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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
E-mail: wulinbo@zju.edu.cn
纸质出版日期:2024-12-20,
网络出版日期:2024-09-26,
收稿日期:2024-05-31,
录用日期:2024-07-12
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李志松, 吴林波. 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. 高分子学报, 2024, 55(12), 1706-1715
Li, Z. S.; Wu, L. B. Rapid synthesis of biobased PEF polyester with high intrinsic viscosity via solid state polycondensation: effect of reaction conditions. Acta Polymerica Sinica, 2024, 55(12), 1706-1715
李志松, 吴林波. 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. 高分子学报, 2024, 55(12), 1706-1715 DOI: 10.11777/j.issn1000-3304.2024.24153. CSTR: 32057.14.GFZXB.2024.7274.
Li, Z. S.; Wu, L. B. Rapid synthesis of biobased PEF polyester with high intrinsic viscosity via solid state polycondensation: effect of reaction conditions. Acta Polymerica Sinica, 2024, 55(12), 1706-1715 DOI: 10.11777/j.issn1000-3304.2024.24153. CSTR: 32057.14.GFZXB.2024.7274.
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(IV
0
)和呋喃二甲酸二甘醇酯链节含量(
ϕ
DF
)及反应温度(
T
SSP
)等因素对固相缩聚(SSP)的影响. 减小粒径、提高IV
0
和
ϕ
DF
、提高
T
SSP
均有利于促进特性黏数的增长;但IV
0
和
T
SSP
的提高会导致色泽加深,
ϕ
DF
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、IV
0
约0.5 dL/g、
ϕ
DF
约6.4 mol%、
T
SSP
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 (IV
0
)
content of diethylene glycol furandicarboxylate units (
ϕ
DF
) of the prepolymer and SSP temperature (
T
SSP
) on the SSP of PEF were investigated. It was found that the increase in
T
SSP
IV
0
and
ϕ
DF
and the decrease in particle size were conducive to promoting the growth of IV. The
ϕ
DF
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 IV
0
should not be higher than 0.60 dL/g
otherwise it will lead to significantly darkened color through SSP. Under optimal conditions (
ϕ
DF
=6.4 mol%
IV
0
=0.50 dL/g
particle size of 0.2-0.8 mm
T
SSP
=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.
生物基聚酯聚25-呋喃二甲酸乙二醇酯固相缩聚特性黏数色泽
Biobased polyesterPoly(ethylene 25-furandicarboxylate)Solid state polycondensationIntrinsic viscosityColor
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