二甘醇二苯磺酸酯与二甘醇二苯醚的合成与表征

从二甘醇开始,经二甘醇二苯磺酸酯合成了二甘醇二苯醚.在中间体二甘醇二苯磺酸酯的合成中,用苯磺酰氯代替传统的对甲基苯磺酰氯作磺酰化试剂,用氯仿作稀释剂以控制催化剂吡啶的恰当使用量,确定了反应的最佳物料配比、反应温度和反应时间,二甘醇二苯磺酸酯的收率达84.5%,与二甘醇二对甲基苯磺酸酯的合成相比,产率提高了 10%以上,成本降低了8%-10%.在二甘醇二苯醚的合成中,增设分水装置以提高酚钠和醚的生成率,用正戊醇代替传统的正丁醇作溶剂,二甘醇二苯醚的收率达到87.6%,比通过Williamson反应的合成产率略高,反应时间缩短6 h.用显微照相、薄层色谱、红外光谱、紫外光谱、元素分析等技术对两种产物的性质、状态进行了系统研究.

Synthesis and characterization of diglycol diphenyl sulfonate and diglycol diphenyl ether

Diglycol diphenyl ether is synthesized from diethylene glycol through diglycol diphenyl sulfonate.In the process of the diglycol diphenyl sulfonate's composite,benzene sulfonyl acyl-chloride takes the place of p-methyl sulfonyl acyl-chloride which is used as conventional sulphonation agent,chloroform is used as diluent in order to control the quantity of catalyst,the optimum reaction condition such as the proportion of the reactant,the mass of catalyst,reaction temperature and time are established.The yield of diglycol diphenyl sulfonate is 84.5%,which is over 10% than the synthesis of diglycol p-methyl diphenyl sulfonate while the production cost is decreased 8%-10%.Diversion device is build up to increase the yield of alcohol ether and phenol sodium,pentyl alcohol replacing butanol used as dissolvant,the productive output can reach 87.6%,higher than that through the Williamson method,and the reaction time is curtailed six hours.The property and state of the two chemical compounds are systematically studied by microphotograph,thin-layer chromatograph,ultraviolet spectroscopy,infrared spectroscopy and IR spectra etc.