基于PA10T的生物基耐高温聚酰胺的合成

Synthesis of Bio-based Heat-Resistant Polyamides Based on PA10T

采用生物基单体2,5–呋喃二甲酸(FDCA)作为第三单体,与癸二胺、对苯二甲酸(PTA)进行共聚合,合成了相对于聚对苯二甲酰癸二胺(PA10T)(55.6%)具有更高生物基含量的聚对苯二甲酰癸二胺/聚呋喃二甲酰癸二胺(PA10T/10F)共聚物(61.6%)。采用核磁共振波谱(NMR)技术表征了共聚物的结构,明确了共聚合过程中FDCA发生了脱羧反应,导致预聚物端基失衡、增黏产物黏度较低。研究了预聚合温度、排水量、固相增黏温度和氮气流速等反应条件对共聚物结构的影响,确定较优的聚合反应条件为:预聚合温度225℃、排水量70 g、增黏温度235℃以及氮气流速≥0.2 L/min。同时研究了聚合条件对共聚物颜色的影响。

Bio-based monomer 2,5-furandicarboxylic acid (FDCA) was used to be copolymerized with 1,10-diaminodecane and terephthalic acid (PTA) to prepare PA10T/10F copolymer which bio-based content was increased to 61.6% compared with PA10T (55.6%). The chain structure of PA10T/10F copolymer was characterized by nuclear magnetic resonance spectrometer (NMR) technique,and the result show that a decarboxylation reaction of FDCA occurred during the copolymerization,leading to the imbalance of the prepolymers’end groups and low viscosity of the copolyamides. The effects of the temperature and the amounts of water discharged during prepolymerization,the temperature and flow rate of N2 during solid state polymerization on the copolymers were studied,and the optimum polymerization conditions were determined as follow :225℃ and 70 g water discharged for prepolymerization,235 ℃ and the flow rate of N2 above 0.2 L/min for solid state polymerization. Moreover,the influence of polymerization conditions on the color of copolymer was also studied.