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运用RAFT活性自由基聚合方法探索了具有一定立构规整性的聚丙烯腈的合成。合成得到RAFT聚合的链转移剂MESA,并以1 H NMR进行了表征;以MESA作为链转移剂、碳酸乙烯酯为溶剂,在单体浓度为0.80 M、60℃、原料配比[AN]0/[MESA]0/[AIBN]0为2500∶5∶1的聚合条件下,成功合成出较高分子量(Mn=5.60×104g/mol)、窄分子量分布(PDI=1.15)的聚丙烯腈;进一步在各单体浓度的RAFT聚合中,加入单体摩尔量3%的AlCl3,得到聚丙烯腈数均分子量为6.1×104~6.5×104g/mol,全同立构组成为mm=32.1%~32.6%,聚合产物分子量分布宽度介于1.31~1.38之间,从而实现了在RAFT活性聚合体系中通过Lewis酸的作用合成得到具有一定立构规整性的聚丙烯腈。
The RAFT active radical polymerization method was used to explore the synthesis of polyacrylonitrile with certain stereoregularity. RAFT polymerization chain transfer agent MESA synthesized and characterized by1H NMR; MESA as a chain transfer agent, ethylene carbonate as a solvent, at a monomer concentration of 0.80 M, 60 ° C, the feed ratio [AN] 0 Polyacrylonitrile with high molecular weight (Mn = 5.60 × 104g / mol) and narrow molecular weight distribution (PDI = 1.15) was successfully synthesized under the polymerization conditions of [MESA] 0 / [AIBN] 0 of 2500: Further, in the RAFT polymerization of each monomer concentration, adding 3% of the monomer molar amount of AlCl3 to obtain a polyacrylonitrile having a number average molecular weight of 6.1104 to 6.5104g / mol and an isotactic composition of mm = 32.1% 32.6%, and the width of the molecular weight distribution ranged from 1.31 to 1.38. Thus, polyacrylonitrile with a certain stereoregularity was synthesized through the action of Lewis acid in the RAFT polymerization system.