Method for purifying 1,2,4-trichlorobenzene from trichlorobenzene mixture

A technology of trichlorobenzene and mixture, applied in the field of fine chemical industry, can solve the problems of low efficiency and product purity, low energy consumption, high cost, etc., and achieve the effect of simple method, high efficiency and low cost

Active Publication Date: 2016-08-17
SICHUAN FOURSTAR BIOTECH RANDD CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims to solve the problems of high cost, Low efficiency and product purity, unsuitable for industrial production and other issues, a new method for the separation and purification of 1,2,

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0016] A method for purifying 1,2,4-trichlorobenzene from a mixture of trichlorobenzene, mixing trichlorobenzene in a melting crystallization device, lowering the temperature from normal temperature to 0°C, releasing uncrystallized mother liquor, and then crystallizing The final solid starts to heat up and sweat from 0°C, the sweating temperature is 0-11°C, and the average heating rate is 0.025 / min, until the total mass of the sweated sweat reaches 1 / 2 of the mass of the crystallized solid in the melting and crystallization device, then stops sweating, and finally discharges Sweat, the crystalline solid in the melting and crystallization device is heated and melted to obtain 1,2,4-trichlorobenzene.

[0017] The purity of 1,2,4-trichlorobenzene obtained in this example was 99.1%.

Embodiment 2

[0019] A method for purifying 1,2,4-trichlorobenzene from a mixture of trichlorobenzene, characterized in that trichlorobenzene is mixed in a melting crystallization device, the temperature is lowered from normal temperature to 0°C, and uncrystallized mother liquor is released , and then the crystallized solid starts to heat up and sweat from 0°C, the sweating temperature is 0-11°C, and the average heating rate is 0.035 / min, until the total mass of sweat reaches 1 / 5 of the mass of the crystallized solid in the melting crystallization device, stop Sweat, and finally discharge sweat, heat up and melt the crystalline solid in the melting and crystallization device to obtain 1,2,4-trichlorobenzene.

[0020] The purity of 1,2,4-trichlorobenzene obtained in this example is 98.3%.

Embodiment 3

[0022] A method for purifying 1,2,4-trichlorobenzene from a mixture of trichlorobenzene, characterized in that trichlorobenzene is mixed in a melting crystallization device, the temperature is lowered from normal temperature to 0°C, and uncrystallized mother liquor is released , and then the crystallized solid starts to heat up and sweat from 0°C, the sweating temperature is 0-11°C, and the average heating rate is 0.030°C / min. 1,2,4-Trichlorobenzene is obtained.

[0023] In this embodiment, the end point of sweating is when the total mass of sweat reaches 1 / 7 of the mass of crystallized solids in the melting crystallization device.

[0024] The purity of 1,2,4-trichlorobenzene obtained in this example is 97.5%.

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Abstract

The invention discloses a method for purifying 1,2,4-trichlorobenzene from a trichlorobenzene mixture, and belongs to the technical field of fine chemical engineering. The method comprises the steps that firstly, trichlorobenzene is mixed in a melt crystallization device, the temperature is lowered to 0 DEG C from room temperature, and uncrystallized mother liquid is drained; secondly, crystallized solids are sweated by increasing the temperature from 0 DEG C, wherein the sweating temperature is 0 DEG C-11 DEG C, the average temperature increasing speed is 0.025 DEG C/min-0.035 DEG C/min, and sweating does not stop until the total mass of sweat generated through sweating accounts for 1/9-1/2 of the mass of the crystallized solids in the melt crystallization device; lastly, the sweat is drained, the crystallized solids in the melt crystallization device are melted by increasing the temperature, and then 1,2,4-trichlorobenzene is obtained. According to the method, 1,2,4-trichlorobenzene is separated out in the mode of melt crystallization and gradual temperature-increasing sweating, and the advantages of being simple in method, low in cost, high in efficiency and suitable for industrialized production are achieved.

Description

technical field [0001] The invention relates to a separation and purification method, in particular to a method for purifying 1,2,4-trichlorobenzene from a mixture of trichlorobenzenes, and belongs to the technical field of fine chemicals. Background technique [0002] There are three isomers of trichlorobenzene, of which 1,2,4-trichlorobenzene is the most widely used, traditionally used as a non-flammable solvent, as a dye carrier in the textile industry, as an additive for insulating and cooling fluids in the power industry, For example, it is widely used in foreign countries as an additive for immersion liquid of power capacitors and cold-resistant transformer oil, as an additive for dielectric materials and insulating materials, etc. In addition, a variety of important pesticides, medicines and dyes can be synthesized, such as pesticides dicamba, dicamba, sodium pentachlorophenate, etc. [0003] Because the trichlorobenzene that obtains after conventional method chlorin...

Claims

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Application Information

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IPC IPC(8): C07C25/10C07C17/392C07C17/38
CPCC07C17/38C07C17/392C07C25/10
Inventor 李舟齐鸿梁剑宋剑峰罗茜彭舟张弦张华王蕾
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP
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