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Continuous synthesis of tetraethyl thiuram disulfide with CO2 as acid agent in a gas-liquid microdispersion system

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Abstract

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.

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Abbreviations

mT :

theoretical mass of TETD (g)

ms :

sample amount (g)

wTETDNa :

the mass ratio of NaEt2DTC in its solution

FTETDNa :

the mass flow rate of NaEt2DTC solution (g/min)

FH2O2 :

the mass flow rate of H2O2 solution (g/min)

mA :

the mass of TETD solid abtained(g)

sH2O2 :

the H2O2 dosage

FCO2 :

the volume flow rate of CO2 (mL/min)

ts :

sampling time(s)

CTETDNa :

the mass ratio of NaEt2DTC detected by UV

mm :

the mass of mother liqour (g)

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Acknowledgements

We gratefully acknowledge the support from the National Natural Science Foundation of China (Nos. 91334201, U1463208 and 21506110).

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Authors and Affiliations

  1. The State Key Laboratory of Chemical Engineering, Department of Chemical Engineering, Tsinghua University, Beijing, 100084, China

    JiaYu Hu, Jiaxin Tian, Kai Wang, Jian Deng & Guangsheng Luo

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  1. JiaYu Hu
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Correspondence to Guangsheng Luo.

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Hu, J., Tian, J., Wang, K. et al. Continuous synthesis of tetraethyl thiuram disulfide with CO2 as acid agent in a gas-liquid microdispersion system. J Flow Chem 9, 211–220 (2019). https://doi.org/10.1007/s41981-019-00046-9

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  • DOI: https://doi.org/10.1007/s41981-019-00046-9

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