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Method for separating dichlorophenol mixture by cross-current dissociation extraction

A dichlorophenol and mixture technology, applied in the field of chemical separation of mixed dichlorophenol, can solve the problems of high equipment requirements, difficult separation, low product yield, etc., and achieve simple process and equipment, low production cost and high product quality. The effect of high purity

Inactive Publication Date: 2010-10-20
NANJING NORMAL UNIVERSITY
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Problems solved by technology

[0003] The properties of 2,4-dichlorophenol, 2,6-dichlorophenol, and 2,4,6-trichlorophenol are similar, especially the physical and chemical properties of 2,4-dichlorophenol and 2,6-dichlorophenol are very similar. Close, it is difficult to completely separate by ordinary rectification and consumes a lot of energy
Before the present invention, there were reports of dissociation, extraction, separation and purification of 2,4-dichlorophenol. It was a double-tower extraction system composed of two rotary extraction towers for continuous countercurrent extraction of mixed dichlorophenols. However, the disadvantage of this method is that the requirements for equipment conditions are relatively high. , the investment is relatively large, the operation is complicated, the consumption of organic solvent and alkali is large, and the product yield is low

Method used

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  • Method for separating dichlorophenol mixture by cross-current dissociation extraction
  • Method for separating dichlorophenol mixture by cross-current dissociation extraction

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Cross-flow dissociation extraction method for separating dichlorophenol mixture, refer to figure 1 Shown technological process and process parameter shown in table 1, 2, in raw material batching kettle 1, 30g raw material thick dichlorophenol (in terms of mass percent, containing 2,4-dichlorophenol 89%, 2,6-dichlorophenol Phenol 6%, 2,4,6-trichlorophenol 5%) and 100mL organic solvent tetrachlorethylene are made into raw material solution and enter raw material solution storage tank 2, prepare sodium hydroxide aqueous solution 45mL simultaneously (internal dissolved solid sodium hydroxide 1.5g) and enter the lye storage tank 3, the first time 20mL lye ( figure 1 The middle stream ②) is added to the extraction kettle 4 of I, and all the raw materials are added ( figure 1 Middle stream ①), stirring at room temperature, stirring shaft speed 150 rpm, stirring for about 10 minutes, standing still for about 20 minutes, taking out the organic layer R1 (lower layer) and water l...

Embodiment 2

[0027] Substantially the same as Example 1, but the tetrachlorethylene consumption is changed into 80mL.

Embodiment 3

[0029] Substantially the same as Example 1, but the tetrachlorethylene consumption is changed into 120mL.

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Abstract

The invention discloses a method for separating dichlorophenol mixture by cross-current dissociation extraction. The method includes the following steps that: the dichlorophenol mixture as a material is dissolved in organic solvent to prepare mixed dichlorophenol solution, aqueous inorganic alkali solution is adopted as an extracting agent, and after cross-current dissociation extraction, the organic layer is distilled, so that 2, 4-dichlorophenol is obtained. Since the method adopts cross-current dissociation extraction to separate the dichlorophenol mixture, the technique and equipment are simple, the usages of the organic solvent and the alkali is small, the consumption of material and energy is reduced, 98 percent of 2, 4-dichlorophenol can be obtained, meanwhile, the recovery rate of2, 4-dichlorophenol is more than 95 percent, and the recovery rate of the organic solvent exceeds 99 percent.

Description

technical field [0001] The invention relates to a chemical separation method of mixed dichlorophenols, in particular to a cross-flow dissociation extraction separation method of mixed dichlorophenols. Background technique [0002] An important use of 2,4-dichlorophenol is to produce dichlorophenoxy acid and its ester herbicides. At present, most of these products use mixed dichlorophenol with a 2,4-dichlorophenol content of about 90%, of which more than 90% is produced by the enterprise itself by the direct chlorination of phenol. When the chlorination of phenol reaches a certain depth, the chlorinated product is mainly 2,4-dichlorophenol (about 90%), and the main impurities are 2,6-dichlorophenol and 2,4,6-trichlorophenol. Due to the low purity of 2,4-dichlorophenol, the yield of dichlorophenoxy acid and its ester herbicides produced is low and the amount of three wastes is large. With the increasing emphasis on environmental protection and the requirement for the purity ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/30C07C37/72
Inventor 林军顾正桂黄群群陈远新
Owner NANJING NORMAL UNIVERSITY
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