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介孔磷钨酸铯盐的液相组装及酸性研究
引用本文:王美银,黄道丰,陈欣,周俊夫,任远航,叶林,岳斌,贺鹤勇. 介孔磷钨酸铯盐的液相组装及酸性研究[J]. 高等学校化学学报, 2021, 42(9): 2734. DOI: 10.7503/cjcu20210102
作者姓名:王美银  黄道丰  陈欣  周俊夫  任远航  叶林  岳斌  贺鹤勇
作者单位:复旦大学化学系,上海市分子催化与功能材料重点实验室,上海200438
基金项目:国家自然科学基金(22088101);国家重点研发计划项目(2017YFB0602204);中国石油化工股份有限公司研究项目(420068-2)
摘    要:以磷钨酸(H3PW12O40)和氯化铯(CsCl)为原料, 两亲型三嵌段共聚物F127为模板剂, 按不同的Cs/P比制备了一系列介孔磷钨酸铯盐(CsxH3-xPW12O40, m-CsPW). 通过X射线粉末衍射(XRD)、 场发射扫描电子显微镜(FESEM)、 场发射透射电子显微镜(FETEM)、 N2吸附-脱附测试和小角X射线散射(SAXS)等手段对所得样品进行了表征. 结果表明, 样品是由纳米微晶组装而成的晶态介孔材料. 以三甲基膦为探针分子, 通过31P魔角旋转固体核磁共振波谱(31P MAS NMR)测定了样品酸处理前后的酸密度和酸强度. 以5,7-二羟基-4-甲基香豆素的Pechmann缩合反应为模型反应, 考察了样品的酸性质与催化活性之间的关系.

关 键 词:介孔多酸盐  31P魔角旋转固体核磁共振波谱  酸性  Pechmann缩合
收稿时间:2021-02-18

Liquid Phase Assembly of Mesoporous CsxH3-xPW12O40 and Characterization of Their Acidity
WANG Meiyin,HUANG Daofeng,CHEN Xin,ZHOU Junfu,REN Yuanhang,YE Lin,YUE Bin,HE Heyong. Liquid Phase Assembly of Mesoporous CsxH3-xPW12O40 and Characterization of Their Acidity[J]. Chemical Research In Chinese Universities, 2021, 42(9): 2734. DOI: 10.7503/cjcu20210102
Authors:WANG Meiyin  HUANG Daofeng  CHEN Xin  ZHOU Junfu  REN Yuanhang  YE Lin  YUE Bin  HE Heyong
Affiliation:Department of Chemistry and Shanghai Key Laboratory of Molecular Catalysis and Innovative Materials,Fudan University,Shanghai 200438,China
Abstract:A series of mesoporous CsxH3-xPW12O40 samples(denoted as m-CsPW) has been prepared using H3PW12O40, CsCl as raw materials and amphiphilic triblock copolymer F127 as template. The sampleswere characterized by means of powder X-ray diffraction(XRD), field emission scanning electron microscopy (FESEM), field emission transmission electron microscopy(FETEM), N2 adsorption-desorption measurement and small angle X-ray scattering(SAXS) spectroscopy. The results indicate that the m-CsPW particles consis-ting of crystallographically ordered nanocrystallites are mesoporous spherical materials. Acid density and strength of the samples before and after acid treatment were characterized by 31P magic-angle spinning NMR spectroscopy(31P MAS NMR) using trimethylphosphine as probe molecule. Taking the Pechmann condensation of 5,7-dihydroxy-4-methylcoumarin as a model reaction, the relationship between the acid properties of the samples and the catalytic activity of the reaction has been investigated.
Keywords:Mesoporous polyoxometalate  31P magic-angle spinning NMR spectroscopy(31P MAS NMR)  Acidic property  Pechmann condensation  
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