H_3PW_(12)O_(40)掺杂制备聚吡啶及其结构表征

Preparation and structural characterization of polypyridine doped with H_3PW_(12)O_(40)

采用H3PW12O40为氧化剂和掺杂剂，用化学氧化法制备聚吡啶．通过红外光谱、扫描电镜TG-DSC手段表征产物的结构和微观形貌，考察产物的热稳定性以及H3PW12O40物质量的浓度对转化率的影响．结果表明，随着体系中H3PW12O40物质量浓度的增加，单体转化率增加，最大可达到57％，之后则降低；制备的聚吡啶是从几十纳米到几个微米、大小不规律的颗粒状，并且伴随有团聚现象．在转化率达到57％之后得到的不用溶剂分离的产物中，含有形状规则的剩余无机H3PW12O40晶体TG-DSC分析表明，在500-590℃聚吡啶很快分解失重．

Polypyridine（PPY） was prepared by means of chemical polymerization with H3PW12O40 as oxidant and dopant, where the method of chemical oxidation was employed. The structure, and micromorphology of the product PPY were characterized with FTIR, SEM and TG-DSC, and the effect thermostability of the product and the concentration of H3PW12O40 on the conversion rate was investigated. The result showed that, the conversion rate of the monomer increased firstly with the concentration of H3PW12O40, with its maximum as 57%, and then decreased. The prepared product exhibited irregular granules of PPY with dimensions from dozens of nanometers to a few ones in diameter. Meantime, there was agglomerative phenomenon accompanying with it. After the conversion rate reached 57 %, the surplus inorganic crystalline of H3PW12O40 with regular form was contained in the product which was separated without solvent. It was shown by TG-DSC test that the polypyridine was decomposed quickly and lost weight when the temperature went up to 500-590 ℃.