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Preparation method of m-dichloroxylene

A dichlorobenzyl, dichlorobenzyl reaction technology, applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, bulk chemical production, etc., can solve the problems of high cost, inhibition of central nervous system, low yield, etc., and achieve high reaction speed fast effect

Active Publication Date: 2016-03-09
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since formaldehyde in the raw materials used in the above process is a highly toxic substance, and carbon tetrachloride can irritate the skin, inhibit the central nervous system, and damage the liver and kidneys, the requirements for raw material procurement, transportation, and environmental protection are very high, and the production process There are problems such as long cycle, high cost and low yield

Method used

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  • Preparation method of m-dichloroxylene
  • Preparation method of m-dichloroxylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The preparation method of m-dichlorobenzyl is as follows:

[0030] (1) Reaction:

[0031] Add 100mL (86.8g) m-xylene, 50mL tetradetrafluorohexane and 0.087g 1-propyl-3-methylimidazolium chloride salt into the reaction tank, and then pass 151.09g into the reaction tank under the illumination of the LED light source Chlorine gas was reacted at 60° C. for 8 hours to obtain a m-dichlorobenzyl reaction solution with a m-dichlorobenzyl content of 80 wt %;

[0032] (2) Separation:

[0033] Add the m-dichlorobenzyl reaction solution into the cooling tank, carry out layering treatment at 35°C, the upper layer solution enters the reaction tank to continue the reaction, and the lower layer solution is the crude m-dichlorobenzyl;

[0034] (3) Refined:

[0035] Add the crude product of m-dichlorobenzyl into the rectification tower, carry out vacuum distillation at 8mmHg, collect the fraction at 145-149°C, and obtain 115.78g of m-dichlorobenzyl, the content is 99%, and the melting...

Embodiment 2

[0037] The preparation method of m-dichlorobenzyl is as follows:

[0038] (1) Reaction:

[0039] Add 100mL (86.8g) m-xylene, 200mL tetradetrafluorohexane and 0.174g 1-hexadecyl-3-methylimidazolium chloride salt into the reaction tank, and then pass 174.3 g chlorine, reacted at 59° C. for 6 h to obtain a m-dichlorobenzyl reaction solution with a m-dichlorobenzyl content of 85 wt %;

[0040] (2) Separation:

[0041] Add the m-dichlorobenzyl reaction solution into the separation tank, and carry out layering treatment at 35°C, the upper layer solution enters the reaction tank to continue the reaction, and the lower layer solution is the crude m-dichlorobenzyl;

[0042] (3) Refined:

[0043] Put the crude product of m-dichlorobenzyl into the rectification tower, carry out vacuum distillation at 8mmHg, collect the distillate at 145-149°C, and obtain 122.9g of m-dichlorobenzyl, the content is 99.1%, and the melting point is 33.4-34.6°C .

Embodiment 3

[0045] The preparation method of m-dichlorobenzyl is as follows:

[0046] (1) Reaction:

[0047] Add 100mL (86.8g) of m-xylene, 300mL of tetradetrafluorohexane and 0.435g of 1-butyl-3-methylimidazolium chloride salt into the reaction tank, and then pass 232.44 g chlorine, reacted at 58° C. for 3 h to obtain a m-dichlorobenzyl reaction solution with a m-dichlorobenzyl content of 90 wt %;

[0048] (2) Separation:

[0049] Add the m-dichlorobenzyl reaction liquid into the separation tank, carry out layering treatment at 35°C, the upper layer solution enters the reaction tank to continue the reaction, and the lower layer solution is the crude m-dichlorobenzyl;

[0050] (3) Refined:

[0051] Add the crude product of m-dichlorobenzyl into the rectification tower, carry out vacuum distillation at 8mmHg, collect the fraction at 145-149°C, and obtain 130.02g of m-dichlorobenzyl, the content is 99.18%, and the melting point is 33.5-34.7°C .

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Abstract

The invention relates to a preparation method of m-dichloroxylene, and belongs to the technical field of organic chemical synthesis. The preparation method comprises the following steps: adding m-xylene, a solvent and an ionic liquid catalyst to a reaction tank, introducing chlorine under the irradiation of an LED light source, carrying out a refluxing reaction to obtain an m-dichloroxylene reaction solution, carrying out cooling separation on the m-dichloroxylene reaction solution, and rectifying to obtain m-dichloroxylene. The melting point of the prepared m-dichloroxylene is 33-35DEG C, and the purity of the m-dichloroxylene is 99% or above; and the preparation method has the characteristics of fast reaction speed, and cycle use of the solvent, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of m-dichlorobenzyl, which belongs to the technical field of organic chemical synthesis. Background technique [0002] m-dichlorobenzyl is an important chemical raw material, its appearance is colorless transparent liquid or white crystal, it can be used as an intermediate in organic synthesis to produce p-phenylenedimethanol and other dyes. [0003] At present, the production techniques of m-dichlorobenzyl mainly include formaldehyde method and solvent method. The formaldehyde method is to react monochlorotoluene with formaldehyde, and the yield is about 63%; the solvent method is to use carbon tetrachloride as a solvent to react m-xylene with chlorine gas to obtain m-dichlorobenzyl. Since formaldehyde in the raw materials used in the above process is a highly toxic substance, and carbon tetrachloride can irritate the skin, inhibit the central nervous system, and damage the liver and kidneys, the requirem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C22/04C07C17/14C07C17/38
CPCC07C17/14C07C17/38C07C22/04Y02P20/54
Inventor 薛居强张善民张泰铭王荣海孙丰春张清新
Owner SHANDONG KAISHENG NEW MATERIALS
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