Two-step continuous synthesis of tetraethylthiuram disulfide in microstructured reactors

Abstract

We present two-step continuous synthesis of tetraethyl thiuram disulfide using microstructured reactors, starting with the formation of N, N-diethyldithiocarbamic acid from carbon disulfide and diethylamine in the first mi- crostructured reactor, and the oxidation of N, N-diethyldithiocarbamic acid by hydrogen peroxide in the second one. We studied the effects of reaction temperature, LHSV and total flow rate on the yield of the product. In the first microstructured reactor assembled with an HPIMM micromixer and a stainless steel capillary as the delay loop, the yield of N, N-diethyldithiocarbamic acid reached 96.3% in the 40 wt% diethylamine ethanol solution under reaction conditions of the CS2/(C2H5)2NH molar ratio of 1.1: 1, total flow rate of 4 mL/min, LHSV of 42.4 h−1, and reaction temperature of 25 °C. Consequently, the obtained N, N-diethyldithiocarbamic acid solution was reacted with H2O2 solution in another microstructured reactor assembled with SIMM-V2 and a PTFE capillary as the delay loop, the yield of the high purity tetraethylthiuram disulfide reached 89.3% under the optimized reaction conditions.