催化学报 ›› 2007, Vol. 28 ›› Issue (10): 890-894.

• 研究论文 • 上一篇    下一篇

超临界抗溶剂法制备纳米氧化铝颗粒

何春燕,姜浩锡,张敏华   

  1. 天津大学石油化工技术开发中心, 绿色合成与转化教育部重点实验室, 天津 300072
  • 收稿日期:2007-10-25 出版日期:2007-10-25 发布日期:2011-10-28

Preparation of Alumina Nanoparticles by Supercritical Antisolvent Process

HE Chunyan, JIANG Haoxi*, ZHANG Minhua   

  1. Key Laboratory for Green Chemical Technology of Ministry of Education, Research and Development Center for Petrochemical Technology, Tianjin University, Tianjin 300072, China
  • Received:2007-10-25 Online:2007-10-25 Published:2011-10-28

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制备了Al2O3前驱体硝酸铝纳米颗粒,考察了温度和溶液浓度等因素对制备过程的影响,并通过焙烧前驱体硝酸铝制得了纳米Al2O3球形颗粒. 采用热重-质谱、X射线衍射、透射电镜和场发射透射电镜对所制备的硝酸铝和Al2O3纳米颗粒进行了表征,并用H2程序升温还原技术初步考察了纳米Al2O3负载Ni催化剂的还原性能,发现纳米Al2O3比一般Al2O3载体对活性组分Ni具有更好的分散性能.

关键词: 超临界抗溶剂法, 二氧化碳, 纳米颗粒, 硝酸铝, 氧化铝

Abstract: The supercritical antisolvent (SAS) process is a novel technique for micronization and has a promising prospect in the production of thermosensitive explosives, polymer microspheres, medicines, superconductors, catalysts, and dyestuffs. Using carbon dioxide as the antisolvent medium and anhydrous ethanol as the solvent, nanoparticles of the aluminum nitrate precursor were prepared by the SAS process. The effects of preparation conditions including precipitation temperature and solution concentration on the SAS process were investigated. Spherical nanoparticles of alumina were prepared through calcination of the aluminum nitrate precursor. The nanoparticles were characterized by thermogravity-mass spectroscopy,X-raydiffraction, transmission electron microscopy, and field emission gun transmission electron microscopy. The reduction properties of nickel supported by SAS alumina nanoparticles were studied by temperature-programmed reduction. It is found that alumina nanoparticles show better dispersion properties for the active component nickel than the commercialγ-Al2O3sample.

Key words: supercritical antisolvent process, carbon dioxide, nanoparticle, aluminum nitrate, alumina