新型双季铵盐[二氯化NN-双(十二烷基二甲基)-3-氮-摩田化学.docVIP

新型双季铵盐[二氯化N,N-双(十二烷基二甲基)-3-氮 杂-1,5-戊二胺]杀菌剂的合成 李洪霞1 王以元2 施云海1* 顾宇辉2 （1华东理工大学化学工程研究所，上海市徐汇区梅陇路130号368信箱，上海200237; 2上海摩田化学有限公司，上海市闵行区虹梅南路786号1301室 上海 200237） 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，将两者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/氯化剂摩尔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12.0h左右；在2,2-二氯二乙胺的合成中，二乙醇胺与氯化亚砜的较适宜摩尔配比为1:2.5，反应时间为5h；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%。 关键词：杀菌剂；十二烷基二甲基叔胺；2,2-二氯二乙胺；二氯化N,N-双(十二烷基二甲基)-3-氮杂-1,5-戊二胺 Synthesis of a New-type germicide of biquaternary ammonium salt and Shi Yunhai* Li Hongxia 1 Wang Yiyuan2 Shi Yunhai1* and Gu Yuhui2 (1Reseach Centre of Chemical Engineering, 130 Meilong Road, East China University of Science and Technology, Shanghai 200237, 2 Shanghai mlandchem Ltd. Co., Room 1301,786 Southern Hongmei Road, Shanghai 200237) Abstract: 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 from N,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 optim