含苯乙酯基共轭微孔聚合物的合成与表征  

Synthesis and characterization of phenethyl ester-containing conjugated microporous polymers

作　　者：崔嘉 藏雨 于洋洋 孙虹 高姗 徐亮[2] 黄孝明[2] CUI Jia;ZANG Yu;YU Yang-yang;SUN Hong;GAO Shan;XV Liang;HUANG Xiao-ming(College of Materials Science and Engineering,Qiqihar University,Heilongjiang Qiqihar 161006,China;Teaching Laboratory Equipment Research Division,Qiqihar University,Heilongjiang Qiqihar 161006,China)

机构地区：[1]齐齐哈尔大学材料科学与工程学院,黑龙江齐齐哈尔161006 [2]齐齐哈尔大学教学实验设备研究处,黑龙江齐齐哈尔161006

出　　处：《齐齐哈尔大学学报（自然科学版）》2022年第3期79-83,共5页Journal of Qiqihar University(Natural Science Edition)

基　　金：国家自然科学基金(52173202);黑龙江省省属高校基本科研业务费科研项目(135409314)。

摘　　要：成功合成了新型单体3,5-二溴苯甲酸(1-苯乙基)酯(RO),其收率高达86%。以RO和1,3,5-三[(4-乙炔基)苯基]苯为单体,采用Sonogashira偶联反应,首次成功制备了含苯乙酯基共轭微孔聚合物(CMP-E),其收率为78%。采用核磁氢谱、傅立叶变换红外光谱、全自动气体吸附分析、扫描电镜和热失重分析等测试方法对单体RO和CMP-E的化学结构进行了表征。CMP-E由微孔和中孔组成,其比表面积为52.3 m^(2)/g,孔径约为1.81 nm和5.4 nm。SEM图片显示CMP-E为直径在800 nm左右的纳米球,且具有良好的热稳定性,其外推起始分解温度T d可达270℃。CMP-E在有机溶剂中也表现出优异的稳定性,是一种性能良好的新型共轭微孔材料。In this work,a novel monomer 3,5-dibromobenzoic acid(1-phenylethyl)ester(RO)was successfully synthesized in 86%yield.The novel phenethyl ester-containing conjugated microporous polymer(CMP-E)was successful synthesized for the first time in 78%yield using RO and 1,3,5-tris[(4-ethynyl)phenyl]benzene as monomers by Sonogashira coupling polymerization.The chemical structures of the monomer RO and CMP-E were characterised by 1H-NMR,FT-IR,fully automated gas adsorption analysis,SEM and TGA.CMP-E consists of micropores and mesopores with a specific surface area of 52.3 m^(2)/g and pore sizes of approximately 1.81 nm and 5.4 nm.SEM image show that CMP-E is a nanosphere with a diameter of around 800 nm and has good thermal stability,with an extrapolation onset temperature of Td up to 270℃.CMP-E also shows excellent stability in a wide range of organic solvents,indicating that CMP-E is a new conjugated microporous material with good performance.

关 键 词：共轭微孔聚合物 SONOGASHIRA偶联反应 1-苯乙醇 

分 类 号：TB383.4[一般工业技术—材料科学与工程] TQ317[化学工程—高聚物工业]