一步法制备长碳链尼龙1012及其性能  

One-pot synthesis of long carbon-chain nylon 1012 and its properties

作　　者：黎杰 王宜迪 王兆程 程瑾 李澜鹏 潘凯[1] 曹长海 LI Jie;WANG Yidi;WANG Zhaocheng;CHENG Jin;LI Lanpeng;PAN Kai;CAO Changhai(Beijing University of Chemical Technology,School of Materials Science and Engineering,Beijing 100029,China;SINOPEC Dalian Research Institute of Petroleum and Petrochemicals Co.,Ltd.,Dalian 116045,China)

机构地区：[1]北京化工大学材料科学与工程学院,北京100029 [2]中石化(大连)石油化工研究院有限公司,辽宁大连116045

出　　处：《工程塑料应用》2024年第7期29-36,共8页Engineering Plastics Application

基　　金：中国石油化工集团公司资助项目(420044-1,222128)。

摘　　要：传统熔融缩聚法制备尼龙通常先制备尼龙盐以提高单体热稳定性、保证酸胺的物质的量比,再进行后续的聚合。而长碳链尼龙由于其单体分子量较大、热稳定性较好,因此可以省略繁琐的成盐工艺,具备一步法熔融缩聚的可能性。笔者通过一步法成功制备了长碳链尼龙1012 (PA1012),探究了预聚工艺、后聚工艺以及终聚工艺对产物性能的影响,得出了适合一步法制备PA1012的最佳聚合参数:预聚时间2.5 h,预聚温度190℃,后聚时间1 h,后聚温度240℃,终聚时间根据制品需要选择合适的时间。随后进一步探究了在190℃下预聚阶段和240℃下后聚阶段PA1012的聚合动力学参数,其反应速率常数分别为16.66 g/(mol·min)和90.01 g/(mol·min)。利用傅里叶变换红外光谱仪和核磁共振氢谱对产物结构进行了表征,结果表明成功合成了PA1012;利用差式扫描量热仪、热重分析仪分析了PA1012的热性能,结果表明PA1012具有良好的耐热性和热稳定性;对PA1012进行力学性能测试,结果表明PA1012力学性能优异。以上结果证明通过一步法合成新型长碳链PA的可行性和高效性。The preparation of nylon by traditional melt polycondensation usually first prepares nylon salt to improve the thermal stability of the monomer and ensure the molar ratio of the acid amine,and then carries out subsequent polymerization.The preparation of long carbon-chain nylon has a higher molecular weight of monomer and better thermal stability,so it has the possibility of one-pot melt polycondensation by omitting the cumbersome salt formation process.Long carbon-chain nylon 1012(PA1012)was successfully prepared by one-pot method,and the effects of pre-polymerization,post-polymerization and final polymerization on the properties of the product were investigated.The optimal polymerization parameters for one-pot preparation of PA1012 were found to be as follows:pre-polymerization temperature,pre-polymerization time,post-polymerization temperature and post-polymerization time were 190℃,2.5 h,240℃and 1 h,respectively,and the final polymerization time is selected according to the needs of the product.Subsequently,the kinetic parameters of polymerization of PA1012 in the pre-polymerization stage at 190℃and in the post-polymerization stage at 240℃were further explored,and the reaction rate constants were 16.66,90.01 g/(mol∙min),respectively.The structure of the product was characterized using infrared spectroscopy and nuclear magnetic resonance hydrogen spectroscopy,which showed that PA 1012 was successfully synthesized.The thermal properties of PA1012 were analyzed using thermal gravimetric analyzer and differential scanning calorimetry,which indicated that PA1012 had good heat resistance and thermal stability.The mechanical properties of PA1012 were tested,which revealed that PA1012 had excellent mechanical properties.The above results demonstrate the feasibility and high efficiency of synthesizing the new long carbon-chain PA by one-pot method.

关 键 词：一步法 熔融缩聚 聚合工艺 长碳链尼龙 尼龙1012 

分 类 号：TQ316.4[化学工程—高聚物工业]