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Method and device for purifying 2,4-dichlorophenol

A technology of dichlorophenol and purification method, which is applied in the field of preparation of pesticide chemical intermediates, and can solve problems such as environmental pollution, waste gas pollution, and large investment

Inactive Publication Date: 2012-09-12
荆州沙隆达控股有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solvent extraction is a method in which the mixture of 2,4-dichlorophenol and 2,6-dichlorophenol is blended into an organic solvent, and other substances are added for extraction and separation; this method is prone to produce a large amount of organic waste and cause environmental pollution and other shortcomings
Vacuum distillation method refers to using the difference in boiling point of 2,4-dichlorophenol and 2,6-dichlorophenol to achieve separation by rectification under high temperature conditions; this method has large investment, large energy consumption and waste gas pollution Serious and other shortcomings

Method used

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  • Method and device for purifying 2,4-dichlorophenol
  • Method and device for purifying 2,4-dichlorophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Import the crude product of 2,4-dichlorophenol from the material pump 1 into the crystallizer 3, lower the temperature to crystallize, pay attention to observe the material condition in the crystallizer, when crystals are precipitated, continue to cool down slowly to make the crystal layer grow. The cooling rate is 0.015°C / min. After cooling down to 10°C, discharge the uncrystallized mother liquor into the mother liquor tank 4, raise the temperature at a rate of 0.06°C / min to make the crystal layer sweat, the end point temperature of sweating is 30°C, discharge the sweat into the sweat tank 7, raise the temperature to make the crystal layer Melting, collecting the molten liquid in the finished product tank 5 of 2,4-dichlorophenol and taking samples for analysis. Collect 2,6-dichlorophenol crystals into 2,6-dichlorophenol finished product tank 6. The purity of the obtained 2,4-dichlorophenol is 99.23%, and the product yield is 99.13% after calculation. The mother liquo...

Embodiment 2

[0021] Import the crude product of 2,4-dichlorophenol into the crystallizer, lower the temperature to crystallize, pay attention to observe the material condition in the crystallizer, when crystals are precipitated, continue to cool down slowly to make the crystal layer grow. The cooling rate is 0.020 / min. After cooling down to 15°C, discharge the uncrystallized mother liquor, raise the temperature at a rate of 0.07°C / min to make the crystal layer sweat, the end point temperature of sweating is 40°C, discharge the sweat, raise the temperature to melt the crystal layer, collect the molten liquid and take samples for analysis. The purity of the obtained 2,4-dichlorophenol is 99.07%, and the product yield is 99.22% after calculation. After collecting the uncrystallized sweat, pump it into the rectification tower kettle, evacuate it, and control the vacuum at 30mmHg, heat the mixed solution to 170°C, and carry out vacuum distillation. Phenol, monochlorophenol, 2,4-dichlorophenol ...

Embodiment 3

[0023] Import the crude product of 2,4-dichlorophenol into the crystallizer, lower the temperature to crystallize, pay attention to observe the material condition in the crystallizer, when crystals are precipitated, continue to cool down slowly to make the crystal layer grow. The cooling rate is 0.035°C / min. After cooling down to 20°C, discharge the uncrystallized mother liquor, raise the temperature at a rate of 0.08°C / min to make the crystal layer sweat, the end point temperature of sweating is 50°C, discharge the sweat, raise the temperature to melt the crystal layer, collect the molten liquid and take samples for analysis. The purity of 2,4-dichlorophenol obtained is 98.84%, and the product yield is 94.63% after calculation. After collecting the uncrystallized sweat, pump it into the rectification tower kettle, evacuate it, control the vacuum at 40mmHg, heat the mixed solution to 180°C, and carry out vacuum distillation. Phenol, monochlorophenol, 2,4-dichlorophenol crude ...

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Abstract

The invention provides a method for purifying 2,4-dichlorophenol. The method comprises the following steps of cooling crude 2,4-dichlorophenol to 10 to 20 DEG C, stopping crystallization to obtain crystals, discharging mother liquor, heating the crystals and sweating at the temperature of between 30 and 50 DEG C, and discharging sweat to obtain the purified 2,4-dichlorophenol. According to the method, rectification is simple and easy to operate, the defects of high energy consumption and high production cost, damage to the health of operators and environment pollution due to the use of organic solvents and the like are overcome by fractional crystallization, and the requirements of industrialized production are met. The purity of the purified 2,4-dichlorophenol is over 98 percent, and requirements for preparing other products by using the purified 2,4-dichlorophenol are met.

Description

technical field [0001] The invention belongs to the field of preparation methods of pesticide chemical intermediates, in particular to a method and device for purifying 2,4-dichlorophenol. Background technique [0002] 2,4-Dichlorophenol is a very important organic intermediate, which is mainly used in the pesticide industry to produce the insecticide phenanophos and the herbicide oxadiazon, webenben, and 2,4-dichlorophenoxy series Acids and their esters; used in the pharmaceutical industry to produce dichlorophen, an anthelmintic; used in the auxiliary industry to produce anti-fogging agent TCS. Due to the increase in the development of downstream products of 2,4-dichlorophenol in China in recent years, especially the successful development of the anti-fogging agent TCS and the pesticide oxadiazone in my country, it has given my country's 2,4-dichlorophenol production industry Development brings great opportunities. [0003] At present, the production methods of 2,4-dichlo...

Claims

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Application Information

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IPC IPC(8): C07C39/30C07C37/84B01D9/02
Inventor 刘国平刘跃李作荣李波殷宏刘建华薛光才鄢圣光熊金华张世钢李传林廖艳范文涛
Owner 荆州沙隆达控股有限公司
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