固相缩聚法快速合成高特性黏数聚2,5-呋喃二甲酸乙二醇酯:反应条件的影响  

Rapid Synthesis of Biobased PEF Polyester with High Intrinsic Viscosity via Solid State Polycondensation:Effect of Reaction Conditions

作　　者：李志松 吴林波[1] Zhi-song Li;Lin-bo Wu(Key Laboratory of Biomass Chemical Engineering of Ministry of Education,State Key Laboratory of Chemical Engineering,College of Chemical and Biological Engineering,Zhejiang University,Hangzhou 310058)

机构地区：[1]生物质化工教育部重点实验室、化学工程联合国家重点实验室、浙江大学化学工程与生物工程学院,杭州310058

出　　处：《高分子学报》2024年第12期1706-1715,共10页Acta Polymerica Sinica

基　　金：浙江省科技计划项目(项目号2022C01060);国家自然科学基金(基金号51773177);浙江大学-恒逸全球未来先进技术研究院资助项目.

摘　　要：以熔融-固相缩聚合成聚2,5-呋喃二甲酸乙二醇酯(PEF),考察了预聚物粒径大小、特性黏数(IV0)和呋喃二甲酸二甘醇酯链节含量(ϕDF)及反应温度(TSSP)等因素对固相缩聚(SSP)的影响.减小粒径、提高IV0和ϕDF、提高TSSP均有利于促进特性黏数的增长;但IV0和TSSP的提高会导致色泽加深,ϕDF高于6.4 mol%会导致PEF颗粒在210℃严重粘连.在优化的条件下(粒径0.2~0.8 mm、IV0约0.5 dL/g、ϕDF约6.4 mol%、TSSP为210℃)经SSP 10 h合成出特性黏数1.25 dL/g的浅色泽PEF,实现了高特性黏数PEF的快速SSP合成.Biobased poly(ethylene 2,5-furandicarboxylate)(PEF)with high intrinsic viscosity and light color can be synthesized via solid state polycondensation(SSP),but the reaction is often too slow so that too long time is required.In this study,the effects of the particle size,intrinsic viscosity(IV0),content of diethylene glycol furandicarboxylate units(ϕDF)of the prepolymer and SSP temperature(TSSP)on the SSP of PEF were investigated.It was found that the increase in TSSP,IV0 andϕDF,and the decrease in particle size were conducive to promoting the growth of IV.TheϕDF should not be higher than 6.4 mol%,and the crystallinity after pre-crystallization should not be less than 30%,otherwise it will lead to serious agglomeration of PEF particles at 210℃.The IV0 should not be higher than 0.60 dL/g,otherwise it will lead to significantly darkened color through SSP.Under optimal conditions(ϕDF=6.4 mol%,IV0=0.50 dL/g,particle size of 0.2-0.8 mm,TSSP=210℃),PEF with light color and high IV(1.25 dL/g)was rapidly(within 10 h)synthesized via SSP.This work presents an approach for rapid synthesis of PEF with high intrinsic viscosity and light color via SSP.

关 键 词：生物基聚酯 聚2 5-呋喃二甲酸乙二醇酯 固相缩聚 特性黏数 色泽 

分 类 号：TQ323.41[化学工程—合成树脂塑料工业]