Method for preparing 2,5-dichlorophenol.

A technology of dichlorophenol and o-chlorophenol, applied in chemical instruments and methods, preparation of organic compounds, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of difficult separation, low yield of target products, etc. , to achieve the effect of reasonable synthesis process, low cost and reduced raw material cost

Active Publication Date: 2016-01-27
兰州诚胜化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the melting and boiling points of 2,4-dichlorophenol and 2,5-dichlorophenol are very close (the melting point of 2,4-dichlorophenol is 42~43°C and the boiling point is 210°C, the melting point of 2,5-dichlorophenol 56~58℃, boiling point 211℃), other characteristics are also very similar, so the separation is very difficult, resulting in a low yield of the target product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 200.0g o-chlorophenol and 7.6g aluminum trichloride to a 500ml four-necked bottle equipped with a tail gas treatment system, stirring, dropping funnel, condenser, tail gas outlet pipe, and thermometer, start stirring, and slowly heat to 50 , began to slowly add 95.4 g of phosphorus oxychloride dropwise, and the dropping time was 1.0 to 1.5 hours; after the dropwise addition, continue to heat and stir at 50 to 60°C for 0.5 hours; After keeping warm, slowly heat to 100-110°C, keep warm for 1 hour, then cool down to 30-50°C; add 100ml of solvent chlorinated alkanes (such as 1,2-dichloroethane, trichloromethane, etc.), add diphenyl 5g of sulfide, stirred for 20-30 minutes, and then began to slowly pass in 121.5g of chlorine gas at 50-60°C, and kept warm for 30 minutes after passing through, then added 750ml of water, then heated up to evaporate the solvent, then heated to 100-105°C, and refluxed React for 8 hours; remove the electric heating pack, add a cold water bath,...

Embodiment 2

[0035] Add 200.0g o-chlorophenol and 7.6g aluminum trichloride to a 500ml four-necked bottle equipped with a tail gas treatment system, stirring, dropping funnel, condenser, tail gas outlet pipe, and thermometer, start stirring, and slowly heat to 50 , began to slowly add 95.4 g of phosphorus oxychloride dropwise, and the dropping time was 1.0 to 1.5 hours; after the dropwise addition, continue to heat and stir at 50 to 60°C for 0.5 hours; After keeping warm, slowly heat to 100-110°C, keep warm for 1 hour, then cool down to 30-50°C; add 100ml of solvent chlorinated alkanes (such as 1,2-dichloroethane, trichloromethane, etc.), add diphenyl Add 220.5g of sulfuryl chloride slowly at 50-60°C, add 750ml of water, then evaporate the solvent by raising the temperature, then heat to 100-105°C, and reflux for 8 hours; remove the electric heating pack, add a cold water bath, Cool to 80°C, remove the waste water, and separate to obtain an oil layer; the oil layer was rectified at a vacuu...

Embodiment 3

[0037] Add 200.0g o-chlorophenol and 6.0g ferric chloride to a 500ml four-necked bottle equipped with a tail gas treatment system, stirring, dropping funnel, condenser, tail gas outlet pipe, and thermometer, start stirring, and slowly heat to 60 ℃, start slowly dropwise adding 80g of phosphorus oxychloride, and the dropping time is 1.5 hours; after the dropwise addition, continue to keep stirring at 60-70℃ for 0.5 hours; After keeping warm, slowly heat to 100-110°C, keep warm for 1 hour, then cool down to 30-50°C; add 100ml of solvent chlorinated alkanes (such as 1,2-dichloroethane, trichloromethane, etc.), add diphenyl Add 220.5g of sulfuryl chloride slowly at 50-60°C, add 750ml of water, then evaporate the solvent by raising the temperature, then heat to 100-105°C, and reflux for 8 hours; remove the electric heating pack, add a cold water bath, Cool to 80°C, remove the waste water, and separate to obtain an oil layer; the oil layer was rectified under vacuum to -0.1MPa to ob...

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Abstract

The invention discloses a method for preparing 2,5-dichlorophenol. In the method, o-chlorophenol is employed as a raw material, a composite catalyst is employed, acidic materials are utilized to protect hydroxys, and then chlorination and hydrolysis are carried out. When the new method for preparing 2,5-dichlorophenol is compared with present production methods in the market, the raw material cost is lower, operation is safer and simpler, the provided method is more friendly to the environment, three wastes (waste gas, waste water and industrial residue) are smaller, the yield is higher, the provided method is suitable for industrial production, and the product quality meets international standards.

Description

technical field [0001] The invention relates to a new process and a new method for preparing 2,5-dichlorophenol, belonging to the field of organic synthesis. Background technique [0002] 2,5-Dichlorophenol is the main raw material of benzoic acid herbicide dicamba. Dicamba has a systemic conduction effect and has significant control effects on annual and perennial broad-leaved weeds. Used for wheat, corn, millet, rice and other gramineous crops to prevent and control pig worms, buckwheat vines, quinoa, beef chickweed, succulents, sow lettuce, cocklebur, thin sycamore, field bindweed, spiny vegetables, Ask jing, carp intestines and so on. Post-emergence spraying, the agent is absorbed through the stems, leaves, and roots of the weed, and conducts up and down through the phloem and xylem, hindering the normal activity of plant hormones and causing them to die. 2,5-Dichlorophenol is also an intermediate for medicines and dyes, a nitrogen fertilizer synergist, and a leather ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/30C07C37/62B01J31/30B01J31/26
Inventor 王耀良刘必焕
Owner 兰州诚胜化工科技有限公司
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