聚二甲基二烯丙基氯化铵的合成

Research on the Polymerization Process of Preparing Polydimethyldiallylammonium Chloride(PDMDAAC)

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。

With industrial monomer solution of dimethyldiallylammonium chloride （DMDAAC） as raw material ,ammonium persulphate（APS） as initiator and NaaEDTA 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 （ NaaEDTA ） ： 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, ^13CNMR and FFIR spectra.