聚癸二酸甘油酯的优化合成

Optimum Synthesis of Poly(Glycerol Sebacate)

用等摩尔量甘油和癸二酸在N2流除水条件下缩聚,对N2流量和反应温度进行优化.采用FTIR、酸值、特性黏度、凝胶渗透色谱和1 H NMR对产物进行分析,得到优化反应条件.当N2流量0.1m3/h,聚合温度160℃,反应时间7.75h时,产物羧基酯化率达90.3%,特性黏度为42.0mL/g,数均相对分子质量为2 200,重均相对分子质量为249 800,相对分子质量大于10 000和3 000的组分质量分数分别为50.5%和71.5%.该方法经济性地合成了较高相对分子质量的聚癸二酸甘油酯.

Under water removed by certain N2 flow rate,PGS was prepared from glycerol and sebacic acid with equal molar ratio.To optimize N2 flow rate and reaction temperature,the products were analyzed by FTIR,acid value,intrinsic viscosity（[η]）,gel permeation chromatography（GPC）,and 1H NMR.The optimized reaction condition was confirmed as N2 flow rate of 0.1 m3/h,polymerization temperature of 160 ℃ and reaction time of 7.75 h.PGS obtained under this condition was with carboxyl esterification percent of 90.3%,[η] of 42.0 mL/g,Mn of 2 200 and Mw of 249 800.The mass percent of fraction with molecular weight over 10 000 and 3 000 were 50.5% and 71.5%,respectively.The results indicate that high molecular weight PGS can be economically synthesized using this method.