光诱导活性沉淀聚合法合成聚甲基丙烯酸甲酯的研究

Study on Light-induced Atom Transfer Radical Precipatation Polymerization of Methyl Methacrylate

本文以2-羟基-2-甲基-1-苯基-1-丙酮(1173)为光引发剂,Fe Cl3·6H2O作为催化剂,六次甲基四胺作为配体,维生素C作为还原剂,在无水乙醇溶剂中进行聚合反应。通过光诱导原子转移自由基沉淀聚合法合成了聚甲基丙烯酸甲酯。研究了反应时间、光引发剂用量、还原剂用量、配体用量、催化剂用量等因素对聚合反应收率的影响。聚合物的红外谱图证实得到目标产物聚甲基丙烯酸甲酯。热分析结果表明该种方法得到的聚甲基丙烯酸甲酯金属残留量较低。并通过改变实验参数得到了甲基丙烯酸甲酯均聚的最佳反应条件:反应时间12 h,引发剂1173与单体总量的摩尔比为1:25,还原剂维生素C与单体总量的摩尔比为3:4,催化剂Fe Cl3·6H2O与单体总量的摩尔比为3:250,配体六次甲基四胺与单体总量的摩尔比为3:100。

In this paper, 1173 as the initiator, FeCl3·6H2O as a catalyst , hexamethylenetetramine as a ligand, vitamin C as a reducing agent, the polymerization reaction was carried out in ethanol solvent. Poly(methyl methacrylate)s were prepared via atom transfer radical polymerization precipitation polymerization. The effects of reaction temperature, the amount of initiator, reducing, ligand, catalyst on the polymerization have been investigated. The Poly(methyl methacrylate)s were characterized by FT-IR and differential thermal analysis of polymers. The optimal reaction conditions of synthesis of Poly(methyl methacrylate) were obtained by changing the experimental factor: the reaction time was 12 h, 1173 was 4.0% of the total monomers (molar ratio) , Vitamin C was 7.5% of the total monomers (molar ratio), catalyst was 1.2% of the total amount of the monomers (molar ratio), hexamethylenetetramine ligand was 3.0% of the total monomers (molar ratio) .