摘要
利用TiO2-SiO2（PVP）凝胶基催化剂（TSP），无溶剂条件下，以碳酸二苯酯与1，4-丁二醇为单体，采用常压预聚和真空缩聚两步熔融酯交换法合成了聚（对亚丁基）碳酸酯（PBC），考察了工艺条件，并对PBC的结构及物理性质进行了表征．实验结果表明，最佳工艺条件如下：预聚时间为2h，预聚温度为220～230℃（N：保护），缩聚温度为220℃，缩聚压力〈300Pa，催化剂用量为0．15wt％．优化条件下，PBC的特性黏数为1．12dL／g，M。为49000，M。为101000，PDI为2．07，Tg为-32．32℃，端羟基含量为6．2×10^-4mol／g，苯酚残留量为5．26wt％．在此工艺条件下，通过控制副产物苯酚的蒸出速率及其量，可以实现产品聚合度的可控，且苯酚几乎能够完全回收．
The synthesis of poly （ 1,4-butylene carbonate） （ PBC ） catalyzed by TiO2-SiO2 （PVP-gel） was studied via a two-step melt transesterification of diphenyl carbonate and 1,4-butanediol. After pre- polymerization of diphenyl carbonate and 1,4-butanediol in the standard atmosphere,the vacuum condensation reaction was operated. The PBC was characterized by IR, NMR, GPC and DSC. The experimental results showed that the optimum conditions of the reaction were as follows ： the reaction time and reaction temperature were 2 h and 220 ~ 230℃C （N2 protection） ,respectively,in the standard atmosphere pre-polymerization step. The reaction time,reaction pressure and the catalyst dosage were 2 h, ≤ 300 Pa and 0.15 wt% ,respectively, in the vacuum condensation step. The properties of the PBC prepared in optimum conditions,were as follows ： [ 7/] was 1. 12 dL/g, the M. was 49000, the Mw was 101000, the polydispersity index was 2.07, the Tg was -32. 32 ℃ ,the terminal hydroxyl content was 6.2×10^-4mol/g and the residue of the phenol was 5.26 wt%. The polymerization degree of PBC can be controlled by the evaporation rate and yield of phenol under the technological conditions. And the phenol by-product was recycled almost completely.
出处
《高分子学报》
SCIE
CAS
CSCD
北大核心
2014年第5期628-635,共8页
Acta Polymerica Sinica
基金
十二五国家科技支撑计划课题(项目号2013BAC11B05)
四川省青年科技创新研究团队专项计划(项目号2013 TD0010)资助项目
作者简介
通讯联系人，E-mail：gywang@cioc．ac．cn.
