微波辐射技术合成3-氯-2-羟基丙磺酸钠  

Synthesis of Sodium 3-Chloro-2-Hydroxy Propanesulfonate Under Microwave Irradiation

作　　者：李丕高[1] 郭妙[1] 李延[2] 

机构地区：[1]延安大学化学与化工学院,陕西延安716000 [2]西北大学分析科学研究所,陕西西安710069

出　　处：《石油化工》2008年第8期832-835,共4页Petrochemical Technology

基　　金：陕西省重点实验室科研基金项目(05JS38)

摘　　要：在微波辐射下,以环氧氯丙烷和亚硫酸氢钠为原料、去离子水为溶剂、四丁基溴化铵为相转移催化剂合成了3-氯-2-羟基丙磺酸钠;通过熔点测定和红外光谱分析对产物结构进行了表征;考察了原料配比、催化剂用量、反应温度、微波辐射功率、环氧氯丙烷滴加时间等因素对产物收率的影响。实验结果表明,微波辐射可明显促进3-氯-2-羟基丙磺酸钠的合成,在 n(亚硫酸氢钠):n(环氧氯丙烷):n(四丁基溴化铵)=1∶1.4∶0.0078、反应温度85℃、环氧氯丙烷滴加时间20 min、后续回流7 min、微波辐射功率500 W、微波辐射时间27 min 时,3-氯-2-羟基丙磺酸钠的收率可达85.8%。该方法具有操作简便、反应时间短、产物收率高等特点。Sodium 3-chloro-2-hydroxy propanesulfonate was synthesized from epichlorohydrin and sodium bisulfite under microwave radiation, using deionized water as solvent and tetrabutyl ammonium bromide as phase transfer catalyst. Structures of products were identified by micro-melting point measuring instrument and IR spectrometer. Experimental results show that microwave radiation tremendously enhanced the yield of sodium 3-chloro-2-hydroxy propanesulfonate. Effects of reactant ratio, dropping time of epichlorohydrin, catalyst dosage, microwave irradiaton power, and irradiation time on reaction were studied. Under optimal reaction conditions： n （sodium bisulfite ） ： n（epichlorohydrin） ： n （tetrabutyl ammonium bromide ） = 1 ： 1.4 ： 0. 007 8, reaction temperature 85 ~C, dropping time of epichlorohydrin 20 min, reflux time 7 rain, microwave irradiation power 500 W and irradiation time 27 min, yield of sodium 3-chloro-2-hydroxy propanesulfonate is 85.8 %. This method features short reaction time, high yield and simple operation.

关 键 词：环氧氯丙烷 亚硫酸氢钠 3-氯-2-羟基丙磺酸钠 微波辐射 催化 

分 类 号：TQ223.24[化学工程—有机化工]