聚醚型聚氨酯弹性体的制备及改性
摘要
聚氨酯由于其结构的特殊性而被广泛用作阻尼材料。聚氨酯的粘弹性可以把机械振动能量转变为热能耗散掉。单一的聚氨酯弹性体由于阻尼损耗因子不够高或阻尼温域较窄,从而需进行改性处理。
本文制备了聚醚型聚氨酯弹性体并进行了有机小分子的改性,通过红外光谱(FT-IR)对材料的化学结构进行讨论；通过差示扫描热分析(DSC)对材料中有机小分子的形态进行分析；通过扫描电子显微镜(SEM)对材料的形貌进行表征；通过硬度计,动态力学分析仪对材料的宏观性能进行了测试。
首先,论文研究了聚醚型聚氨酯的性能影响因素：软段分子量越大,损耗因子越小,柔顺性越好；TDI体系比IPDI体系的损耗因子高,刚性大。综合考虑确定以硫醚作为扩链剂,扩链系数选取0.8,并加入预聚体质量10%的DBP作为稀释剂制备改性基体。
其次,研究了DZ对聚醚型聚氨酯的改性作用。DZ的引入使得PU硬度下降、低温下储能模量的上升、tg和tanδ均升高。PU/DZ中DZ的有三种存在方式：(1)以氢键与PU结合；(2)在PU内部结晶；(3)在PU表面析出结晶。不同体系的改性作用对比表明：60%含量的DZ对IPDI体系的改性作用优于TDI体系；对PPG-1000体系的改性作用优于PPG-2000体系。不同DZ加入量的PPG-1000/TDI体系性能研究表明：60%含量DZ的的损耗因子峰值最大,为0.87。80%含量DZ的玻璃化转变温度最高,为3.5℃。对不同加入方式的改性研究表明：DZ的分散性越好,改性作用越强。
最后,研究了抗氧剂1010对聚醚型聚氨酯的改性作用。1010的引入使得PU硬度下降、低温下储能模量的上升、tg和tanδ均升高。PU/1010中1010有四种存在方式：(1)以化学键与PU结合；(2)以氢键与PU结合；(3)在PU内部结晶；(4)在PU表面析出结晶。不同体系的改性作用对比表明：60%质量含量的抗氧剂1010的加入对IPDI体系的改性作用更为明显,损耗因子峰值增加了一倍。不同1010加入量的PPG-1000/TDI体系性能研究表明：40%含量1010的PU/1010材料的损耗因子峰值最大为0.89。70%含量DZ的PU/DZ材料的玻璃化转变温度升至7℃。对不同加入方式的改性研究表明：1010的分散性越好,改性作用越强。
Polyurethane has been widely used as damping materials because of the specificity of its structure. Mechanical vibration energy can be transformed into heat and dissipative attenuation by the viscoelasticity of polyurethane. The pure polyurethane elastomer has low damping loss factor and narrow damping temperature domain, which need to be modified.
In this paper, polyether-polyurethane elastomer was synthesized and modified by small organic molecules. The chemical structure of materials was discussed by FT-IR spectra. The form of small organic molecules in material was analyzed by DSC. The morphology of material was characterized by SEM. And the macroeconomic performances were characterized by DMA and sclerometer.
First of all, factors that affect the performance of polyether-polyurethane were studied. Greater soft segment molecular weight makes the smaller loss factor and the better flexibility. Compared with the system of IPDI, the system of TDI has a higher loss factor. The modified matrix was synthesized with the DMTDA as chain extenders, equivalent coefficient of 1.1 and 10% of DPB, which used as diluents.
Second, modified polyether-polyurethane by DZ was studied. When put DZ-doped into the PU, the performance of material was changed:hardness decreased, storage modulus at the low temperature raised, tg and tan8 increased. There are three state of DZ in PU/DZ hybrid materials:(1) combination with PU by hydrogen; (2) as crystal in the PU internal; (3) as crystal on the surface of PU. The performance of PU/DZ in different system, which containing DZ with 60% mass fraction of prepolymer, was compared. Modification of IPDI system is superior to the modification of TDI system. Modification of PPG-2000 system is superior to the modification of PPG-1000 system. The performance of PPG-1000/TDI system with different content of DZ was compared. The PU/DZ with 60% content of DZ has the largest loss factor, which was 0.87. The PU/DZ with 80% content of DZ has the highest tg, which was 3.5℃. The performance of PPG-1000/TDI system with different way to add DZ was compared. Better dispersion of DZ, better performance of materials.
Finally, modified polyether-polyurethane by 1010 was studied. When put 1010-doped into the PU, the performance of material was changed:hardness decreased, storage modulus at the low temperature raised, tg and tanδincreased. There are four state of DZ in PU/DZ hybrid materials:(1) combination with PU by chemical bonds; (2) combination with PU by hydrogen; (3) as crystal in the PU internal; (4) as crystal on the surface of PU. The performance of PU/1010 in different system, which containing 1010 with 60% mass fraction of prepolymer, was compared. Modification of IPDI system is superior to the modification of TDI system. The Loss factor peak of IPDI system was doubled. The performance of PPG-1000/TDI system with different content of 1010 was compared. The PU/1010 with 40% content of DZ has the largest loss factor, which was 0.89. The PU/DZ with 70% content of DZ has the highest tg, which was 7℃. The performance of PPG-1000/TDI system with different way to add 1010 in PU was compared. Better dispersion of 1010, better performance of materials.
