APS引发制备高分子量PDMDAAC

Preparation of Poly(dimethyldiallylammonium chloride) via APS Initiation

以已知杂质种类和含量的一步法工业二甲基二烯丙基氯化铵（DMDAAC）单体水溶液为原料．用过硫酸铵（APS）为引发剂，采取低温一次性加入引发剂，分阶段升温方式进行聚合反应．通过合成工艺的优化方法，得到了最高特性黏数值为3．17dL／g的聚二甲基二烯丙基氯化铵（PDMDAAC），单体转化率为94．8％．采用NMR、IR光谱测试技术对产物进行了结构表征。分别考察了DMDAAC质量分数为57．5％～70．0％、APS与DMDAAC质量比为0．15：100～0．40：100、Na4EDTA与DMDAAC质量比为0—0．0142：100、聚合反应引发温度T1在40—50℃、聚合反应熟化温度T3在50—90℃范围内的以上5个因素对产物特性黏数和单体转化率的影响规律。结果表明，DMDAAC质量分数为65．0％、APS与DMDAAC质量比为0．35：100、Na4EDTA与DMDAAC质量比为0．0071：100、T1为46℃、T2为50℃，T3为70℃。各反应3h为最佳工艺条件。

Using ammonium persulphate as the initiator and industrial grade dimethyldiallylammonium chloride（DMDAAC） as the monomer, PDMDAAC with high molecular mass was obtained by adding all the initiator in one shot and raising the polymerization temperature in steps. The maximum intrinsic viscosity of the product PDMDAAC could reach 3.17 dL/g, and the monomer conversion rate was 94. 8%. The product structure was characterized by FTIR and NMR. The effect of process conditions, such as the concentration of DMDAAC, the mass ratio of APS to DMDAAC, the mass ratio of Na4EDTA to DMDAAC, initiating temperature T1 and reaction temperature T3 on the intrinsic viscosity of the product and monomer conversion were investigated respectively. The results showed that the optimum process conditions were mass concentration of DMDAAC 65.0%, mass ratio of APS to DMDAAC 0.35：100, mass ratio of Na4EDTA to DMDAAC 0. 007 1： 100, T1 =46 ℃, T2 =50 ℃ and T3 =70 ℃, with 3 h reaction time at each temperature.