聚苯乙烯交联微球的氯甲基化方法研究

Study on preparing chloromethylated crosslinking polystyrene microsphere

以异戊醇、多聚甲醛及氯化亚砜为主要原料,合成了氯甲基化试剂氯甲基异戊醚。并采用原位法对聚苯乙烯交联微球进行氯甲基化。利用傅里叶红外光谱仪对产物结构进行了表征,以莫尔滴定法对氯球的氯含量进行了测定。考察了各物料配比、反应时间对氯甲基化反应的影响规律。获得最佳反应条件为：异戊醇∶多聚甲醛∶氯化亚砜∶聚苯乙烯∶四氯化锡∶二氯甲烷（均为物质的量比）=1∶2.4∶2.4∶7.2∶0.8∶7.2,氯甲基异戊醚合成阶段反应温度为3~5℃,反应时间为7h;氯甲基化合成阶段反应温度为15~20℃,反应时间为12h,总计反应时间为19h。制得的氯球的氯含量可达18%（wt,质量分数）。

A new chloromethylation reagent, chloromethylisoamylether, was prepared by isoamyl alcohol, paraform- aldehyde and thionyl chloride. The chloromethylation of polystyrene （PS） was prepared by chloromethylisoamylether in-situ generation way. The chemical structure and composition of products were characterized with FT-IR and Mohr method. The effects of molar ratio of reactants and reaction time on the chloromethylation were studied. The optimal reaction conditions were as follows： n （ isoamyl alcohol） ： n （paraformaldehyde） ： n （ thionyl chloride） ： n （polystyrene） ： n （ tin tetrachloride） ：n （ di- chloromethane） =1：2.4：2.4：7.2：0.8： 7.2. The chloromethylation reaction were at 15~20℃ for 19h. Under these condi tions, the chlorine content of chloromethylated crosslinking polystyrene microsphere reached 18% （wt）.