微量三氟甲烷磺酸钇催化合成聚酯二元醇的工艺优化

Process optimization of polyester glycol with trace yttrium trifluoromethanesulfonate as catalyst

以微量三氟甲烷磺酸钇（Y（OTf），）为催化剂，在低于220℃的温度范围内，采用阶梯升温的方式，讨论了催化剂种类的用量、己二酸（AA）与1，4-丁二醇（BDO）单体配比、反应温度、反应时间等对产物特性黏数（[目]）的影响，优化了合成聚己二酸1，4-丁二醇酯二醇（PBAG）的工艺条件。采用FTIR和’HNMR技术对产物的结构进行了表征；采用DSC，TG，DTG技术对产物的热行为进行了研究。实验结果表明，在n（BDO）：n（AA）=1．5、Y（OTf），用量为0．0125％（x）（基于反应物AA的物质的量）、120～180℃阶梯升温反应10h的条件下所得产物PBAG的[η]=0．2219dL／g。表征结果显示，PBAG熔融温度为54．5℃，结晶温度为28．7℃，起始分解温度为316．2℃，失重50％时的温度为456．2℃。

Process optimization of poly（butylenes adipate） glycol （PBAG） with trace yttrium trifluoromethanesulfonate （Y（OTf）3） as catalyst by step-heating below 220 ℃ was studied. The influence of types and amount of catalyst, monomer mole ratio, reaction temperature and reaction time on intrinsic viscosity were discussed. Structure of the product was characterized by FTIR and 1H NMR. Thermal behavior of the product was studied by DSC, TG and DTG. Results showed that the intrinsic viscosity of the product was 0.221 9 dL/g when n（1, 4-butanediol, BDO） ： n（acrylic acid, AA） 1.5 and the usage of Y（OTf）3 was 0.012 5%（based on AA moles） by step-heating in 120-180 % for 10 h. Melting point of PBAG was 54.5 ℃, and crystallization point was 28.7 %. The initial thermal decomposition temperature of PBAG was 316.2 ℃, and fifty-percent weight-loss temperature was 456.2 ℃.