A safe and efficient process for the preparation of difluoromethane in continuous flow

doi:10.1016/j.cjche.2020.02.024

Chinese Journal of Chemical Engineering ›› 2020, Vol. 28 ›› Issue (7): 1860-1865.DOI: 10.1016/j.cjche.2020.02.024

• Catalysis, Kinetics and Reaction Engineering • Previous Articles Next Articles

A safe and efficient process for the preparation of difluoromethane in continuous flow

Tao Shen¹, Xin Ge², Hengjun Zhao³, Zhixiong Xu³, Shaofeng Tong³, Shaodong Zhou¹, Chao Qian¹, Xinzhi Chen¹

1 College of Chemical and Biological Engineering, Zhejiang University, Zhejiang Provincial Key Laboratory of Advanced Chemical Engineering Manufacture Technology, Hangzhou 310027, China;
2 School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122, China;
3 Jiangsu Sanmei Chemical Co., Ltd., Nantong 226461, China

Received:2019-12-24 Revised:2020-02-20 Online:2020-08-31 Published:2020-07-28
Contact: Xin Ge, Chao Qian
Supported by:
The authors are grateful for the financial support from the National Natural Science Foundation of China (21878265, 21606104) and the National Key Research and Development Program of China(2016YFB0301800).

A safe and efficient process for the preparation of difluoromethane in continuous flow

Tao Shen¹, Xin Ge², Hengjun Zhao³, Zhixiong Xu³, Shaofeng Tong³, Shaodong Zhou¹, Chao Qian¹, Xinzhi Chen¹

1 College of Chemical and Biological Engineering, Zhejiang University, Zhejiang Provincial Key Laboratory of Advanced Chemical Engineering Manufacture Technology, Hangzhou 310027, China;
2 School of Chemical and Material Engineering, Jiangnan University, Wuxi 214122, China;
3 Jiangsu Sanmei Chemical Co., Ltd., Nantong 226461, China

通讯作者: Xin Ge, Chao Qian
基金资助:
The authors are grateful for the financial support from the National Natural Science Foundation of China (21878265, 21606104) and the National Key Research and Development Program of China(2016YFB0301800).

Abstract

Abstract: Difluoromethane is typically produced vialiquid-phase fluorination as performed in a batch reactor. However, this process suffers from some problems, e.g., severe corrosion of the reactor, high safety risk, and the regeneration of the catalyst. In this paper, a flow process as performed in the tubular reactor was designed. The optimum conditions for continuous synthesis of difluoromethane were obtained as follows: the reaction temperature was 100 ℃, the molar ratio of dichloromethane to hydrogen fluoride was 1.6:1 and the reaction time was 300 s. The operation of the cyclic process was stable for 24 h with the conversion per pass of hydrogen fluoride up to 16.2%. The unreacted raw materials were easily reused. The deactivation of the common catalyst, antimony pentachloride, was investigated by catalyst concentration curve and XPS analysis. The approach proposed in this work is proven to be safe, efficient and low amount of catalyst.

Key words: Tubular reactor, Continuous synthesis, Difluoromethane, Catalyst

摘要： Difluoromethane is typically produced vialiquid-phase fluorination as performed in a batch reactor. However, this process suffers from some problems, e.g., severe corrosion of the reactor, high safety risk, and the regeneration of the catalyst. In this paper, a flow process as performed in the tubular reactor was designed. The optimum conditions for continuous synthesis of difluoromethane were obtained as follows: the reaction temperature was 100 ℃, the molar ratio of dichloromethane to hydrogen fluoride was 1.6:1 and the reaction time was 300 s. The operation of the cyclic process was stable for 24 h with the conversion per pass of hydrogen fluoride up to 16.2%. The unreacted raw materials were easily reused. The deactivation of the common catalyst, antimony pentachloride, was investigated by catalyst concentration curve and XPS analysis. The approach proposed in this work is proven to be safe, efficient and low amount of catalyst.

关键词: Tubular reactor, Continuous synthesis, Difluoromethane, Catalyst

Tao Shen, Xin Ge, Hengjun Zhao, Zhixiong Xu, Shaofeng Tong, Shaodong Zhou, Chao Qian, Xinzhi Chen. A safe and efficient process for the preparation of difluoromethane in continuous flow[J]. Chinese Journal of Chemical Engineering, 2020, 28(7): 1860-1865.

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A safe and efficient process for the preparation of difluoromethane in continuous flow

A safe and efficient process for the preparation of difluoromethane in continuous flow

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