活性炭负载对甲苯磺酸催化合成硫代二甘醇二软脂酸酯  

Synthesis of Dithiodinglycol Dipalmitate by p-Toluenesulphonic Acid Supported on Activated Carbon

作　　者：黄敏[1] 余梅[1] 蒋达洪[1] 黄艳仙[1] 周如金[1] 杜辉[1] 

机构地区：[1]广东石油化工学院化学与生命科学学院,广东茂名525000

出　　处：《湘潭大学自然科学学报》2013年第1期88-91,共4页Natural Science Journal of Xiangtan University

基　　金：广东省茂名市科技计划项目(201145)

摘　　要：采用浸渍法制备了活性炭负载对甲苯磺酸(TsOH/C)催化剂,以硫代二甘醇和软脂酸为原料合成硫代二甘醇二软脂酸酯.研究了催化剂的浸泡时间、干燥温度、对甲苯磺酸的质量分数对催化反应活性的影响,探讨了反应温度、醇酸比和催化剂用量对产物产率的影响.实验结果表明:TsOH/C催化剂是合成硫代二甘醇二软脂酸酯的良好催化剂.活性碳浸泡于质量浓度为25%的对甲苯磺酸溶液35h、TsOH/C催化剂的干燥温度为110℃、TsOH/C的质量分数为20%、催化剂用量0.8g、n(硫代二甘醇)∶n(软脂酸)=1.5∶1、带水剂二甲苯30mL、反应温度170～180℃,在此工艺条件下硫代二甘醇二软脂酸的产率为98.6%.采用元素分析、IR、1 H NMR、13C NMR、MS鉴定了产物结构.TsOH/C催化剂制备方法简单,催化活性高,重复使用性好.p-toluenesulphonic acid （TsOH} supported on active carbon {TsOH /C} solid acid catalyst was prepared by incipient impregnation process. Dithiodinglycol dipalmiticctate was synthesized from thiodiglyco and palmitic acid through esterification, with TsOH /C as catalyst. The effects of immersion time of catalyst, drying temperature, TsOfI loading, reaction temperature, n （ thiodiglyeo } ： n （ palmitic acid}and catalyst dosage on the synthesis were discussed. Optimal conditions arc： immersion of activated carbon in the p-toluenesulfonic acid solution with concentration of 25~ for 35 h, drying TsOH/C catalyst at temperature of 110 ＊C, TsOH loading {mass fraction }20~, catalyst dosage 0.8 g for esterification, n （thiodiglyco） z n{palmitic acid}= 1.5 ： 1, reaction temperature 170~180 ＂C, and 30 mL Xylene {dimeth- ylbenzene} as azetropic ＂~ater remover{ dehydrant }. Under these conditions the yield of dithiodinglycol di- palmitate was up to 98.6 %. Structure of the product was characterized by IR, 1 H NMR, is C NMR, MS and elementary analysis. Under the optimum conditions,TsOH solid acid catalyst supported on active carbon features simple preparation procedure, high catalytic activity, good repeatability.

关 键 词：浸渍法 活性炭 对甲苯磺酸 硫代二甘醇二软脂酸酯 

分 类 号：TQ314.249[化学工程—高聚物工业]