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探索了由对苯二甲酰氯和 1 ,3-丙二醇在“假高稀”条件下合成聚 (对苯二甲酸 -1 ,3-丙二酯 ) ( PTT)环状低聚物的可行性 .通过柱色谱分离了环状低聚物和线形低聚物 ;用核磁共振、质谱和元素分析表征了产物的化学结构 ;用 GPC和 HPLC研究了不同大小环的分布 ,发现在本文实验条件下合成的 PTT环状低聚物主要由二、三、四、五和七聚体构成 ,其中环状三聚体含量最多 ,没有发现环状六聚体的存在 .PTT环状低聚物的熔程为 92 .3～ 2 2 2 .6℃ ,熔融后是无色、透明的低粘度液体 .于 2 5 0℃将 PTT环状低聚物分别在辛酸亚锡、 1 -乙基 -3-氯四丁基锡氧烷、钛酸四丁酯和三氧化二锑催化下进行开环聚合反应 ,制备了特性粘数为0 .1 8～ 0 .4 9d L/ g的聚合物
The feasibility of synthesizing poly (1, 3-propane terephthalate) (PTT) cyclic oligomers from terephthaloyl chloride and 1,3-propanediol under “pseudosubstance” conditions was explored. The cyclic oligomers and linear oligomers were separated by column chromatography. The chemical structure of the products was characterized by NMR, MS and elemental analysis. The distribution of different size rings was investigated by GPC and HPLC. The results showed that under the experimental conditions Of the PTT cyclic oligomers are mainly composed of two, three, four, five and heptamer, in which the content of cyclic trimer is the most, and the existence of cyclic hexamers is not found.The melting range of PTT cyclic oligomer 92. 3 ~ 2 2 2 .6 ℃, after melting is a colorless, transparent, low viscosity liquid at 250 ℃ PTT cyclic oligomers were stannous octoate, 1 - ethyl-3-chloro Tetrabutylstannoxane, tetrabutyl titanate and antimony trioxide under the catalysis of a ring-opening polymerization reaction to prepare the intrinsic viscosity of 0.18 ~ 0. 49d L / g polymer