水-乙醇溶剂热法制备聚酰亚胺及其电化学性能研究  

Preparation of Polyimide by Ethanol-Water Solvothermal Method and its Electrochemical Properties

作　　者：张春梅 韩卓 刘璐 李欣妍 张宇 范佳鑫 ZHANG Chunmei;HAN Zhuo;LIU Lu;LI Xinyan;ZHANG Yu;FAN Jiaxin(School of Chemistry and Materials Engineering,Liupanshui Normal University,Liupanshui 553004,China)

机构地区：[1]六盘水师范学院化学与材料工程学院,贵州六盘水553004

出　　处：《化工技术与开发》2024年第12期5-8,12,共5页Technology & Development of Chemical Industry

基　　金：六盘水师范学院一流专业建设项目(LPSYylbkzy-2020-09);六盘水师范学院高层次人才引进计划项目(LPSSYKYJJ201908);六盘水师范学院科学研究(培育)项目(LPSSY2023KJYBPY08);大学生创新训练计划项目(202310977083,202310977099,202310977133,202310977157)。

摘　　要：传统的聚酰亚胺制备过程,会使用有毒的有机溶剂如N-甲基吡咯烷酮(NMP)、N,N-二甲基甲酰胺(DMF)、二甲亚砜(DMSO)等。本文开发了一种较为绿色的水-乙醇溶剂热法,以1,4,5,8-萘四甲酸酐和尿素为原料,在不同体积比的水-乙醇(1∶2、1∶1、2∶1)溶液中,200℃下反应24h,制备了聚酰亚胺(PIs)电极材料,产品分别标记为P12、P11和P21。扫描电子显微镜(SEM)测试结果表明,水-乙醇的体积比为1∶2时,PI呈空心方管状结构。红外光谱分析(FTIR)结果表明,在3444cm^(-1)、1692cm^(-1)、1258cm^(-1)、623cm^(-1)等处出现了聚酰亚胺的特征峰。X射线衍射(XRD)分析结果表明,15°~28°处出现了多个衍射峰,28°处的峰最尖锐,表明PI具有较高的结晶度。以PI为工作电极,锌为对电极,恒电流充放电的测试结果表明,在浓度为1mol·L^(-1)的ZnSO_(4)电解液中,PI的最大放电比容量为304mAh·g^(-1);在0.5mol·L^(-1) Na_(2)SO_(4)+0.5mol·L^(-1) ZnSO_(4)的混合电解液中,PI的最大放电比容量为248.6mAh·g^(-1)。循环伏安测试(CV)发现,在0.44V/0.88V、0.21V/0.65V附近出现了2对氧化还原峰,表明材料具有可逆的充放电性能。The traditional polyimide preparation process usually used toxic organic solvents such as N-methyl-2-pyrrolidone(NMP),N,N-dimethylformamide(DMF)and dimethyl sulfoxide(DMSO).This article provide a greener water-ethanol solvothermal method.1,4,5,8-naphthalenetetracarboxylic dianhydride and para-urea were used as starting materials,and different volume ratios of waterethanol solution(1:2,1:1,and 2:1)were employed in a solvothermal reaction at 200℃for 24h to prepare polyimide(PIs)electrode materials.The products were labeled as P12,P11,and P21,respectively.Scanning electron microscopy(SEM)tests showed that when the volume ratio was 1:2,the PI exhibited a hollow square-tubular structure.Fourier transform infrared spectroscopy(FTIR)analysis indicated characteristic peaks of polyimide at multiple positions,included 3444 cm^(-1),1692 cm^(-1),1258 cm^(-1),and 623 cm^(-1).X-ray diffraction(XRD)analysis revealed several diffraction peaks between 15°~28°,with the sharpest peak at 28°,indicated high crystallinity of the PI.Applied PI as working electrode,zinc as counter electrode,the constant current charge-discharge tests demonstrated that the maximum specific discharge capacity reached 304mAh/g in a 1mol/L ZnSO₄electrolyte solution.In a mixed electrolyte solution of 0.5mol/L Na_(2)O_(4)+0.5mol/L ZnSO_(4),the maximum specific discharge capacity was 248.6 mAh/g.Cyclic voltammetry(CV)tests showed two pairs of redox peaks near 0.44V/0.88V and 0.21V/0.65V,indicated reversible charge-discharge properties of the material.

关 键 词：聚酰亚胺 溶剂热法 乙醇-水 电池 

分 类 号：TQ323.7[化学工程—合成树脂塑料工业]