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以4,4-(9-芴)二苯酚(BHPF)和碳酸二苯酯(DPC)为原料,采用熔融酯交换法合成了4,4-(9-芴)二苯酚型聚碳酸酯(BHPF-PC).红外光谱、核磁共振碳谱及氢谱测试结果证实了所得聚合物的化学结构.采用了四苯基膦苯酚盐(C_(30)H_(25)OP)等2种季磷盐以及3种碱性无机盐催化剂作为合成聚碳酸酯的催化剂,结果四苯基膦苯酚盐的催化效果最好.分析了DPC/BHPF初始摩尔比对BHPF-PC的影响规律,随着DPC/BHPF初始摩尔比的增加,BHPF-PC的分子量呈现先增加后降低的趋势.进一步研究了聚合工艺包括缩聚时间和缩聚温度对BHPF-PC的影响,结果表明BHPF-PC分子量达到最大值所需要的时间随DPC/BHPF初始摩尔比的增加而增加.初始摩尔比为1.1∶1的DPC和BHPF,在1×10~(-5)mol/mol(BHPF)的四苯基膦苯酚盐催化作用下,于330℃缩聚150 min可以获得分子量最大的BHPF-PC.最后研究了BHPF-PC的耐高温性能和光学性能,其Tg达到了275℃,空气中失重率为5%时的分解温度T5%为440℃,同时透光率达到了88.1%,表明BHPFPC是一种具有优异耐高温性能的高光学透明材料.
4,4 ’(9-fluorene) diphenol polycarbonate (BHPF) was synthesized by melt transesterification using 4,4- (9-fluorene) diphenol (BHPF) and diphenyl carbonate (DPC) -PC) .The results of FT-IR, 1HNMR and 1HNMR confirmed the chemical structure of the obtained polymer.We used two kinds of quaternary phosphonium salts such as tetraphenylphosphine phenoxide (C_ (30) H_ (25) OP) As well as three kinds of basic inorganic salt catalysts as catalysts for the synthesis of polycarbonates, the tetraphenylphosphine phenolate has the best catalytic effect.The influence of the initial molar ratio of DPC / BHPF on BHPF-PC was analyzed. With the increase of DPC / BHPF The molecular weight of BHPF-PC first increased and then decreased, and the effect of polymerization process including polycondensation time and polycondensation temperature on BHPF-PC was further studied.The results showed that the time required for BHPF-PC to reach the maximum value With the increase of the initial molar ratio of DPC / BHPF, DPC and BHPF with the initial molar ratio of 1.1: 1 catalyzed by tetraphenylphosphinophenol under 1 × 10 ~ (-5) mol / mol (BHPF) The highest molecular weight BHPF-PC was obtained by polycondensation at 330 ℃ for 150 min. Finally, the high temperature and optical properties of BHPF-PC were studied. The Tg reached 275 ℃, The decomposition temperature T5% at the rate of 5% weight loss in gas was 440 ℃, and the light transmittance reached 88.1%, indicating that BHPFPC is a kind of highly optically transparent material with excellent high temperature resistance.