摘要
新型杀菌剂双季铵盐以其杀菌效果好、毒性低、水溶性好等特点在工业中具有广泛应用前景。本文以十二胺、甲酸和甲醛为原料制备出中间体十二烷基二甲基叔胺,以二乙醇胺、氯化亚砜为原料合成连接基团分子2,2-二氯二乙胺,将合成的二种中间体进行加成反应得到二氯化N,N-双(十二烷基二甲基)-3-氮杂-1,5-戊二胺——一种新型双季铵盐。实验考察了十二烷基二甲基叔胺、2,2-二氯二乙胺以及双季铵盐的合成工艺条件,以单因素法考察了反应时间、反应温度及醇胺/氯化剂配比对合成产物的影响,筛选了较适宜的工艺条件。结果表明:在十二烷基二甲基叔胺的合成中,较适宜的总反应时间为12h左右;在2,2-二氯二乙胺的合成中,较适宜的n(二乙醇胺)∶n(氯化亚砜)为1∶2.5,反应时间为2h;在双季铵盐的合成中,较适宜的反应温度为80℃,反应时间为4h,在此工艺条件下,双季铵盐的收率可达81.2%。
The new-type germicide of biquaternary ammonium salt has wide application prospect in industry for its good sterilization effect,low toxicity and good solubility in water.In this paper,N,N-dimethyldodecylamine was prepared from dodecylamine,formic acid and formaldehyde as materials.And 2,2-chloride diethylamine was manufactured from diethanolamine,sulfoxide chloride,which is used as a group of the molecule space linker.Then,dichloride N,N-bis(dimethyldodecyl)-3-nitrogen-1,5-pentanediamine(a new-type of biquaternary ammonium salt)was synthesized fromN,N-dimethyldodecylamine and 2,2-chloride diethylamine by addition reaction.This synthesis conditions of N,N-dimethyldodecylamine,2,2-chloride diethylamine and the new-type germicide of biquaternary ammonium salt were inverstigated experimentally.And the method of single factor was used for studying the influences of reaction time and the molar ratio of diethanolamine to sulfoxide chloride on the yield of 2,2-chloride diethylamine.The results show that the optimum total reaction time is 12 hfor synthesis of N,N-dimethyldodecylamine;the optimum molar ratio of diethanolamine to sulfoxide chloride is 1∶2.5and the reaction time 2hfor manufatcuring2,2-chloride diethylamine;as well as the optimum reaction temperature is 80℃,reaction time 4hfor the new-type of biquaternary ammonium salt synthesis.And at these conditions,the yield of the new-type of biquaternary ammonium salt may attain 81.2%.
出处
《精细与专用化学品》
CAS
2015年第4期21-24,共4页
Fine and Specialty Chemicals