Poly(butylene 2,5-furan dicarboxylate), a Biobased Alternative to PBT: Synthesis, Physical Properties, and Crystal Structure

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• 作者：Jianhui Zhu ; Jiali Cai ; Wenchun Xie ; Pin-Hsuan Chen ; Massimo Gazzano ; Mariastella Scandola ; Richard A. Gross
• 刊名：Macromolecules
• 出版年：2013
• 出版时间：February 12, 2013
• 年：2013
• 卷：46
• 期：3
• 页码：796-804
• 全文大小：407K
• 年卷期：v.46,no.3(February 12, 2013)
• ISSN：1520-5835

文摘

This paper describes the synthesis, crystal structure, and physicomechanical properties of a biobased polyester prepared from 2,5-furandicarboxylic acid (FDCA) and 1,4-butanediol. Melt-polycondensation experiments were conducted by a two-stage polymerization using titanium tetraisopropoxide (Ti[OiPr]₄) as a catalyst. Polymerization conditions (catalyst concentration, reaction time and second stage reaction temperature) were varied to optimize poly(butylene-FDCA), PBF, and molecular weight. A series of PBFs with different M_w were characterized by DSC, TGA, DMTA, X-ray diffraction and tensile testing. Influence of molecular weight and melting/crystallization enthalpy on PBF material tensile properties was explored. Cold-drawing tensile tests at room temperature for PBF with M_w 16K to 27K showed a brittle-to-ductile transition. When M_w reaches 38K, the Young modulus of PBF remains above 900 MPa, and the elongation at break increases to above 1000%. The mechanical properties, thermal properties and crystal structures of PBF were similar to petroleum derived poly(butylenes-terephthalate), PBT. Fiber diagrams of uniaxially stretched PBF films were collected, indexed, and the unit cell was determined as triclinic (a = 4.78(3) 脜, b = 6.03(5) 脜, c = 12.3(1) 脜, 伪 = 110.1(2)掳, 尾 = 121.1(3)掳, 纬 = 100.6(2)掳). A crystal structure was derived from this data and final atomic coordinates are reported. We concluded that there is a close similarity of the PBF structure to PBT 伪- and 尾-forms.