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室温下以膦腈碱(t-Bu P4)为催化剂,催化甲基丙烯酸烯丙酯(AMA)和甲基丙烯酸甲酯(MMA)进行负离子共聚反应.用核磁(1H-NMR、13C-NMR)、红外光谱(FTIR)、凝胶渗透色谱(GPC)、示差扫描量热仪(DSC)和热失重分析仪(TGA)等对聚合物结构和性能进行表征.结果发现,t-Bu P4能在室温下成功催化AMA与MMA的共聚反应,一步法合成结构可控的含悬垂双键共聚物.共聚反应中单体AMA和MMA的转化率均高于90%,且无交联或凝胶生成.通过NMR和FTIR对聚合物进行结构分析表明,AMA单体仅甲基丙烯酸酯双键参与聚合反应,烯丙基双键不参与聚合反应、无交联反应、环化反应等.聚合物中烯丙基结构单元的含量可通过体系中AMA/MMA的投料比调节.GPC结果表明所得共聚物分子量可控且分子量分布较窄.TGA和DSC结果表明,共聚物的热分解温度升高,玻璃化温度降低.
At room temperature, the allyl methacrylate (AMA) and methyl methacrylate (MMA) were catalyzed by phosphazene base (t-Bu P4) (FTIR), gel permeation chromatography (GPC), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) were used to characterize the structure and properties of the polymer. It was found that t- The copolymerization of AMA and MMA was successfully catalyzed at room temperature, and the structure-controlled double-bond-containing copolymer with a controlled structure was synthesized in one step.The conversion of monomer AMA and MMA in the copolymerization was higher than 90%, and no cross-linking or gel formation . The structural analysis of the polymer by NMR and FTIR showed that only the methacrylate double bond of AMA monomer was involved in the polymerization reaction, the allyl double bond did not participate in the polymerization reaction, no cross-linking reaction, cyclization reaction, etc. In the polymer The content of allyl structural units can be adjusted by the feeding ratio of AMA / MMA in the system.GPC results show that the molecular weight of the copolymer is controlled and the molecular weight distribution is narrow.TAGA and DSC results show that the thermal decomposition temperature of the copolymer increases, The temperature is lower.