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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

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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0.2~0.8mm、IV0约0.5 dL/g、φDF约6.4 mol%、TSSP为210 ℃)经SSP 10h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.
Rapid Synthesis of Biobased PEF Polyester with High Intrinsic Viscosity via Solid State Polycondensation:Effect of Reaction Conditions
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 and φDF,and the decrease in particle size were conducive to promoting the growth of Ⅳ.The φDF 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.

Biobased polyesterPoly(ethylene 25-furandicarboxylate)Solid state polycondensationIntrinsic viscosityColor

李志松、吴林波

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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

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

2024

高分子学报
中国科学院化学研究所 中国化学会

高分子学报

CSTPCD北大核心
影响因子:0.844
ISSN:1000-3304
年,卷(期):2024.55(12)