三相相转移催化合成仲丁基二硫醚

Synthesis of Sec-butyl Disulfide by Tri-phase Transfer Catalysis

摘要:

以仲丁基溴（RBr），升华硫，九水硫化钠为原料，采用自制的SiO2-g-PS负载季铵盐的三相相转移催化剂合成二仲丁基二硫醚。通过正交实验得最佳工艺条件：n(Na2S)：n(RBr)=1:0.8，催化剂用量为0.75%，反应温度为30 ℃，反应时间为9h。在此条件下重复3次实验，平均收率57.65%。与其他三相催化剂相比较，该催化剂催化效果最好，且重复使用6次活性并未明显的降低，产物经1HNMR和FTIR确证。

Abstract:

We present here a tri-phase transfer catalysis synthesis of Sec-butyl disulfide using sec-butyl bromine, sulfur and sodium sulfide nonahydrate as the raw material, the self-made SiO2-g-PS load of quaternary ammonium salt as the tri-phase transfer catalyst. Via the orthogonal experiment, the optimum conditions were obtained as follows: n(Na2S):n(RBr)=1:0.8, the dosage of catalyst is 0.75%,reaction temperature 30℃, reaction time 9h. Repeated the experiment 3 times, the mean of yield is 57.65%. Compared with other tri-phase transfer catalyst, the catalyst this experiment used has the best catalyst effect. What's more, by repeated use 6 times, the catalytic activity did not significantly reduced. The product was confirmed by 1HNMR and FTIR.