中性聚合物键合剂的精确合成方法

摘要

Neutral polymeric bonding agent(NPBA) was synthesized by means of the free radical copolymerization with acrylonitrile(AN) and hydroxyethyl methacrylate(HEA) in acetone solvent,with azobisisbutyronitrile(AIBN) as the initiator,β-mercap-toethanol(β-ME) as the chain transfer agent.The feeding mode was controlled according to the free radical copolymerization composition equation,the initiator dosage was determined according to the decomposition dynamics equation,chain transfer agent dosage was optimized according to the relation of the chain transfer agent and molecular weight,and ultimately the precision synthesis method of NPBA with more uniform structural composition,and controlled relative molecular weight and hydroxyl value was achieved.The study shows that optimal reactive condition for synthesizing 100 g NPBA with relative molecular weight of 4 000,hydroxyl value [OH] of 1.8 mmol/g is as follows:the dosage of HEA is 20 g,the dosage of AN is 80 g,the dosage of initiator AIBN and chain transfer agent β-ME are 6.037 g and 3.0 g respectively,and the dosage of HEA(7.62 g) drips off within 4 h,the reactive temperature is 65 ℃,and reactive time is 6 h.%采用丙烯酸羟乙酯(HEA)与丙烯腈(AN)在丙酮溶剂中进行自由基聚合来制备中性聚合物键合剂(NPBA),其中,偶氮二异丁腈(AIBN)为引发剂,β-巯基乙醇(β-ME)为链转移剂.根据自由基共聚组成方程来控制投料方式,根据引发剂分解动力学方程来确定引发剂用量,根据链转移剂与分子量关系来优化链转移剂用量,最终实现结构组成较均匀、相对分子质量和羟值可控的NPBA精确合成方法.研究表明,合成100 g相对分子质量为4 000、羟值为1.8 mmol/g左右的NPBA的反应条件为HEA用量为20 g、AN用量为80 g,AIBN用量为6.037 g,β-ME用量为3.0g.其中,7.62 g HEA 4 h滴完,反应温度为65℃,反应时间6h.