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SO42-/ZrO2/Fe3O4/TiO2磁性固体酸催化剂的制备与性能

Preparation and Properties of Nano Magnetic Solid Acid Catalyst SO42-/ZrO2/Fe3O4/TiO2

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【作者】 李占双范美青刘岩峰张艳王君刘琦

【Author】 Li Zhanshuang~1,Fan Meiqing~2,Liu Yanfeng~1,Zhang Yan~1,Wang Jun~1,Liu Qi~1 (1.School of Material Science and Chemical Engineering,Harbin Engineering University,Harbin Heilongjiang 150001,China; 2.College of Chemical Engineering,Jilin Technology Institute of Industry,Jilin Jilin 132011,China)

【机构】 哈尔滨工程大学材料科学与化学工程学院吉林工业职业技术学院化工系

【摘要】 采用化学共沉淀法制备了SO42-/ZrO2/Fe3O4/TiO2磁性固体酸,利用X射线衍射、示差扫描量热、M(o|¨)ssbauer谱、透射电子显微镜、NH3-程序升温脱附、N2吸附-脱附、磁滞回线等手段对磁性固体酸的结构与性质进行了表征。表征结果显示,磁性基质Fe3O4及TiO2的引入有利于四方晶相ZrO2(t)的稳定;ZrO2晶体生长取向于ZrO2(t)的(101)方向,(101)晶面间距为0.293 nm;M(o|¨)ssbauer谱中双峰的存在表明磁性基质Fe3O4的存在;在室温下磁性固体酸具有超顺磁性。以乙酸乙酯的合成为探针反应,考察了SO42-/ZrO2/Fe3O4/TiO2磁性固体酸催化剂的催化性能,实验结果表明,外加磁场使酯化反应的醋酸转化率提高到92%。

【Abstract】 Nano magnetic solid acids SO42-/ZrO2/Fe3O4/TiO2 were prepared by co-precipitation. Obtained samples were characterized by XRD,DSC,M(o|¨)ssbauer,TEM,NH3-TPD,N2 adsorptiondesorption and magnetic hysteresis loop.The introduction of TiO2 and magnetic substrate Fe3O4 were beneficial to keep tetragonal crystalline structure of ZrO2 from transferring to monoclinic form in calcination, ZrO2 crystals grew along the direction of(101) crystal plane.The interplanar distance of ZrO2(t)(101) plane were 0.293 nm.M(o|¨)ssbauer results revealed the existence of magnetic substrate Fe3O4 particles. Magnetic measurement showed superparamagnetism of solid acid catalyst at ambient temperature.Taking synthesis of ethyl acetate as probe reaction for evaluating the activity of nano magnetic solid acid SO42-/ZrO2/Fe3O4/TiO2 catalyst,the conversion of acetic acid in the esterification mounted to 92%in external magnetic field and aggregation of nano magnetic solid acid catalyst was avoided.

【基金】 黑龙江省科技攻关资助项目(TB06A05);哈尔滨市科学研究基金项目(2008RFQXG028);哈尔滨工程大学基础研究基金项目(HEUF04072)
  • 【文献出处】 石油化工 ,Petrochemical Technology , 编辑部邮箱 ,2009年11期
  • 【分类号】O643.36
  • 【被引频次】17
  • 【下载频次】514
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