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1, 4-bis(chloromethyl)benzene synthesis technology

A synthesis process, the technology of p-dichlorobenzyl, applied in the direction of organic chemistry, preparation of halogenated hydrocarbons, chemical instruments and methods, etc., can solve the problems of low product conversion rate and high cost, and achieve high yield, low cost and good dissolution effect of ability

Active Publication Date: 2016-03-09
SHANDONG KAISHENG NEW MATERIALS
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  • Abstract
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  • Claims
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Problems solved by technology

CN104230653A discloses chlorination with p-xylene at 80°C, when the p-dichlorobenzyl content in the sample reaches 35wt%, stop passing chlorine, then obtain p-dichlorobenzyl by performing flash distillation and rectification, the process is in When the conversion rate of benzyl dichloride reaches 35%, flash distillation and vacuum distillation are carried out, and there are problems such as low product conversion rate and high cost

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  • 1, 4-bis(chloromethyl)benzene synthesis technology
  • 1, 4-bis(chloromethyl)benzene synthesis technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The synthetic technique of p-dichlorobenzyl is as follows:

[0029] (1) Reaction:

[0030] Add 100g of p-xylene and 0.1g of 1-dodecyl-3-methylimidazolium chloride salt into the reaction tank, pass 173.9g of chlorine gas under the irradiation of LED light source, react at 110°C for 10h, and obtain the content of p-dichlorobenzyl: 70wt% p-dichlorobenzyl reaction solution;

[0031] (2) Separation:

[0032] Add the p-dichlorobenzyl reaction solution into the separation tank, carry out layering treatment at 90°C, return the upper layer solution to the reaction tank to continue the reaction, and the lower layer solution is the crude p-dichlorobenzyl;

[0033] (3) Refined:

[0034] Put the crude p-dichlorobenzyl into the rectification tower, conduct vacuum distillation at 8mmHg, collect 150-155°C fractions, and obtain 116.60g p-dichlorobenzyl with a content of 99% and a melting point of 98.5-100.9°C.

Embodiment 2

[0036] The synthetic technique of p-dichlorobenzyl is as follows:

[0037] (1) Reaction:

[0038] Add 100g of p-xylene and 0.2g of 1-dodecyl-3-methylimidazolium chloride salt into the reaction tank, pass 200.6g of chlorine gas under the irradiation of LED light source, and react at 115°C for 6h, and the content of p-dichlorobenzyl is 75wt% p-dichlorobenzyl reaction solution;

[0039] (2) Separation:

[0040] Add the p-dichlorobenzyl reaction solution into the separation tank, carry out layering treatment at 85°C, return the upper layer solution to the reaction tank to continue the reaction, and the lower layer solution is the crude p-dichlorobenzyl;

[0041] (3) Refined:

[0042] Put the crude p-dichlorobenzyl into the rectification tower, carry out vacuum distillation at 8mmHg, collect 150-155°C fractions, and obtain 124.86g p-dichlorobenzyl with a content of 99.05% and a melting point of 99.1-100.6°C.

Embodiment 3

[0044] The synthetic technique of p-dichlorobenzyl is as follows:

[0045] (1) Reaction:

[0046] Add 100g of p-xylene and 0.5g of 1-butyl-2,3-methylimidazolium chloride salt into the reaction tank, pass 267.5g of chlorine gas under the irradiation of LED light source, and react at 120°C for 3 hours to obtain the content of p-dichlorobenzyl Be 80wt% p-dichlorobenzyl reaction solution;

[0047] (2) Separation:

[0048] Add the p-dichlorobenzyl reaction liquid from the overflow port of the reaction tank to the separation tank, and carry out layering treatment at 80°C, return the upper layer solution to the reaction tank to continue the reaction, and the lower layer solution is the crude p-dichlorobenzyl;

[0049] (3) Refined:

[0050] Put the crude p-dichlorobenzyl into the rectification tower, carry out vacuum distillation under the pressure of 8mmHg, collect the 150-155°C fraction, and obtain 133.12g p-dichlorobenzyl, the content is 99.1%, and the melting point is 99.5-100....

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Abstract

The invention relates to a 1, 4-bis(chloromethyl)benzene synthesis technology and belongs to the technical field of organic chemical synthesis. The technology comprises that under LED light source irradiation, p-xylene and chlorine undergo a reaction in the presence of an ionic liquid catalyst to produce a 1, 4-bis(chloromethyl)benzene reaction solution, the 1, 4-bis(chloromethyl)benzene reaction solution is cooled and separated so that a 1, 4-bis(chloromethyl)benzene crude product is obtained, and the 1, 4-bis(chloromethyl)benzene crude product is subjected to vacuum rectification so that 1, 4-bis(chloromethyl)benzene is obtained. The 1, 4-bis(chloromethyl)benzene has a melting point of 98-101 DEG C and purity of 99% or more. The 1, 4-bis(chloromethyl)benzene synthesis technology is free of any solvent, guarantees high product purity, has the characteristics of high conversion rate, fast reaction rate and low cost and is suitable for industrial production.

Description

technical field [0001] The invention relates to a synthesis process of p-dichlorobenzyl, which belongs to the technical field of organic chemical synthesis. Background technique [0002] p-Dichlorobenzyl is an important chemical raw material, its appearance is white flaky crystal, as an intermediate of organic synthesis, it is mainly used in the manufacture of p-xylylenedimethanol, p-xylylene dimethyl ether, terephthalaldehyde and other dyes. Can be used as pharmaceutical intermediates. CN104230653A discloses chlorination with p-xylene at 80°C, when the p-dichlorobenzyl content in the sample reaches 35wt%, stop passing chlorine, then obtain p-dichlorobenzyl by performing flash distillation and rectification, the process is in When the conversion rate of benzyl dichloride reaches 35%, flash distillation and vacuum distillation are carried out, which has problems such as low product conversion rate and high cost. Contents of the invention [0003] The purpose of the presen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/14C07C22/04
CPCC07C17/14C07C22/04
Inventor 薛居强孙丰春张善民毕义霞张泰铭谢圣斌
Owner SHANDONG KAISHENG NEW MATERIALS
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