4-(1-甲基胍基)丁酸的合成及其在造纸杀菌上的应用  

SYNTHESIS OF 4-METHYLGUANIDINE BUTYRIC ACID AND APPLIED IN TREATMENT OF PAPER MAKING WASTEWATER

作　　者：马璐[1] 郭睿[1] 来肖[1] 韦鹏[1] 田茂远 孙靖 

机构地区：[1]陕西科技大学教育部轻化工助剂化学与技术重点实验室,陕西西安710021 [2]陕西天宏硅材料有限责任公司,陕西西安710075 [3]西安三业精细化工有限责任公司,陕西西安710075

出　　处：《精细石油化工》2011年第3期70-73,共4页Speciality Petrochemicals

摘　　要：实验以N-甲基吡咯烷酮、盐酸、三氧化硫脲为原料，经两步反应合成了一种含羧基结构胍类杀菌剂——4-（1-甲基胍基）丁酸。第一步最佳合成条件为：n（N-甲基吡咯烷酮）：n（HCl）=1：2，反应温度135℃，反应时间5h，此时中间体4-甲基氨基丁酸盐酸盐的收率72．89％。第二步最佳合成条件为：n（4-甲基氨基丁酸盐酸盐）：n（三氧化硫脲）-1：1.2、反应温度25℃、反应时间12h，目标产物的收率79．45％。用傅里叶变换红外光谱、’HNMR对中间体和目标产物进行了结构表征。同时，将4-（1-甲基胍基）丁酸用于处理造纸污水，当污水中4-（1-甲基胍基）丁酸的质量分数为0．010％、杀菌时间24h，杀菌效果较佳。The 4-methylguanidine butyric acid was synthesized by N-methyl-pyrrolidone, hydrochloric acid, thiourea trioxide. The intermediate 4-（methylamino）butanoic acid salts was first prepared from N-metbyl-pyrroIidone in 10% HCI. Under the optimized reaction conditions： n（N-methyl pyrroli- done） ： n（HCl）=1 ： 2, reaction temperature 135 ℃, reaction time 5 h, the intermediate 4-（methyl- amino）butanoic acid salts was synthesized with the yield of 72.89%. The 4-methylguanidine butyric acid was obtained by reacting the intermediate with thiourea trioxide . Under the optimized reactionconditions for 4-methylguanidine butyric acid synthesis, n（4-（methylamino）butanoic acid salts） ： n （thiourea trioxide）=1 ： 1.2, reaction temperature 25 ℃, reaction time 12 h, the target product was synthesized with the yield of 79.45%. Both the intermediate and target product was characterized by means of FTdR, 1H NMR. The target product had been applied in the treatment of paper making wastewater and had promising property under the following appropriate conditions： target product mass fraction 0. 010% and sterilizing time 24 h.

关 键 词：N-甲基吡咯烷酮 盐酸 三氧化硫脲 羧基 胍类杀菌剂 

分 类 号：TQ455.47[化学工程—农药化工]