手性共价有机骨架掺杂有机聚合物毛细管整体柱的制备及表征  

Preparation and Characterization of Chiral Covalent Organic Framework Doped Organic Polymer Capillary Monolithic Column

作　　者：黄钰鑫 罗晶 郑美玲 黄露[1,2,3] HUANG Yu-xin;LUO Jing;ZHENG Mei-ling;HUANG Lu(College of Materials and Chemical Engineering,Minjiang University,Fujian Fuzhou 350108;Fujian Provincial University Engineering Research Center of Green Materialsand Chemical Engineering,Fujian Fuzhou 350108;Fujian Key Laboratory of Functional Marine Sensing Materials,Fujian Fuzhou 350108,China)

机构地区：[1]闽江学院材料与化工学院,福建福州350108 [2]绿色材料与化工福建省高校工程研究中心,福建福州350108 [3]福建省海洋传感功能材料重点实验室,福建福州350108

出　　处：《广州化工》2023年第12期80-82,99,共4页GuangZhou Chemical Industry

基　　金：福建省自然科学基金(2021J011018);福州市科技项目(2021SG042);闽江学院校长基金项目。

摘　　要：采用1,3,5-三甲酰间苯三酚和二乙酰-L-酒石酸酐在无水四氢呋喃反应生成手性有机单体CTp,继而与对苯二胺在无水乙醇和无水四氢呋喃的条件下反应,生成手性共价有机骨架CTpPa-1。以制得的CTpPa-1为手性功能单体,十二烷醇和环己醇为二元制孔剂,甲基丙烯酸缩水甘油酯为非手性功能单体,2,2-偶氮二异丁腈为引发剂,乙二醇二甲基丙烯酸酯作为交联剂在内径75μm的毛细管中进行缩合反应,最终制备出手性CTpPa-1毛细管整体柱。通过X射线衍射、红外光谱对CTpPa-1进行了表征、通过红外光谱、扫描电子显微镜对手性CTpPa-1毛细管整体柱进行了表征,探究了整体柱固定相的组成、形貌。实验结果表明,手性CTpPa-1毛细管整体柱可以承受高压,不会在流动相作用下坍塌,具有较好的通透性。1,3,5-triformylm-resorcinol and diacetyl-L-tartaric anhydride were reacted in anhydrous tetrahydrofuran to produce chiral organic monomer CTp,which was then reacted with p-phenylenediamine in anhydrous ethanol and anhydrous tetrahydrofuran to produce the chiral covalent organic framework CTpPa-1.The prepared CTpPa-1 was used as the chiral functional monomer,dodecanol and cyclohexanol as the binary pore-forming agent,glycidyl methacrylate as the ahiral functional monomer,2,2-azodiisobutyronitrile as the initiator,and ethylene glycol dimethacrylate as the cross-linking agent for condensation reaction in a capillary of 75μm inner diameter.Finally,a chiral CTpPa-1 capillary monolithic column was prepared.CTpPa-1 was characterized by X-ray diffraction and infrared spectroscopy,and the chiral CTpPa-1 capillary monolithic column was characterized by infrared spectroscopy and scanning electron microscopy.The composition and morphology of the stationary phase of the monolithic column were investigated.The experimental results showed that the chiral CTpPa-1 capillary monolithic column could withstand high pressure without collapsing under the action of mobile phase,and has good permeability.

关 键 词：毛细管色谱柱 手性整体柱 手性共价有机骨架 CTpPa-1 

分 类 号：O652[理学—分析化学]