公斤级生物基聚对苯二甲酸丙二醇酯制备及性能
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1.大连理工大学高分子系;2.大连理工大学高分子材料系

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Kilogram-scale Preparation and Performance Study on Bio-based Poly(propylene glycol terephthalate)
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    摘要:

    以对苯二甲酸、生物基1,3-丙二醇为原料,选用钛酸四丁酯为催化剂,通过熔融缩聚工艺在5L不锈钢反应釜中制备了公斤级生物基聚对苯二甲酸丙二醇酯(PTT)。研究了不同分子量对生物基PTT性能的影响。采用1H-NMR对所合成的PTT结构进行分析表征,采用乌氏粘度计测试聚酯特性粘度,换算得到聚酯黏均分子量在47000~63000g/mol之间。采用差示扫描量热法(DSC)、x射线衍射仪(XRD)和偏光显微镜(POM)研究了分子量对结晶熔融行为的影响,结果表明结晶度和结晶速率随着分子量增加而减小,平衡熔点则随着分子量的增加而增大,但均在分子量高于55427g/mol达到平衡;流变测试表明分子量的增加提高了材料的弹性,降低了黏性;力学性能测试表明所有样品在单轴拉伸时均出现二次屈服现象,屈服强度随着分子量的增加而增大,断裂伸长率则先增大后减小。该研究对获得具有实用价值的高性能生物基PTT聚酯具有重要意义。

    Abstract:

    Kilograms of polytrimethylene terephthalate (PTT)with different molecular weight was synthesized by direct melt condensation in a 5L stainless steel reactor, which used terephthalic acid and biological 1,3-propylene glycol as raw materials and tetrabutyl titanate as catalyst. The synthesized PTT was identified by 1H-NMR. The viscosity average molecular weight was calculated from the intrinsic viscosity by Ubbelohde viscometer, and its value was between 47000 and 63000g/mol. The crystallization and melting behavior as function of molecular weight were investigated by Differential Scanning Calorimetry (DSC), XRD and polarizing microscope (POM). The results demonstrated that the crystallinity and crystallization rate decreased with the increase of molecular weight, while the equilibrium melting point increased with the increase of molecular weight. It reached equilibrium when the molecular weight was higher than 55427g/mol. Rheological tests showed that the increase of molecular weight improved the elasticity and decreased the viscosity of the material. The mechanical properties test showed that the secondary yield phenomenon occurred in all samples under uniaxial tension. The yield strength increased with the increase of molecular weight, while the elongation at break increased first and then decreased. This work is important for the acquisition of excellent performance biological PTT polyester with practical value.

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  • 收稿日期:2022-02-28
  • 最后修改日期:2022-03-24
  • 录用日期:2022-03-28
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