公斤级生物基聚对苯二甲酸丙二醇酯制备及性能  

Kilogram-Scale Preparation and Performance of Bio-Based Poly(propylene glycol terephthalate)

作　　者：王浩南 魏志勇[1] 冷雪菲 李杨[1] Haonan Wang;Zhiyong Wei;Xuefei Leng;Yang Li(Department of Polymer Materials,School of Chemical Engineering,Dalian University of Technology,Dalian 116024,China)

机构地区：[1]大连理工大学化工学院高分子材料系,辽宁大连116024

出　　处：《高分子材料科学与工程》2022年第10期8-16,共9页Polymer Materials Science & Engineering

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5 L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)。研究了不同相对分子质量对生物基PTT性能的影响。采用核磁共振对所合成的PTT结构进行分析表征,采用乌氏黏度计测试聚酯特性黏度,换算得到聚酯黏均分子量在(4.7~6.3)×10^(4)之间。采用差示扫描量热法、X射线衍射仪和偏光显微镜研究了相对分子质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相对分子质量增加而减小,平衡熔点则随着相对分子质量的增加而升高,但均在相对分子质量高于5.5×10^(4)达到平衡;流变测试表明,相对分子质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,屈服强度随着相对分子质量的增加而增大,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。Kilograms of polytrimethylene terephthalate(PTT)with different molecular weight was synthesized by direct melt condensation in a 5 L stainless steel reactor, using terephthalic acid and biological 1,3-propylene glycol as raw materials and tetrabutyl titanate as catalyst. The synthesized PTT was identified by1HNMR. The viscosity average molecular weight was calculated from the intrinsic viscosity by Ubbelohde viscometer, and its value is(4.7~6.3) ×10^(4). The crystallization and melting behavior as function of molecular weight were investigated by differential scanning calorimetry(DSC), XRD and polarizing microscope(POM).The results demonstrate that the crystallinity and crystallization rate decrease with the increase of molecular weight, while the equilibrium melting point increases with the increase of molecular weight, reaching the equilibrium when the molecular weight is higher than 5.5 ×10^(4). Rheological tests show that the increase of molecular weight improves the elasticity and decreases the viscosity of the material. The mechanical properties test shows that the secondary yield phenomenon occurs in all samples under uniaxial tension. The yield strength is increased with the increase of molecular weight, while the elongation at break increases first and then decreases. This work is important for the acquisition of excellent performance biological PTT polyester with practical value.

关 键 词：生物基 聚对苯二甲酸丙二醇酯 熔融聚合 流变学 结晶动力学 

分 类 号：TQ323.41[化学工程—合成树脂塑料工业]