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Method for separating 2,5-dichlorophenol and 2,4-dichlorophenol

A technology of dichlorophenol and mixture, which is applied in the field of separation of 2,5-dichlorophenol and 2,4-dichlorophenol, can solve the problems of separation and separation cost, low processing cost, complex process, etc., and achieve low processing cost, The effect of appropriate concentration of reactants and simple operation process

Inactive Publication Date: 2016-07-27
SICHUAN FOURSTAR BIOTECH RANDD CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims to solve the problems that 2,4-dichlorophenol and 2,5-dichlorophenol cannot be completely separated, the separation cost is high, and the process is complicated in the prior art, and a new method for separating 2,5-dichlorophenol is proposed. The method of phenol and 2,4-dichlorophenol, after separating 2,5-dichlorophenol by urea addition method, and then repeatedly purifying by ammonia solution, crystallization and other steps, a small amount of 2,5-dichlorophenol Separation from 2,4-dichlorophenol, so as to realize the complete separation of 2,5-dichlorophenol and 2,4-dichlorophenol, which has the advantages of low processing cost, simple operation process and low energy consumption

Method used

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Examples

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Embodiment 1

[0032] A method for separating 2,5-dichlorophenol and 2,4-dichlorophenol, comprising the following steps:

[0033] A. Urea addition

[0034] Add urea to the mixture of 2,5-dichlorophenol and 2,4-dichlorophenol, react at 90°C, lower the temperature to below 90°C, then add organic solvent, and filter with suction after cooling to obtain filtrate and filter cake ;Add water to the filter cake, raise the temperature to 60°C, continue the reaction, and then separate the liquids to obtain an organic phase and an aqueous phase. The organic phase is 2,5-dichlorophenol; after removing the organic solvent from the filtrate, 2,5 - a mixture of dichlorophenol and 2,4-dichlorophenol;

[0035] B. Ammonia treatment

[0036] To the mixture of 2,5-dichlorophenol and 2,4-dichlorophenol obtained in step A, add water and ammonia water in an amount 0.5 times the total moles of the mixture, raise the temperature to 40°C, and continue the reaction until the temperature of the solution drops to room...

Embodiment 2

[0039] A method for separating 2,5-dichlorophenol and 2,4-dichlorophenol, comprising the following steps:

[0040] A. Urea addition

[0041] Add urea to the mixture of 2,5-dichlorophenol and 2,4-dichlorophenol, react at 120°C, lower the temperature to below 90°C, then add organic solvent, and filter with suction after cooling to obtain filtrate and filter cake ;Add water to the filter cake, raise the temperature to 90°C, continue the reaction, and then separate the liquids to obtain an organic phase and an aqueous phase, the organic phase is 2,5-dichlorophenol; after removing the organic solvent from the filtrate, 2,5 - a mixture of dichlorophenol and 2,4-dichlorophenol;

[0042] B. Ammonia treatment

[0043]To the mixture of 2,5-dichlorophenol and 2,4-dichlorophenol obtained in step A, add water and ammonia water in an amount 1.5 times the total moles of the mixture, raise the temperature to 80°C, and continue the reaction until the temperature of the solution drops to room...

Embodiment 3

[0047] A method for separating 2,5-dichlorophenol and 2,4-dichlorophenol, comprising the following steps:

[0048] A. Urea addition

[0049] Add urea to the mixture of 2,5-dichlorophenol and 2,4-dichlorophenol, react at 100°C, lower the temperature to below 90°C, then add organic solvent, and filter with suction after cooling to obtain filtrate and filter cake ;Add water to the filter cake, raise the temperature to 80°C, continue the reaction, and then separate the liquids to obtain an organic phase and an aqueous phase, the organic phase is 2,5-dichlorophenol; after removing the organic solvent from the filtrate, 2,5 - a mixture of dichlorophenol and 2,4-dichlorophenol;

[0050] B. Ammonia treatment

[0051] To the mixture of 2,5-dichlorophenol and 2,4-dichlorophenol obtained in step A, add water and ammonia water in an amount 1 times the total molar number of the mixture, raise the temperature to 60°C, and continue the reaction until the temperature of the solution drops t...

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PUM

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Abstract

The invention discloses a method for separating 2,5-dichlorophenol and 2,4-dichlorophenol, belonging to the technical field of fine chemical industry. According to the method, the 2,5-dichlorophenol is separated out by a urea addition process, and then the less 2,5-dichlorophenol is separated from the 2,4-dichlorophenol by steps of ammonia water dissolution, crystallization and the like, so that the 2,5-dichlorophenol is thoroughly separated from the 2,4-dichlorophenol. Compared with the prior art, the method has the advantages of being low in cost, simple in operation technology and less in energy consumption.

Description

technical field [0001] The invention relates to a method for separating 2,5-dichlorophenol and 2,4-dichlorophenol, belonging to the technical field of fine chemicals. Background technique [0002] Dichlorophenol is an important class of organic intermediates. Among many dichlorophenol compounds, 2,5-dichlorophenol and 2,4-dichlorophenol play a very prominent role. 2,5-Dichlorophenol is a key intermediate of the herbicide dicamba, a nitrogen fertilizer synergist and a leather antifungal agent. 2,4-Dichlorophenol is an important fine chemical product, mainly used in pesticides, medicines and auxiliary products. [0003] Dichlorophenol produced by hydrolysis of 1,2,4-trichlorobenzene has three isomers: 2,5-dichlorophenol, 2,4-dichlorophenol and 3,4-dichlorophenol. 3,4-dichlorophenol can be separated by rectification because its boiling point is about 40°C higher than that of 2,5-dichlorophenol and 2,4-dichlorophenol, while 2,5-dichlorophenol and 2,4- Dichlorophenol is diffic...

Claims

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Application Information

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IPC IPC(8): C07C37/88C07C37/84C07C39/30
CPCC07C37/88C07C37/84C07C39/30
Inventor 李舟齐鸿梁剑罗茜彭舟张弦张华王蕾
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP
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