α-氰基丙烯酸正丁酯合成工艺的优化探究  

Optimizing exploration of synthesis process of n-butyl α-cyanoacrylate

作　　者：陈亚桥 伍林[1] 童坤[1] 丁建强[1] 李泽亚[1] 张琪[1] 张军锋[1] 刘盈[1] 饶文昊[1,2] 李亚伟 Chen Yaqiao;Wu Lin;Tong Kun;Ding Jianqiang;Li Zeya;Zhang Qi;Zhang Junfeng;Liu Ying;Rao Wenhao;Li Yawei(Institute of Applied Chemistry, Wuhan University of Science and Technology, Wuhan 430081, China;Institute of Nuclear Technology and Chemical Biology, Hubei Institute of Science and Technology, Xianning 437100, China)

机构地区：[1]武汉科技大学应用化学研究所,湖北武汉430081 [2]湖北科技学院核技术与化学生物学院,湖北咸宁437100

出　　处：《中国胶粘剂》2017年第12期12-16,共5页China Adhesives

摘　　要：在前期无溶剂法工艺的基础上,对医用胶粘剂α-氰基丙烯酸正丁酯单体的合成工艺进行了优化。着重探讨了复合助剂用量、脱水剂加入时间和反应完成后体系的不同p H对该合成反应的影响。研究结果表明:复合助剂在一定程度上简化了合成工艺,并且最佳质量比为m(复合助剂)∶m(氰乙酸正丁酯)=0.05∶1;当脱水剂在反应前或反应完成后加入体系时,前者具有相对更好的单体收率;当采用磷酸调节反应完成后体系的p H至8.0~8.5时,单体收率相对最高。采用FT-IR(红外光谱)法和1H-NMR(核磁共振氢谱)法成功表征了单体的结构,并且体外抗菌性试验也证实了目标单体能初步达到临床要求。The synthesis process of a n-butyl α-cyanoacrylate monomer for medical adhesive was optimizedon the basis of the previous solvent-free method. The influences of compound additive contents,adding time ofdehydrating agent and different p H values of system after reaction completion on the reaction were emphaticallydiscussed. The research results showed that the use of compound additive simplified the synthesis process on acertain extent,and the optimal mass ratio of m（compound additive）∶m（cyanide n-butyl acetate）was 0.05∶1.When the dehydrating agent was introduced into system before or after reaction completion,the former had therelatively better monomer yield. The monomer yield was relatively maximal when p H value of system after reactioncompletion was adjusted by phosphoric acid between 8.0 and 8.5. The monomer structure was successfullycharacterized by FT-IR（infrared spectroscopy）and1 H-NMR（nuclear magnetic resonance hydrogen spectrum）,and in vitro antibacterial test also confirmed that the target monomer can meet the clinical requirements.

关 键 词：医用胶粘剂 Α-氰基丙烯酸正丁酯 工艺优化 结构表征 抗菌性 

分 类 号：TQ225.24[化学工程—有机化工]