生物基耐高温PA5T/56的高效制备及表征  

Efficiently preparation and characterization of bio-based high temperature resistant PA5T/56

作　　者：雪冰峰 张烨 张斌 付鹏[2,3] 崔喆 张袁铖[2,3] 李鑫 庞新厂 赵蔚[2,3] 张晓朦 刘民英[2,3] XUE Bingfeng;ZHANG Ye;ZHANG Bin;FU Peng;CUI Zhe;ZHANG Yuancheng;LI Xin;PANG Xinchang;ZHAO Wei;ZHANG Xiaomeng;LIU Minying(Engineering Division,Huanghe University of Science and Technology,Zhengzhou 450000,China;School of Materials Science and Engineering,Zhengzhou University,Zhengzhou 450001,China;Henan Key Laboratory of Advanced Nylon Materials and Applications,Zhengzhou 450052,China)

机构地区：[1]黄河科技学院工学部,郑州450000 [2]郑州大学材料科学与工程学院,郑州450001 [3]河南省先进尼龙材料及应用重点实验室,郑州450052

出　　处：《工程塑料应用》2024年第7期22-28,69,共8页Engineering Plastics Application

基　　金：河南省重点研发专项(231111231900)。

摘　　要：目前,耐高温尼龙(PA)的生产主要采用“预聚合+固相后聚合”法,然而固相后聚合过程中存在的制备周期长、副反应多等技术难题长期得不到有效解决。笔者以生物基戊二胺(PDA)、对苯二甲酸(TPA)和己二酸(AA)为原料,通过在固相后聚合过程前期加入适量水,高效制备了生物基耐高温PA5T/56。研究了TPA与AA的物质的量比对产物熔点的影响,结果表明当其物质的量比为6∶4时,产物(P64)的熔点为309℃,可以作为耐高温工程塑料使用。考察了固相后聚合阶段用水量、反应温度、保温时间和预聚物粒径对固相后聚合产物相对黏度的影响,确定了优化工艺条件:用水量与设备的体积比为1∶300、反应温度为260℃、保温时间为6h、预聚物粒径<0.1mm。通过傅里叶变换红外光谱仪和核磁共振氢谱确认了产物的分子结构。热性能测试结果表明,P64的熔点为309℃,起始热分解温度为375℃,即样品具有很宽的温度加工区间和良好的熔融加工温度窗口。力学性能测试结果表明,P64拉伸强度为85.7 MPa、断裂伸长率15.4%、缺口冲击强度为5.56kJ/m^(2),这与商品化PA6T共聚物的性能相近,表明该样品可以部分代替PA6T共聚物使用,拓宽了应用领域。At present,the main production method of high temperature resistant nylon(PA)is"pre-polymerization+solid state polymerization"method,however,the technical problems such as long preparation cycle and many side reactions in the solid state polymerization process can not be effectively solved for a long time.Bio-based high temperature resistant PA5T/56 was efficiently prepared by adding appropriate amount of water in the early stage of solid state polymerization with pentaenediamine(PDA),terephthalic acid(TPA)and adipic acid(AA)as raw materials.The effect of the molar ratio of TPA to AA on the melting point of the product was studied.The results show that the melting point of the product(P64)is 309℃when the ratio is 6∶4,which can be used as high temperature resistant engineering plastics.The effects of water consumption,reaction temperature,holding time and particle size of prepolymer on the relative viscosity of solid state polymerization were investigated.The optimized process conditions were determined as water consumption to equipment volume ratio of 1∶300,reaction temperature of 260℃,holding time of 6 h and particle size of prepolymer<0.1 mm.The molecular structure of the product was confirmed by Fourier transform infrared spectroscopy and hydrogen nuclear magnetic resonance spectroscopy.The thermal performance test results show that the melting point of P64 is 309℃,and the initial thermal decomposition temperature is 375℃,indicating the sample has a wide temperature processing range and a good melting processing temperature window.The mechanical properties test results show that the tensile strength of P64 is 85.7 MPa,the elongation at break is 15.4%,and the notch impact strength is 5.56 kJ/m^(2),which is similar to the properties of commercial PA6T copolymer,which means that the sample can partially replace the PA6T copolymer and expand the application field.

关 键 词：耐高温尼龙 生物基尼龙5T/56 聚合工艺 预聚合+固相后聚合 结构与性能 

分 类 号：TQ322.3[化学工程—合成树脂塑料工业]