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Synthesis method of 2, 5-dichlorophenol

A synthesis method and technology of dichlorophenol, applied in directions such as organic chemistry, can solve problems such as unfavorable clean production, large equipment investment, long reaction time, etc., and achieve the effects of increasing effective output, reducing raw material consumption, and reducing three wastes

Inactive Publication Date: 2012-12-26
SHANDONG WEIFANG RAINBOW CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods generally have some disadvantages: long reaction route, long reaction time, complicated process, large equipment investment, serious corrosion, and a large amount of waste acid or waste alkali produced after the reaction, which pollutes the environment and is not conducive to clean production.

Method used

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  • Synthesis method of 2, 5-dichlorophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 636g of water to a 1000ml four-neck flask, then take 50g of concentrated sulfuric acid with a mass fraction of 98%, and add it to the above flask under stirring to form a 3.68% dilute sulfuric acid solution. After the mixing is complete, add 81.8g 2,5-dichloroaniline with a mass fraction of 98%, then heated to 92°C, and kept warm until the material was completely dissolved. The material was then transferred to a 2L zirconium autoclave. Nitrogen was passed to 0.8Mpa to replace the gas inside, and then the autoclave was sealed for heating. Raise the temperature to 160°C, keep it warm for 2 hours, then lower the temperature, wait until the temperature drops to 60°C, open the air, then stand still, layer and separate liquids to obtain 629.8.1g of water phase, 0.12% of phenol content, 86g of oil phase, 90.6% of phenol content , the oil phase was decompressed and rectified under a vacuum of 0.099Mpa, and a total of 77.3g of fractions above 70°C were collected. The conten...

Embodiment 2

[0023] Add 950g of water to a 1000ml four-neck flask, then take 100g of concentrated sulfuric acid with a mass fraction of 98%, and add it to the above flask under stirring to form a 9.33% dilute sulfuric acid solution. After the mixing is complete, add 81.8g 2,5-dichloroaniline with a mass fraction of 98%, then heated to 90°C, and kept warm until the material was completely dissolved. The material was then transferred to a 2L zirconium autoclave. Nitrogen was passed to 5.0Mpa to replace the gas inside, and then the autoclave was sealed for heating. Raise the temperature to 280°C, keep it warm for 3 hours, then lower the temperature, wait until the temperature drops to 50°C, open the air, then stand still, separate layers and separate liquids to obtain 1044.1g of water phase with 0.13% phenol content, 86.1g of oil phase with 90.3% phenol content , the oil phase was decompressed and rectified under a vacuum of 0.099Mpa, and a total of 77g of fractions above 70°C were collected...

Embodiment 3

[0025] Add 861g of water to a 1000ml four-neck flask, then take 108.9g of concentrated sulfuric acid with a mass fraction of 98%, and add it to the above flask under stirring to form a 11.00% dilute sulfuric acid solution. After mixing, add 81.8 g of 2,5-dichloroaniline with a mass fraction of 98%, then heated to 90°C, and kept warm until the material was completely dissolved. The material was then transferred to a 2L zirconium autoclave. Nitrogen was passed to 3.0Mpa to replace the gas inside, and then the autoclave was sealed for heating. Raise the temperature to 180°C, keep it warm for 5 hours, then lower the temperature, wait until the temperature drops to 70°C, open the air, then stand still, layer and separate liquids to obtain 964.7g of water phase, phenol content 0.18%, 85.6g of oil phase, phenol content of oil phase 91.3%, yield 96.4%.

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Abstract

The invention discloses a synthesis method of 2, 5-dichlorophenol, which comprises the following steps of: using 2, 5-dichloroaniline as raw materials and inorganic acid water solution as hydrolytic agent and solvent, firstly heating and premixing the 2, 5-dichloroaniline and the inorganic acid water solution at normal pressure, enabling the 2, 5-dichloroaniline to be fully dissolved in the inorganic acid water solution, then hydrolyzing the mixed solution in the existence of inert gas under conditions of high temperature and high pressure, reducing the temperature and the pressure of reaction solution after hydrolysis is completed, and statically placing the reaction solution for layering to separate out an organic phase which is the 2, 5-dichlorophenol. The synthesis method of 2, 5-dichlorophenol has the advantages that since diluted acid is used as the hydrolytic agent, the consumption of raw materials is reduced; and since the 2, 5-dichloroaniline is hydrolyzed through the high activity of the diluted acid solution at high temperature and high pressure to directly obtain the 2, 5-dichlorophenol, the conversion rate is high, the flow is short, the process is simple, the treatment method is simple after synthesis and the 2, 5-dichlorophenol can be well recovered.

Description

technical field [0001] The invention relates to a synthesis method of 2,5-dichlorophenol, in particular to a synthesis method of 2,5-dichlorophenol with short route, simple process and low cost. Background technique [0002] 2,5-Dichlorophenol is an important organic intermediate. It is the key intermediate of dicamba, a benzoic acid herbicide. It is also a nitrogen fertilizer synergist and a leather fungicide. High-purity 2,5-dichlorophenol is a white needle-like crystal with a special odor, and it will gradually turn yellow when placed in the air, and the color will gradually deepen. [0003] At present, the synthesis methods of 2,5-dichlorophenol mainly include: dichloroaniline diazonium hydrolysis method; trichlorobenzene hydrolysis method; trichlorobenzene sulfonation alkali dissolution method. These methods generally have some disadvantages: long reaction route, long reaction time, complicated process, large equipment investment, serious corrosion, and a large amoun...

Claims

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Application Information

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IPC IPC(8): C07C39/30C07C37/05
Inventor 孙国庆侯永生陈桂元李志清邹宗加张杰
Owner SHANDONG WEIFANG RAINBOW CHEM
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