摘要
以N,N-二甲基-1,3-丙二胺、尿素及1,4-二氯丁烷为原料,通过共缩聚反应两步法制备了一种新的主链型的水溶性聚季铵盐。采用正交试验获得了制备聚季铵盐的最佳条件:N,N-二甲基-1,3-丙二胺与尿素的物质的量比为2∶1,反应温度为135℃,反应时间为11 h,得到中间体双[3-(N,N-二甲基丙胺基)]丙脲,产率高达99%;中间体与1,4-二氯丁烷的物质的量比为1∶1,于90℃下反应6 h。采用红外光谱和核磁氢谱对产物结构进行表征,测定了其热稳定性和特性粘数。
Through two-step copolymerization using N, N-Dimethyl-l,3-propanediamine, urea, 1,4-dichlorobutane as raw materials, a new primary-chain water-soluble quaternary ammonium polymers was synthesized. The relationship between dosage of raw materials, reaction temperature, reaction time and rate of conversion was studies by orthogonal experiments. The optimum conditions were ascertained as follow: the molar ratio of N, N-dimethyl-l,3-propanediamine to urea is 2 : 1; the reaction temperature is 135~C; time is 11 h, the conversion of the intermediate was as high as 99%; and then the molar ratio of the intermediate to 1,4-dichlorobutane is 1 : l; the reaction temperature is 90℃; time is 6 h. The title polymers were characterized by FTIR, HNMR, thermoanalyses and intrinsic viscosity.
出处
《广州化学》
CAS
2013年第4期1-6,共6页
Guangzhou Chemistry
基金
广东省中科院战略合作项目(2011B090300003)
广东省农业攻关项目(2012B020308006)
石化技术转化服务平台建设项目(2012A01012)
关键词
主链型聚季铵盐
共缩聚两步法
正交试验
main-chain quaternary ammonium polymers
two-step copolymerization
orthogonal experiments
作者简介
干建群(1983~),女,工程师,硕士.
通讯作者:张敏,女,研究员,硕士生导师。zhangmin@gic.ac.cn