溶液聚合法制备聚膦腈

Solution Polymerization of Polyphosphazenes

以六氯环三膦腈为原料溶液聚合制备聚膦腈,用气泡观察法确定反应终点,代替目前采用的粘度观察法,制备了相对分子质量较高且分布较窄的聚膦腈并进行了表征,考察催化剂质量、溶剂质量、温度等因素对聚合反应的影响,同时探讨了两种聚膦腈衍生物的纯化方法。结果表明,聚膦腈的相对分子质量可达2×105以上,分布指数为1.6~1.7,收率为30%~40%（以聚二氯膦腈计）。聚合反应条件：六氯环三膦腈24 g;氨基磺酸50~55 mg;二水合硫酸钙45 mg;1,2,4-三氯苯20 mL;温度为210~215℃。

Polyphosphazenes with higher molecular weight and narrow polydispersities were synthesized from hexachlorocyclotriphosphazene by solution polymerization and then characterized. A bubble--observing method, a substitute of traditional viscosity--observing, was developed to determine the end--point of the reaction. The factors of polymerization such as the amount of catalyst, solvent and temperature were investigated. The Purifying of two polyphosphazene derivatives were also discussed. The results show that polyphosphazenes with molecular weight above 2 × 10^5 and polydispersity index of 1.6-1.7 can be obtained with 30%- 40% yield based on poly（dichlorophosphazene）. Polymerization conditions are as follows： hexachlorocyclotriphosphazene 24 g, sulfamic acid 50 - 55 mg, CaSO4 · 2H2O 45 mg, 1,2, 4 - trichlorobenzene 20 mL, reaction temperature 210-215℃.