4-(1-甲基胍基)丁酸的合成及其在造纸杀菌上的应用

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(HCI)=1∶2,反应温度135℃,反应时间5 h,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12 h,目标产物的收率79.45%.用傅里叶变换红外光谱、1H NMR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24 h,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-methyl-pyrrolidone in 10％ HCl. Under the optimized reaction conditions: n(N-methyl pyrrolidone) : 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 reaction conditions 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 FT-IR, 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.