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采用单电子转移活性自由基聚合(SET-LRP)方法,以丙烯酰胺(AM)、2-丙烯酰胺-2-甲基丙磺酸(AMPS)和N-乙烯基吡咯烷酮(NVP)为单体原料,Cu0粉为催化剂,四氯化碳(CCl4)为引发剂,三(2-二甲氨基乙基)胺(Me6-TREN)为配体,在水溶液中实现了星形三元共聚物P(AM-AMPS-NVP)的合成。通过IR与13 C-NMR分析,证明所得聚合物是目标产物。通过系列实验,考察了催化剂用量、引发剂用量、配体用量及w(单体)和单体物质的量比对三元共聚物P(AM-AMPS-NVP)聚合反应的影响。结果表明,得到共聚物的最佳制备条件为引发温度25.0℃,单体n(AM)∶n(AMPS)∶n(NVP)=8.5∶1∶0.5,反应物溶液中w(单体)=25%,引发剂w(CCl4)=0.082%、催化剂w(Cu0)=0.019 0%、配体w(Me6-TREN)=0.073%时,所得聚合物产品相对分子质量最高,达到227万。
A single electron transfer active radical polymerization (SET-LRP) method was used to synthesize acrylamide (AM), 2-acrylamide-2-methylpropanesulfonic acid (AMPS) and N-vinyl pyrrolidone (NVP) , Cu0 powder as catalyst, carbon tetrachloride (CCl4) as initiator and tris (2-dimethylaminoethyl) amine (Me6-TREN) as ligand, a ternary terpolymer P AM-AMPS-NVP). By IR and 13 C-NMR analysis, it was confirmed that the resulting polymer was the target product. A series of experiments were conducted to investigate the influence of the amount of catalyst, the amount of initiator, the amount of ligand and the ratio of w (monomer) to monomer on the polymerization of terpolymer P (AM-AMPS-NVP). The results showed that the optimal conditions for the preparation of the copolymer were as follows: the initiator temperature was 25.0 ℃, the monomer n (AM): n (AMPS): n (NVP) = 8.5:1:0.5, 25%, CCl4 = 0.082%, catalyst w (Cu0) = 0.019 0%, ligand w (Me6-TREN) = 0.073%, the highest molecular weight of the obtained polymer product reached 2.27 million.