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Preparation method of 4-(2,4-dichlorophenoxy) phenol

A technology of dichlorophenoxy and phenol, applied in the 4-(2 field, can solve the problems of difficult removal of sodium bisulfite, increased cost of sulfuric acid, no way to recover sulfuric acid, etc., achieves low price, solves the problem of three wastes, and reduces production cost effect

Inactive Publication Date: 2011-07-20
YIFAN AGRI CHEM PLANT ZHEJIANG PROV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the diazotization reaction using sodium nitrite, a large amount of sodium bisulfite will be generated, and sodium bisulfite is difficult to remove, resulting in no way to recycle sulfuric acid, resulting in a large amount of salty and strongly acidic wastewater, which brings great harm to the treatment of three wastes. problem, and the cost of sulfuric acid also increases a lot

Method used

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Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0009] Specific embodiment 1: in reactor, add xylene 1000L, 60% recovery sulfuric acid 550kg, 4-(2,4-dichlorophenoxy group) aniline 267kg (content 95%), be warming up to 120 o C, keep warm for two hours. After the heat preservation is over, cool down to 0~5 o Add 130kg of nitrosyl sulfuric acid (M=127) dropwise to C, and keep the temperature at 0~5 o C, keep warm for 2-3 hours after dripping, and set aside. Above-mentioned diazonium solution is warmed up to 120 o C reflux, dropwise add 525kg of 60% sulfuric acid, keep the temperature at 115~120 o C, add in about 3 hours, and then keep warm for 1~2 hours. After the heat preservation is over, cool down to 70~80 o C. Stand for stratification, recover the lower acid water layer (1100kg, content 60~65%), add 1500L water to wash the oil layer, stand for stratification, and desolvate the oil phase to 120 o C, 255kg of 4-(2,4-dichlorophenoxy)phenol was obtained, the content was 95%, and the yield was 95%.

specific Embodiment 2

[0010] Specific embodiment 2: in reactor, add xylene 1000L, 60% recovery sulfuric acid 550kg, 4-(2,4-dichlorophenoxy group) aniline 267kg (content 95%), be warming up to 120 o C, keep warm for two hours. After the heat preservation is over, cool down to 0~5 o Add 260kg of nitrosyl sulfuric acid (M=127) dropwise to C, and keep the temperature at 0~5 o C, keep warm for 2-3 hours after dripping, and set aside. Above-mentioned diazonium solution is warmed up to 120 o C reflux, dropwise add 525kg of 60% sulfuric acid, keep the temperature at 115~120 o C, add in about 3 hours, and then keep warm for 1~2 hours. After the heat preservation is over, cool down to 70~80 o C. Stand for stratification, recover the lower acid water layer (1200kg, content 60~65%), add 1500L water to wash the oil layer, stand for stratification, and desolvate the oil phase to 120 o C, 260kg of 4-(2,4-dichlorophenoxy)phenol was obtained, the content was 95%, and the yield was 96.8%.

specific Embodiment 3

[0011] Specific embodiment 3: in reactor, add xylene 1000L, 60% recovery sulfuric acid 550kg, 4-(2,4-dichlorophenoxy group) aniline 267kg (content 95%), be warming up to 120 o C, keep warm for two hours. After the heat preservation is over, cool down to 0~5 o Add 520kg of nitrosyl sulfuric acid (M=127) dropwise to C, and keep the temperature at 0~5 o C, keep warm for 2-3 hours after dripping, and set aside. Above-mentioned diazonium solution is warmed up to 120 o C reflux, dropwise add 525kg of 60% sulfuric acid, keep the temperature at 115~120 o C, add in about 3 hours, and then keep warm for 1~2 hours. After the heat preservation is over, cool down to 70~80 o C. Stand for stratification, recover the lower acid water layer (1450kg, content 60~65%), add 1500L water to wash the oil layer, stand for stratification, and desolvate the oil phase to 120 o C, 250kg of 4-(2,4-dichlorophenoxy)phenol was obtained, the content was 95%, and the yield was 93.1%.

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Abstract

The invention relates to a preparation method of 4-(2,4-dichlorophenoxy) phenol. The method is characterized by comprising the following steps of: diazotizing 4-(2,4-dichlorophenoxy) aniline in a sulfuric acid medium with nitrosylsulfuric acid; and hydrolyzing in the sulfuric acid medium to obtain the 4-(2,4-dichlorophenoxy) phenol. The adopted nitrosylsulfuric acid is an industrial byproduct which absorbs sulfur dioxide, and has very low price. Due to the adoption of a new process, the problem of three wastes is solved, and the production cost is lowered.

Description

technical field [0001] The invention relates to a preparation method of 4-(2,4-dichlorophenoxy)phenol, in particular to a kind of simple disassembly and compact structure which can conveniently form a variety of different filtration forms and provide a variety of water qualities at the same time. , The preparation method of 4-(2,4-dichlorophenoxy)phenol which is easy to maintain. Background technique [0002] Diclofop products are systemic herbicides. The herbicide can be absorbed through roots and leaves, and is only effective against annual grass weeds. It is safe for dicotyledonous plants except cotton. Crabgrass and dogtail have effects, so they are widely used. At present, the production of diclofop-methyl requires the use of intermediate 4-(2,4-dichlorophenoxy)phenol, but the existing process for preparing 4-(2,4-dichlorophenoxy)phenol basically uses 4-(2,4-dichlorophenoxy)aniline is diazotized with sodium nitrite in sulfuric acid medium, and then hydrolyzed in sulf...

Claims

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Application Information

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IPC IPC(8): C07C43/295C07C41/26
Inventor 吴克崇吴贯中王学胜陈光海
Owner YIFAN AGRI CHEM PLANT ZHEJIANG PROV
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