生物基半芳香尼龙PA5T/6T合成副反应的影响  

Effects of synthetic side reaction about bio-based semi-aromatic nylon PA5T/6T

作　　者：文联磊 蔡荣森 方开东 叶淑娴 龙健宇 李建伟 姜苏俊 王丰 丁超 曹民 WEN Lianlei;CAI Rongsen;FANG Kaidong;YE Shuxian;LONG Jianyu;LI Jianwei;JIANG Sujun;WANG Feng;DING Chao;CAO Min(Kingfa Sci.and Tech.Co.,Ltd.,Guangzhou 510663,China;Kingfa Science&Technology(Zhuhai)Ltd.,Zhuhai 519050,China;Guangdong Provincial Key Laboratory of Special Engineering Plastics Enterprise,Guangzhou 510663,China)

机构地区：[1]金发科技股份有限公司,广州510663 [2]珠海万通特种工程塑料有限公司,广东珠海519050 [3]广东省特种工程塑料企业重点实验室,广州510663

出　　处：《工程塑料应用》2024年第11期50-56,共7页Engineering Plastics Application

基　　金：广东省科技计划专项(2023B1212070027)。

摘　　要：为调控尼龙(PA)5T/6T在合成过程中戊二胺的副反应以及探究副反应对戊二胺基半芳香PA性能的影响,以戊二胺、己二胺和对苯二甲酸为原料,采用悬浮聚合和固相增黏结合的工艺,合成了生物基耐高温半芳香尼龙PA5T/6T。通过核磁共振波谱仪和傅里叶变换红外光谱仪分析了聚合物结构,证明PA5T/6T合成成功,且具有无规分布的序列结构。通过研究在预聚反应阶段去离子水的添加量对聚合反应的影响,发现当去离子水添加质量分数为12%时,能够得到低哌啶含量、合适端基含量的PA5T/6T预聚物。在经过固相增黏后,低哌啶含量的PA5T/6T更容易得到高黏度聚合物。通过采用差示扫描量热仪和热重分析仪表征了不同哌啶含量的PA5T/6T的热性能,发现尽管哌啶含量更高的树脂结晶性更优,但是热稳定性更差。进一步采用抽提实验测量了树脂中小分子含量,发现高哌啶含量的树脂具有更高的小分子含量。最后,通过分析树脂的力学性能,发现高哌啶含量的树脂具有更低的拉伸强度,弯曲强度和缺口冲击强度。此项研究能够为戊二胺基的半芳香PA的研究和开发提供一定参考。Bio-based semi-aromatic heat-resistant nylon(PA)5T/6T based on pentylenediamine,using bio-based pentane diamine,hexamethylene diamine and terephthalic acid as raw material,was synthesized through the combination with suspension polymerization and solid phase polymerization.Random polymeric structure of PA5T/6T was successfully characterized through nuclear magnetic resonance spectrometer and fourier transform infrared spectrometer.Noteworthily,PA5T/6T prepolymer with the low-content piperidine and optimal end-group content was obtained with the adjustment of deionized water at 12 wt%.After the solid phase polymerization,the high-viscosity PA5T/6T with low by-product content could be synthesized successfully.Compared to PA5T/6T with low-content piperidine,PA5T/6T with high-content piperidine show the higher crystallizability but poor thermostability through the measurement of differential scanning calorimeter and thermal gravimetric analyzer.Further,extractive experiment of PA5T/6T with different piperidine contents indicate that PA5T/6T with high-content piperidine has the more small molecules.More importantly,PA5T/6T with low-content piperidine present the more excellent mechanical property than that with high-content piperidine.The exploration of side reaction of PA5T/6T could provide some references for the research and development of semiaromatic nylon with based on pentylenediamine.

关 键 词：PA5T/6T 环化副反应 去离子水 哌啶 性能 

分 类 号：TQ323.6[化学工程—合成树脂塑料工业]