三相相转移催化合成二仲丁基二硫醚

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

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负载季铵盐为三相相转移催化剂合成二仲丁基二硫醚。通过正交实验得到最佳工艺条件为:n(Na2S)∶n(RBr)=1∶0.8,催化剂质量分数为0.75%,反应温度为30℃,反应时间为9 h。在该条件下重复3次实验,平均收率为57.65%。与其他三相催化剂相比,该催化剂催化效果最好,且重复使用6次活性并未明显降低,产物结构经1HNMR和FTIR确证。

This thesis presents a tri-phase transfer catalysis synthesis of sec-butyl disulfide using sec- butyl bromine, sulfur and sodium sulfide nonahydrate as raw materials, 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 ascertained as follows ： n （ Na2 S） ：n （RBr） = 1：0. 8, the dosage of catalyst 0. 75 %, reaction temperature 30℃, reaction time 9 h. The experiment was repeated for 3 times under such conditions, and the mean of yield was 57.65%. Compared with other tri-phase transfer catalysts,the catalyst used in this experiment has the best catalytic effect. What＇s more, after 6 times＇ reuse, the catalytic activity did not show any significant decline. The product was confirmed by ^1HNMR and FTIR.