聚二甲基二烯丙基氯化铵的合成

以一步法工业单体二甲基二烯丙基氯化铵(DMDAAC)为原料,以过硫酸铵(APS)为引发剂,采用一次性加入引发剂,梯度升温,分步引发水溶液聚合反应的方法,对制备聚二甲基二烯丙基氯化铵(PDMDAAC)的聚合反应的工艺进行了优化研究。在前期实验基础上,用正交优化等方法研究了w(DMDAAC)(简称A)、w(APS)(简称B,以其质量占单体质量的百分比计)、w(Na4EDTA)(简称C,以其质量占单体质量的百分比计)和聚合反应引发温度(简称D)等因素对产物PDMDAAC特征黏度影响强弱的顺序和影响规律。结果表明:各因素影响强弱排序为A>B>D>C。最佳工艺条件为:A为65.0%,B和C分别为0.35%和0.007%,聚合反应在引发温度D44℃下反应3 h后,再在聚合反应温度50℃下反应3 h,最后在成熟温度70℃下完成反应3 h。在最佳工艺条件下得到的PDMDAAC产物的特征黏度为1.59 dL.g-1,单体转化率为95%;产物的最高特征黏度达到1.71 dL.g-1,单体转化率为94%。此外,对产物的结构、性质用1HNMR1、3CNMR和FTIR进行了分析表征。研究表明,所得的合成工艺方法是一种经济、清洁、易于工业化的PDMDAAC制备方法。

Research on the Polymerization Process of Preparing Poly-dimethyldiallylammonium Chloride(PDMDAAC)

With industrial monomer solution of dimethyldiallylammonium chloride(DMDAAC) as raw material,ammonium persulphate(APS) as initiator and Na_4EDTA as chelating agent,using the methods of adding initiator all at once,graduated increasing of temperature and stepwise initiation and polymerization,the polymerization process of preparing poly-dimethyldiallylammonium chloride(PDMDAAC) was researched.The influencing factors such as initial content of monomer w(DMDAAC)(A),m(APS)∶m(DMDAAC)(B),m(Na_4EDTA)∶m(DMDAAC)(C) and the temperature of initiation(D) on the intrinsic viscosity of PDMDAAC were investigated via the orthogonal experimental method.The results showed that the functional strength order of the factors was A>B>D>C,and the optimal process conditions were A=65.0%,B=0.35%,C=0.007%,and polymerization carried out at 44 ℃,50 ℃ and 70 ℃,each for 3 h.The intrinsic viscosity of PDMDAAC and conversion rate of monomer under optimal process conditions reached 1.59 dL·g~(-1) and 95% respectively.The highest value of intrinsic viscosity of PDMDAAC was 1.71 dL·g~(-1),and the corresponding monomer conversion rate was 94%.Structure of the product was characterized via ~1HNMR,~(13)CNMR and FTIR spectra.