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Continuous synthesis of tetraethyl thiuram disulfide with CO 2 as acid agent in a gas-liquid microdispersion system
Journal of Flow Chemistry ( IF 2.7 ) Pub Date : 2019-08-27 , DOI: 10.1007/s41981-019-00046-9
JiaYu Hu , Jiaxin Tian , Kai Wang , Jian Deng , Guangsheng Luo

Herein, a continuous synthetic method of tetraethyl thiuram disulfide (TETD) with CO2 as a weak acid reagent in a gas-liquid microdispersion reaction system has been described. A microdispersion reaction system comprising two microreactors for CO2 absorption and diethyldithiocarbamate acid subsequent oxidation reaction was developed. In the first step, the main products of absorption and oxidation reactions were identified. Next, the yield of TETD and selectivity of sodium diethyldithiocarbamate under different flow rates of raw materials, amount of CO2, aging effect, and pressure in the microreaction system were determined. The yield reached 89.03% based on 60% H2O2 dosage and the selectivity was 92.86% in less than 3 min of residence time, which was more than 30 min in the batch process. The space time yield in the microreaction system was ~20 times of that achieved in the batch process. The study provides a new successful reference for replacing batch synthesis by a continuous process using a microreaction system.



中文翻译:

气液微分散体系中以CO 2为酸剂连续合成二乙基秋兰姆二硫化物

在此,已经描述了在气-液微分散反应系统中以CO 2作为弱酸试剂的四乙基秋兰姆二硫化物(TETD)的连续合成方法。开发了包括两个用于吸收CO 2的微反应器和二乙基二硫代氨基甲酸随后的氧化反应的微分散反应系统。第一步,确定吸收和氧化反应的主要产物。接下来,确定了在不同原料流量,CO 2量,老化效果和微反应体系中的压力下,TETD的产率和二乙基二硫代氨基甲酸钠的选择性。基于60%H 2 O 2,产率达到89.03%在少于3分钟的停留时间内,其选择性和选择性为92.86%,在分批过程中超过30分钟。微反应系统中的时空产率约为分批工艺中的时空产率的20倍。该研究为通过使用微反应系统的连续过程代替批量合成提供了新的成功参考。

更新日期:2019-08-27
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