酯交换缩聚法合成高摩尔质量聚醚型聚氨酯的合成工艺与表征  

Synthesis Process and Characterization of High Molecular Weight Polyether-Polyurethane Elastomer by Transesterification Polycondensation Method

作　　者：刘冰灵 田恒水[1] 度静恬 

机构地区：[1]华东理工大学化工学院,上海200237

出　　处：《塑料工业》2015年第1期18-22,38,共6页China Plastics Industry

摘　　要：采用酯交换缩聚法,以聚四氢呋喃醚二醇(PTMEG)和1,6-六亚甲基二氨基甲酸甲酯(HDU)为原料,二丁基氧化锡为催化剂制备热塑性聚醚型聚氨酯(EU)弹性体。用红外光谱(IR)、凝胶渗透色谱(GPC)、热重分析(TGA)、力学性能测试等表征合成聚合物的性能。通过一系列单因素实验探讨了原料配比、预聚温度、缩聚温度等对EU弹性体特性黏数的影响规律。最佳制备工艺为:预聚阶段,分段变温80℃(0.5 h)→90℃(0.5 h)→100℃(0.5 h),压力为2.6 k Pa(1 h)→1.4 k Pa(0.5 h);缩聚阶段:温度为185℃,压力为0.2 k Pa,时间为1.75 h。制得特性黏数为1.553 d L/g、数均摩尔质量为87 079 g/mol的EU弹性体。其邵尓A硬度为68,拉伸强度为4.393 MPa,断裂伸长率为1 325.96%。Thermoplastic polyether-polyurethanes （EUs） elastomers were prepared by transesterification polycondensation from dimethyl-hexane-1, 6-dicarbamate （HDU） and PTMEG as raw materials and dibutyltin oxide as a catalyst. The properties of the EUs were characterized by IR, GPC, TGA and mechanical tests. The influence of synthesis conditions such as the ratio of the material, prepolymerization temperature and polycondensation temperature on the intrinsic viscosity was investigated by a series of single factor experiments. The EUs showed the optimum preparing condition was as follows： 80 ℃ （0. 5 h） -90 ℃ （0. 5 h） -100 ℃ （0.5 h） and 2. 6 kPa （1 h） -1.4 kPa （0.5 h） in the prepolymerization process, 185 ℃ （1.75 h） and 0.2 kPa （1.75 h） in the polycondensation process. The intrinsic viscosity of EU elastomer reached 1. 553 dL · g ^-1and the average molecular weight reached 87 079 g/mol. The mechanical testing of the EU elastomer Showed the Shore A hardness of 68, tensile strength of 4. 393 MPa, elongation at break of 1 325.96%.

关 键 词：酯交换缩聚 热塑型弹性体 1  6-六亚甲基二氨基甲酸甲酯 特性黏数 

分 类 号：TQ334.1[化学工程—橡胶工业]