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Preparation process of high-purity p-chlorophenol

A technology for p-chlorophenol and preparation process, which is applied to the field of high-purity p-chlorophenol preparation technology, can solve problems such as unsatisfactory effect, influence on ordinary rectification separation effect, low relative volatility, etc., and achieves improved yield and improved extraction. Separation effect, good comprehensive quality effect

Active Publication Date: 2018-06-01
HUAIHAI INST OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both are the products of phenol chlorination. The chlorination of phenol is the mixed chlorinated phenol in the ortho and para positions. After separation, p-chlorophenol and o-chlorophenol are obtained. The boiling point of o-chlorophenol (175.0°C) and The boiling point of p-chlorophenol (217.0°C) differs greatly. At present, most manufacturers use ordinary rectification methods to separate and refine it, but the actual effect is often unsatisfactory. After analysis, although the two isomers have a large difference in boiling point, they are due to each other. Hydrogen bonds are formed between them, and the actual relative volatility is not large, which directly affects the separation effect of ordinary rectification

Method used

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Examples

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Effect test

Embodiment 1

[0020] A process for preparing high-purity p-chlorophenol, comprising a chlorination process and a rectification process, the specific process steps are as follows:

[0021] Chlorination process: use phenol as raw material, use steam to indirect heating to liquid state at 55±2°C, then send it to the enamel reaction kettle with quantitative pressure by pump, and introduce chlorine gas in the way of first fast and then slow under normal pressure , carry out chlorination reaction, the reaction time is 32h, get chlorinated phenol; After the reaction is completed, take phenol as calculation basis, the conversion rate of chlorination reaction is 99.17%, the conversion rate of o-chlorophenol is 42.7%, and the conversion rate of p-chlorophenol is 56.07%, 2,4-dichlorophenol conversion rate is 0.36%, 2,6-dichlorophenol conversion rate is 0.04%;

[0022] Rectification process: Cool the chlorinated phenol to 55°C, then add the compound extractant, stir evenly and send them together to the...

Embodiment 2

[0024] A process for preparing high-purity p-chlorophenol, comprising a chlorination process and a rectification process, the specific process steps are as follows:

[0025] Chlorination process: use phenol as raw material, use steam to indirect heating to liquid state at 55±2°C, then send it to the enamel reaction kettle with quantitative pressure by pump, and introduce chlorine gas in the way of first fast and then slow under normal pressure , carry out chlorination reaction, the reaction time is 34h, get chlorinated phenol; After the reaction is completed, take phenol as calculation basis, the conversion rate of chlorination reaction is 99.27%, the conversion rate of o-chlorophenol is 42.6%, and the conversion rate of p-chlorophenol is 56.27%, 2,4-dichlorophenol conversion rate is 0.35%, 2,6-dichlorophenol conversion rate is 0.05%;

[0026] Rectification process: Cool the chlorinated phenol to 58°C, then add the compound extractant, stir evenly and send them together to the...

Embodiment 3

[0028] A process for preparing high-purity p-chlorophenol, comprising a chlorination process and a rectification process, the specific process steps are as follows:

[0029] Chlorination process: use phenol as raw material, use steam to indirect heating to liquid state at 55±2°C, then send it to the enamel reaction kettle with quantitative pressure by pump, and introduce chlorine gas in the way of first fast and then slow under normal pressure , carry out chlorination reaction, the reaction time is 36h, get chlorinated phenol; After the reaction is completed, take phenol as the calculation basis, the conversion rate of chlorination reaction is 99.54%, the conversion rate of o-chlorophenol is 42.2%, and the conversion rate of p-chlorophenol is 56.94%, 2,4-dichlorophenol conversion rate is 0.38%, 2,6-dichlorophenol conversion rate is 0.02%;

[0030] Rectification process: Cool the chlorinated phenol to 58°C, then add the compound extractant, stir evenly and send them together to...

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Abstract

The invention provides a preparation process of high-purity p-chlorophenol, which includes the steps of: 1) chlorination: heating phenol as a raw material to liquid state, quantitatively pressure-feeding the phenol to an enamel reaction kettle via a pump, feeding chlorine under a normal pressure in a manner of firstly high speed and then low speed to perform the chlorination reaction for 32-38 h,thus producing chlorophenol; 2) rectification: cooling the chlorophenol to 55-60 DEG C and adding a composite extraction agent, uniformly stirring the mixture, and feeding the mixture into a rectification column to perform vacuum distillation, wherein firstly reflux is carried out under vapor pressure of 0.3-0.35 MPa for 3-3.5 h, and then sampling analysis is carried out under the vacuum degree of-0.096 - 0.098 MPa and at temperature of 68-73 DEG C, and receiving o-chlorophenol; 3) regulating the temperature to 115-120 DEG C and vapor pressure to 0.55 MPa, and performing sampling analysis andreceiving p-chlorophenol. In the method, reasonable technical modification is carried out so as to significantly improve conversion rate and yield of the chlorophenol. The method is good separation effect and can reach 99.4% in purities of both the p-chlorophenol and o-chlorophenol. The products have good comprehensive quality. The method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of preparation and separation of chemical products, in particular to a preparation process of high-purity p-chlorophenol. Background technique [0002] Both o-chlorophenol and p-chlorophenol are important organic chemical raw materials. o-chlorophenol can be used in medicine, pesticides, dyes and other organic synthesis raw materials. o-chlorophenol can be obtained by phosgenation of o-chlorophenyl chloroformate, which is carbamic acid The intermediate of the ester insecticide dipacarb, ortho-chlorophenol is also the intermediate of the insecticide profenofos. p-Chlorophenol is mainly used in pesticides, medicines, dyes, plastics and other industries. It is also used as ethanol discoloration agent, refined mineral oil selective solvent, microscopic analysis, etc., and in agricultural industry, it is mainly used in the synthesis of fenoxin, trefloxacin, and wool fungicides. , anti-falling element, profenfos,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/62C07C37/80C07C39/28
CPCC07C37/62C07C37/80C07C39/28
Inventor 徐国想徐韶康王国荣
Owner HUAIHAI INST OF TECH
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