聚癸二酸甘油酯的优化合成

Optimum Synthesis of Poly(Glycerol Sebacate)

  • 摘要: 用等摩尔量甘油和癸二酸在N<sub<2</sub<流除水条件下缩聚,对N<sub<2</sub<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<sup<1</sup<H NMR对产物进行分析,得到优化反应条件. 当N<sub<2</sub<流量0.1 m<sup<3</sup</h,聚合温度160 ℃,反应时间7.75 h时,产物羧基酯化率达90.3%,特性黏度为42.0 mL/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.

     

    Abstract: Under water removed by certain N<sub<2</sub< flow rate, PGS was prepared from glycerol and sebacic acid with equal molar ratio. To optimize N<sub<2</sub< flow rate and reaction temperature, the products were analyzed by FTIR, acid value, intrinsic viscosity (<em<η</em<), gel permeation chromatography (GPC), and <sup<1</sup<H NMR. The optimized reaction condition was confirmed as N<sub<2</sub< flow rate of 0.1 m<sup<3</sup</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%,<em<η</em< of 42.0 mL/g, <em<M</em<<sub<n</sub< of 2 200 and <em<M</em<<sub<w</sub< 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.

     

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