Continuous preparation technology of m-methyl benzoyl chloride

A technology of m-toluoyl chloride and m-toluoyl chloride, applied in the field of continuous production process of m-toluoyl chloride, can solve the problems of low equipment automation, high labor intensity, unstable product quality, etc., and achieve Good low-temperature evaporation effect, high evaporation intensity, and large operating flexibility

Inactive Publication Date: 2016-02-24
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of them adopt batch production process to prepare p-toluyl chloride. The batch process has the characteristics of simple equipment and wide versatility. When the demand is low, it is more economical to adopt this method, but with the expansion of production scale, When using a batch process to produce m-toluoyl chloride, there are problems such as unstable product quality in different batches, low equipment automation and high labor intensity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The continuous production process of m-toluoyl chloride is as follows:

[0018] (1) Add 500kg of m-toluic acid, 463kg of thionyl chloride and 1000kg of xylene into the reaction kettle, then add 0.25kg of benzyltriethylammonium chloride, and react at 50°C for 2h until no gas emerges. out, and then continue to insulate for 0.5h to obtain the reaction solution;

[0019] (2) Add the reaction liquid to the rectification tower, the flow rate into the tower is 4.7kg / min, the tower still of the rectification tower is heated by steam, the temperature is controlled at 95°C, and the output flow rate of light components at the top of the tower is 4.2kg / min, the light component is returned to the reactor after being condensed by the condenser;

[0020] (3) The m-toluoyl chloride crude product in the rectifying tower still is joined in the film evaporator, and feed flow rate is 3.9kg / min, and regulating vacuum degree is 510mmHg, carries out underpressure distillation at 120 ℃, obta...

Embodiment 2

[0022] The continuous production process of m-toluoyl chloride is as follows:

[0023] (1) Add 957kg of m-toluic acid, 919.6kg of thionyl chloride and 1914kg of dichloromethane into the reaction kettle, then add 0.957kg of dodecyltrimethylammonium chloride, and react at 40°C for 4.5h , until no gas emerges, and then continue to keep warm for 0.5 hours to obtain a reaction solution;

[0024] (2) Add the reaction solution to the rectification tower, the flow rate into the tower is 4.7kg / min, the tower still of the rectification tower is heated by steam, the temperature is controlled at 99°C, and the output flow rate of the light components at the top of the tower is 4.2kg / min, the light component is returned to the reactor after being condensed by the condenser;

[0025] (3) The crude product of m-toluoyl chloride in the rectifying tower still is added in the thin-film evaporator, and the feed flow rate is 3.9kg / min, and the vacuum degree of regulation is 570mmHg, carries out ...

Embodiment 3

[0027] The continuous production process of m-toluoyl chloride is as follows:

[0028] (1) 1360kg m-toluic acid, 1453kg thionyl chloride and 2720kg dimethylbenzene are joined in the reactor, then add 2.04kg tetrabutyl ammonium bisulfate, react 4h at 45 ℃, until no gas emerges, Continue to insulate for another 0.5 hour to obtain the reaction solution;

[0029] (2) Add the reaction solution to the rectification tower, the flow rate into the tower is 4.7kg / min, the tower still of the rectification tower is heated by steam, the temperature is controlled at 105°C, and the output flow rate of the light components at the top of the tower is 4.2kg / min, the light component is returned to the reactor after being condensed by the condenser;

[0030] (3) The m-toluoyl chloride crude product in the rectifying tower still is joined in the thin-film evaporator, and feed flow rate is 3.9kg / min, and regulating vacuum degree is 630mmHg, carries out underpressure distillation at 127 ℃, obtains...

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PUM

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Abstract

The invention relates to a continuous preparation technology of m-methyl benzoyl chloride, and belongs to the technical field of fine chemical engineering. The continuous preparation technology comprises the steps of adding m-methyl benzoic acid, thionyl chloride and an organic solvent in a reaction kettle for reaction under a condition that a phase transfer catalyst exists, and obtaining reaction liquid; then adding the reaction liquid in a rectifying tower for carrying out normal-pressure rectifying so as to recycle the thionyl chloride and the organic solvent in the reaction liquid, and obtaining a m-methyl benzoyl chloride crude product; adding the m-methyl benzoyl chloride crude product in a film evaporator to carry out pressure-reduction distillation, and obtaining the m-methyl benzoyl chloride. According to the continuous preparation technology disclosed by the invention, the problems existing in a batch method/technology that the product quality is unstable, the automation degree of a device is low, and the labor intensity is large are solved; the continuous preparation technology has the characteristics that the technological route is concise, the production period is short, and the product yield is high; a side reaction can be prevented from being generated while the production capacity is increased.

Description

technical field [0001] The invention relates to a continuous production process of m-toluoyl chloride, which belongs to the technical field of fine chemicals. Background technique [0002] With the rapid development of polymer materials, m-toluoyl chloride has gradually become an important chemical intermediate, and has attracted more and more attention from researchers. Its excellent performance is widely used in the production of medicine, pesticides, dyes and photosensitive materials, etc. has been widely applied. At present, most of them adopt batch production process to prepare p-toluyl chloride. The batch process has the characteristics of simple equipment and wide versatility. When the demand is low, it is more economical to adopt this method, but with the expansion of production scale, When using a batch process to produce m-toluoyl chloride, there are problems such as unstable product quality in different batches, low equipment automation and high labor intensity. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/04C07C51/60C07C51/44
CPCC07C51/60C07C51/44C07C63/04
Inventor 张聪聪张泰铭张善民孙丰春毕义霞谢圣斌
Owner SHANDONG KAISHENG NEW MATERIALS
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