摘要
基于小试的反应原料和工艺条件,通过中试合成端氨基超支化聚合物(NH_2-HBP),并通过正交试验,以产率和氨基含量为检测指标,对中试合成工艺参数进行优化.结果表明:NH_2-HBP的最佳中试合成条件为N,N-亚甲基双丙烯酰胺和二乙烯三胺(DETA)的摩尔比为1∶1.2、反应温度为80℃、总反应时间为24h,相对于最佳小试合成条件,DETA的用量和反应温度均有所提高;NH_2-HBP的中试合成具有重复性和稳定性,平均产率为90.23%,平均氨基含量为2.717mmol/g,变异系数均较低,但相对于NH_2-HBP的最佳小试实验结果 ,产率和氨基含量稍有降低.
Based upon the raw materials and reaction conditions in bench-scale test,the aminoterminated hyperbranched polymers(NH2-HBP)was synthesized in bulk production.To optimize the synthesis process parameters were optimized through orthogonal test in which the yield and amino content were as indexes.The results showed that when the mol ratio of N,N′-methylene bisacrylamide and diethylene triamine was 1∶1.2,the temperature was 80 ℃and reaction time was 24 h,the NH2-HBP had the best yield and amino content.Compared with the optimal conditions of small scale synthesis of NH2-HBP,the amount of DETA and temperature were improved.The bulk production of NH2-HBP had repeatability and stability.The average yield of NH2-HBP was 90.23%,the average amino content of NH2-HBP was2.717mmol/g,and the coefficient of variation were low.But compared to the best synthesis result of NH2-HBP in small scale,the yield and amino content were slightly lower.
出处
《陕西科技大学学报(自然科学版)》
2016年第2期16-19,共4页
Journal of Shaanxi University of Science & Technology
基金
国家十二五科技支撑计划项目(2014BAE02B02)
陕西省科技厅重点科技创新团队计划项目(2013KCT-08)
陕西科技大学科研创新团队计划项目(TD12-04)
陕西科技大学研究生创新基金项目
关键词
端氨基超支化聚合物
中试
产率
氨基含量
amino-terminated hyperbranched polymers
bulk production
yield
amino content