in the filtrate, and then 28.0 g of high-purity 2,4-dichlorophenol can be obtained by distillation, the yield is 93%, and the purity is 98%. Recrystallize the crude product of 2,6-dichlorophenol once with 100ml of methanol, add it to 60ml of 10% dilute hydrochloric acid solution for a full reaction at room temperature, then add 60ml of benzene for extr...

example 3

[0043] Add 150ml ethanol and 50g 2,4 dichlorophenol, 2,6-dichlorophenol mixture in 200ml beaker, wherein 2,4-dichlorophenol and 2, the content of 6-dichlorophenol are respectively 60% and 40%, then add 12.5g piperazine, stir and heat at 70°C for 2 minutes until the solution is clear. Placed at room temperature for 8 days, colorless and transparent crystals precipitated, and filtered under reduced pressure to obtain 30.5 g of filter cake crystals and filtrate. The crystals were crude 2,6-dichlorophenol, which was the mixture of 2,6-dichlorophenol and piperazine. The complex, while 2,4-dichlorophenol is left in the filtrate, and then high-purity 2,4-dichlorophenol 29.1g can be obtained by distillation, the yield is 97%, and the purity is 98%. Use 100ml of acetone to recrystallize the crude 2,6-dichlorophenol once, add it to 60ml of 10% dilute hydrochloric acid solution for a full reaction at room temperature, then add 60ml of chloroform for extraction, let it stand for layers, a...

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Abstract

The invention discloses a method for separating 2,4-Dichlorophenol and 2,6-Dichlorophenol, comprising the following steps: dissolving the mixture of the 2,4-Dichlorophenol and the 2,6-Dichlorophenol in an organic solvent, adding alkalic organism, stirring and reacting at the temperature of 40-80 DEG C until the reaction liquid is clear, cooling the reaction liquid after the reaction is finished, standing and precipitating crystals, filtering to obtain a filter cake A and a filtrate A, and retaining the 2,4-Dichlorophenol in the filtrate A, wherein the filter cake A is a crude product of the 2,6-Dichlorophenol; the alkalic organism is triethylene diamine, morpholine, piperazidine, ethylpiperazine or methyl piperazine; and the organic solvent is ethanol, methanol, acetone or ethyl acetate. The invention has higher separation efficiency and only need crystallization for one time; the total yield of the 2,4-Dichlorophenol is 90-95%, and the purity thereof is 96-99%; the total yield of the 2,6-Dichlorophenol is 77-89%, and the purity thereof is 90-99%; and the invention has the advantages of simple operation, good repeatability and low implementation cost, and is favor of industrialized scale-up.

Description

(1) Technical field [0001] The invention relates to a method for separating 2,4-dichlorophenol and 2,6-dichlorophenol. (2) Background technology [0002] 2,4-Dichlorophenol is an important fine chemical product, mainly used in pesticides, medicines and auxiliary products. Due to the intensified development of downstream products of p-dichlorophenol in China in recent years, especially the successful development of antifungal agent TCS and pesticide oxadiazone in my country, it has brought great benefits to the application and development of 2,4-dichlorophenol in my country. opportunity. [0003] In the pesticide industry, 2,4-dichlorophenol is mainly used in the production of insecticides phenophos and herbicides, methyl ester herbicides, biben, dichlorophenoxy acid and its esters; in the pharmaceutical industry for the production of Insect repellent sulfur bisdichlorophene; used in the auxiliary industry to produce preservative TCS. However, the amount of 2,4-dichlorophen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/30C07C37/86
Inventor 金志敏胡来文杨振陈刚
Owner ZHEJIANG UNIV OF TECH
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