超临界抗溶剂法纳米Al2O3-ZrO2颗粒的制备与表征

doi:10.3724/SP.J.1077.2010.01065

无机材料学报 ›› 2010, Vol. 25 ›› Issue (10): 1065-1070.DOI: 10.3724/SP.J.1077.2010.01065 CSTR: 32189.14.SP.J.1077.2010.01065

超临界抗溶剂法纳米Al₂O₃-ZrO₂颗粒的制备与表征

姜浩锡^1,2,3,4, 何春燕^1,2, 孙焕花^1,2, 李桂明^1,2, 张敏华^1,2

(天津大学 1. 石油化工技术开发中心; 2. 绿色合成与转化教育部重点实验室; 3. 化学工程与技术博士后科研流动站, 天津 300072; 4. 山东海化集团博士后科研工作站, 潍坊 262737)

收稿日期:2010-01-11 修回日期:2010-04-20 出版日期:2010-10-20 网络出版日期:2010-09-26
基金资助:
国家自然科学基金(20976120); 天津市应用基础及前沿技术研究计划(09JCYBJC06200)

Preparation and Characterization of Composed Alumina-zirconia Nanoparticles by Supercritical Anti-solvent Process

JIANG Hao-Xi^1,2,3,4, HE Chun-Yan^1,2, SUN Huan-Hua^1,2, Li Gui-Ming^1,2, ZHANG Min-Hua^1,2

(1. Research and Development Center for Petrochemical Technology, Tianjin University, Tianjin 300072, China; 2. Key Laboratory for Green Chemical Technology of Ministry of Education, Tianjin University, Tianjin 300072, China; 3. Post-doctoral Station for Science and Technology of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China; 4. Post-doctoral Workstation for Science and Technology of Shandong Haihua Group, Weifang 262737, China)

Received:2010-01-11 Revised:2010-04-20 Published:2010-10-20 Online:2010-09-26
Supported by:
National Nature Science of China (20976120); Tianjin Research Program of Application Foundation and Advanced Technology (09JCYBJC06200)

摘要/Abstract

摘要： 以CO₂为抗溶剂介质, 无水乙醇为溶剂, 采用超临界抗溶剂法(SAS)制备了纳米Al₂O₃-ZrO₂复合氧化物颗粒的前驱体—纳米Al(NO₃)₃-Zr(NO₃)₄颗粒, 系统考察了温度和压力等因素对制备过程的影响, 并对前驱体中Al、Zr组分的共抗溶剂效应进行了研究, 通过焙烧前驱体Al(NO₃)₃-Zr(NO₃)₄制得了纳米Al₂O₃-ZrO₂球形颗粒. 采用热重质谱(TG-MS)、X射线衍射(XRD)、X射线光电子能谱(XPS)、场发射透射电镜(FEG-TEM)和程序升温还原(TPR)等技术对所制备的前驱体Al(NO₃)₃-Zr(NO₃)₄和Al₂O₃-ZrO₂纳米颗粒的物化性能进行了表征, 初步考察了Al₂O₃-ZrO₂纳米颗粒负载Ni催化剂的还原性能. 研究发现, 该纳米复合氧化物比用浸渍?沉淀法制得的Al₂O₃-ZrO₂载体对活性组分Ni具有更好的分散性能, 作为新型催化剂载体材料有良好的应用前景.

关键词: 超临界抗溶剂法, 二氧化碳, 纳米颗粒, Al₂O₃-ZrO₂复合氧化物

Abstract: The nanoparticles of Al(NO₃)₃-Zr(NO₃)₄as the precursor of nano Al₂O₃-ZrO₂ particulates were prepared by means of supercritical fluid antisolvents (SAS) process using CO₂as antisolvents and absolutely ethanol as solvent. The effects of temperature and pressure on the preparation process and the co-antisolvent effect of Al and Zr components in the precursor were investigated. The spherical Al₂O₃-ZrO₂nanoparticles were obtained via the calcination of Al(NO₃)₃-Zr(NO₃)₄. The nanoparticles and precursor were characterized by TG-MS, XRD, XPS, FEG-TEM and TPR. In addition, the reducing property of Al₂O₃-ZrO₂nanoparticles supported Ni was examined. Compared with the catalyst support prepared from conventional impregnation-precipitation method, Ni could be dispersed better on the Al₂O₃-ZrO₂ nanoparticles prepared from SAS. It suggests that the nano-particulates prepared from SAS can be a promising candidate for catalyst support.

Key words: supercritical anti-solvent process (SAS), carbon dioxide, nanoparticles, alumina-zirconia composed oxide

中图分类号:

O643

姜浩锡, 何春燕, 孙焕花, 李桂明, 张敏华. 超临界抗溶剂法纳米Al₂O₃-ZrO₂颗粒的制备与表征[J]. 无机材料学报, 2010, 25(10): 1065-1070.

JIANG Hao-Xi, HE Chun-Yan, SUN Huan-Hua, Li Gui-Ming, ZHANG Min-Hua. Preparation and Characterization of Composed Alumina-zirconia Nanoparticles by Supercritical Anti-solvent Process[J]. Journal of Inorganic Materials, 2010, 25(10): 1065-1070.

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超临界抗溶剂法纳米Al₂O₃-ZrO₂颗粒的制备与表征

Preparation and Characterization of Composed Alumina-zirconia Nanoparticles by Supercritical Anti-solvent Process

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