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本文研究了以碳酸钾和对一二一溴甲基苯(PXDB)为原料,采用(?)基三乙基氯化铵(BTEAC/三乙胺(Et_3N)双催化法合成聚对苯二亚甲基碳酸酯(简称PC)的新工艺,测定了PC的分子量,用IR和NMR对产物结构进行了分析鉴定;并对聚合反应机理进行了探讨。实验结果表明:以乙腈为容剂,反应温度为80±2℃,催化剂用量BTEAC/K_2CO_3分子比为1/5,反应时间为48小时,可得到转化率为80.7%的聚碳酸酯。与文献相比本法具有如下优点:转化率高,反应时间短,生产成本降低,环境污染大为改善。此外,本文还对冠醚(CE)/Et_3N、季铵盐/KI、聚乙二醇(PEG)/Et_3N双催化体系进行了试验,发现双催化法比单催化法对PC的合成都有缩短反应时间和提高转化率的作用。
In this paper, we studied the synthesis of poly-p-phenylenebis (p-phenylenediamine) by potassium bicarbonate and p-dibromomethylbenzene (PXDB) Methyl carbonate (referred to as PC), the molecular weight of PC was measured, the structure of the product was analyzed and identified by IR and NMR, and the mechanism of polymerization was discussed.The experimental results show that with acetonitrile as the solvent, the reaction At the temperature of 80 ± 2 ℃, the BTEAC / K_2CO_3 ratio was 1/5 and the reaction time was 48 hours, the conversion of polycarbonate was 80.7% .Compared with the literature, this method has the following advantages: high conversion , The reaction time is short, the production cost is reduced and the environmental pollution is greatly improved.In addition, the dual ether (CE) / Et_3N, quaternary ammonium / KI, polyethylene glycol (PEG) / Et_3N catalysts were also tested in this paper, It is found that the dual catalysis method can shorten the reaction time and improve the conversion rate than the single catalysis method.