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Preparation method of benzoyl chloride

A technology of benzoyl chloride and benzoic acid, which is applied in the field of preparation of benzoyl chloride, can solve the problems of high catalyst or corrosive toxicity, unstable nature and low catalytic efficiency, etc., so as to speed up the chlorination reaction rate and improve the utilization of light sources. efficiency and low production cost

Active Publication Date: 2015-03-25
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
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AI Technical Summary

Problems solved by technology

The existing problems are that the power consumption of the light source is large, the utilization rate of light energy is low, the life of the light source is short, the catalytic efficiency of the catalyst for the main reaction is not high, and the catalyst is highly corrosive or toxic or unstable in nature, and there are risks such as explosion.

Method used

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  • Preparation method of benzoyl chloride
  • Preparation method of benzoyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 100g of toluene and 0.1g of inhibitor (the mass ratio of benzoquinone, DNBP, and DDBSA to 1:2:4) into the reaction bottle, first raise the temperature to 85°C, and start to pass the reaction bottle under the irradiation of LED light (wavelength: 380nm-450nm). Chlorine, the temperature rises slowly with the reaction, and the final temperature is controlled at 130°C. The total reaction time is 6 hours. The chlorine gas flow rate is 50g / h for 0-3 hours. As the degree of chlorination continues to increase, the chlorine gas flow rate is 30g / h for 4-6 hours. 210 g of crude benzyl trichloride was obtained with a chromatographic content of 97.2% and a yield of 96.2%.

[0036] Weigh 50g of benzoic acid and 0.25g of zinc chloride, heat up and melt the benzoic acid, add 81.2g of the crude benzyl trichloride obtained in the above reaction dropwise at 130±5°C, and keep the temperature for 0.5h after dropping over 0.5h. No tail gas is generated. , at 20mmHg underpressure distilla...

Embodiment 2

[0040] Add 200g of toluene and 1g of inhibitor (the mass ratio of benzoquinone, DNBP, and DDBSA is 1:2.1:4.2) to the reaction bottle, and pass chlorine gas at 100±10°C under the irradiation of LED light (wavelength: 380nm-450nm). Slowly heat up with the reaction, total reaction 8h, 0~3h chlorine gas flow rate is 85g / h, 4h chlorine gas flow rate is controlled at 70g / h, 5~6h chlorine gas flow rate is 55g / h, 7~8h chlorine gas flow rate is 45g / h. At the end of the reaction, 424 g of the crude product of benzyl trichloride was obtained, the chromatographic content was 97.1%, and the yield was 97.5%.

[0041] Weigh 100g of benzoic acid, 0.1g of ferric trichloride, heat up and melt the benzoic acid, add 168g of the crude benzyl trichloride obtained in the above reaction dropwise at a temperature of 130±5°C, and keep the temperature for 0.5h after dropping for 1 hour. Distilled under reduced pressure at 15 mmHg to obtain 222 g of fine benzoyl chloride with a chromatographic content of...

Embodiment 3

[0043] Add 150g of toluene and 0.3g of inhibitors (the mass ratio of benzoquinone, DNBP, and DDBSA is 0.8:2.2:4) to the reaction flask, and slowly heat up at 110±10°C under the irradiation of LED light (wavelength: 380nm-450nm). A total of 7 hours of reaction, 0 ~ 3h chlorine gas flow rate of 70g / h, 4 ~ 5h chlorine gas flow rate of 45g / h, 6 ~ 7h chlorine gas flow rate of 35g / h. At the end of the reaction, 317 g of crude product benzyl trichloride was obtained, the chromatographic content was 97.5%, and the yield was 97.4%.

[0044] Weigh 80g of benzoic acid and 0.3g of aluminum trichloride, heat up and melt the benzoic acid, add dropwise 126g of the crude benzyl trichloride obtained in the above reaction at a temperature of 130±5°C, and keep the temperature for 0.5h after dropping over 0.5h. No tail gas is generated. , Distilled under reduced pressure at 30mmHg to obtain 179g of benzoyl chloride refined product, with a chromatographic content of 99.7% and a yield of 97.2%.

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Abstract

The invention relates to a preparation method of benzoyl chloride and belongs to the technical field of the preparation of the benzoyl chloride. The preparation method of the benzoyl chloride comprises the following steps: (1) under the irradiation of an LED light source, firstly, adding a side reaction inhibitor, and then introducing chlorine into methylbenzene, and performing a heating and stirring reaction to obtain the crude product of benzyl trichloride; (2) heating benzoic acid for melting, and in the presence of a catalyst, adding the crude product of the benzyl trichloride obtained in the step (1) for reacting to obtain the crude product of benzoyl chloride; (3) purifying the obtained crude product of the benzoyl chloride by virtue of reduced pressure distillation, thereby obtaining the refined benzoyl chloride. The preparation method of the benzoyl chloride is simple to operate, short in reaction period, low in energy consumption, high in product purity and yield, low in production cost and suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of benzoyl chloride, which belongs to the technical field of preparation of benzoyl chloride. Background technique [0002] Benzoyl chloride is an important intermediate for the preparation of dyes, fragrances, organic peroxides, medicines and resins, and is also used in photography and the production of artificial tannins. In the process of synthesizing benzoyl chloride with toluene as raw material, the reaction time is mainly concentrated in the synthesis of benzyl trichloride, while the rate of toluene side chain chlorination reaction in the prior art is low, and benzyl trichloride is caused by side reactions. The productive rate is low, and then lead to take toluene as the reaction rate of the whole technique of raw material synthetic benzoyl chloride also lower, yield is low, energy consumption is high, caused environmental pollution to a certain extent. [0003] Benzyl trichloride, also known as tric...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/10C07C51/60C07C22/06C07C17/14
CPCC07C17/14C07C51/60C07C51/64C07C22/06C07C63/10
Inventor 宋国城张泰铭宋立伟杨德耀薛居强毕义霞张聪聪谢圣斌张善民
Owner SHANDONG KAISHENG NEW MATERIALS
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