本文制备了聚醚型聚氨酯弹性体并进行了有机小分子的改性,通过红外光谱(FT-IR)对材料的化学结构进行讨论；通过差示扫描热分析(DSC)对材料中有机小分子的形态进行分析；通过扫描电子显微镜(SEM)对材料的形貌进行表征；通过硬度计,动态力学分析仪对材料的宏观性能进行了测试。
首先,论文研究了聚醚型聚氨酯的性能影响因素：软段分子量越大,损耗因子越小,柔顺性越好；TDI体系比IPDI体系的损耗因子高,刚性大。综合考虑确定以硫醚作为扩链剂,扩链系数选取0.8,并加入预聚体质量10%的DBP作为稀释剂制备改性基体。
其次,研究了DZ对聚醚型聚氨酯的改性作用。DZ的引入使得PU硬度下降、低温下储能模量的上升、tg和tanδ均升高。PU/DZ中DZ的有三种存在方式：(1)以氢键与PU结合；(2)在PU内部结晶；(3)在PU表面析出结晶。不同体系的改性作用对比表明：60%含量的DZ对IPDI体系的改性作用优于TDI体系；对PPG-1000体系的改性作用优于PPG-2000体系。不同DZ加入量的PPG-1000/TDI体系性能研究表明：60%含量DZ的的损耗因子峰值最大,为0.87。80%含量DZ的玻璃化转变温度最高,为3.5℃。对不同加入方式的改性研究表明：DZ的分散性越好,改性作用越强。
最后,研究了抗氧剂1010对聚醚型聚氨酯的改性作用。1010的引入使得PU硬度下降、低温下储能模量的上升、tg和tanδ均升高。PU/1010中1010有四种存在方式：(1)以化学键与PU结合；(2)以氢键与PU结合；(3)在PU内部结晶；(4)在PU表面析出结晶。不同体系的改性作用对比表明：60%质量含量的抗氧剂1010的加入对IPDI体系的改性作用更为明显,损耗因子峰值增加了一倍。不同1010加入量的PPG-1000/TDI体系性能研究表明：40%含量1010的PU/1010材料的损耗因子峰值最大为0.89。70%含量DZ的PU/DZ材料的玻璃化转变温度升至7℃。对不同加入方式的改性研究表明：1010的分散性越好,改性作用越强。
Polyurethane has been widely used as damping materials because of the specificity of its structure. Mechanical vibration energy can be transformed into heat and dissipative attenuation by the viscoelasticity of polyurethane. The pure polyurethane elastomer has low damping loss factor and narrow damping temperature domain, which need to be modified.
In this paper, polyether-polyurethane elastomer was synthesized and modified by small organic molecules. The chemical structure of materials was discussed by FT-IR spectra. The form of small organic molecules in material was analyzed by DSC. The morphology of material was characterized by SEM. And the macroeconomic performances were characterized by DMA and sclerometer.
First of all, factors that affect the performance of polyether-polyurethane were studied. Greater soft segment molecular weight makes the smaller loss factor and the better flexibility. Compared with the system of IPDI, the system of TDI has a higher loss factor. The modified matrix was synthesized with the DMTDA as chain extenders, equivalent coefficient of 1.1 and 10% of DPB, which used as diluents.
Second, modified polyether-polyurethane by DZ was studied. When put DZ-doped into the PU, the performance of material was changed:hardness decreased, storage modulus at the low temperature raised, tg and tan8 increased. There are three state of DZ in PU/DZ hybrid materials:(1) combination with PU by hydrogen; (2) as crystal in the PU internal; (3) as crystal on the surface of PU. The performance of PU/DZ in different system, which containing DZ with 60% mass fraction of prepolymer, was compared. Modification of IPDI system is superior to the modification of TDI system. Modification of PPG-2000 system is superior to the modification of PPG-1000 system. The performance of PPG-1000/TDI system with different content of DZ was compared. The PU/DZ with 60% content of DZ has the largest loss factor, which was 0.87. The PU/DZ with 80% content of DZ has the highest tg, which was 3.5℃. The performance of PPG-1000/TDI system with different way to add DZ was compared. Better dispersion of DZ, better performance of materials.
Finally, modified polyether-polyurethane by 1010 was studied. When put 1010-doped into the PU, the performance of material was changed:hardness decreased, storage modulus at the low temperature raised, tg and tanδincreased. There are four state of DZ in PU/DZ hybrid materials:(1) combination with PU by chemical bonds; (2) combination with PU by hydrogen; (3) as crystal in the PU internal; (4) as crystal on the surface of PU. The performance of PU/1010 in different system, which containing 1010 with 60% mass fraction of prepolymer, was compared. Modification of IPDI system is superior to the modification of TDI system. The Loss factor peak of IPDI system was doubled. The performance of PPG-1000/TDI system with different content of 1010 was compared. The PU/1010 with 40% content of DZ has the largest loss factor, which was 0.89. The PU/DZ with 70% content of DZ has the highest tg, which was 7℃. The performance of PPG-1000/TDI system with different way to add 1010 in PU was compared. Better dispersion of 1010, better performance of materials.
引文
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