石油炼制与化工 ›› 2020, Vol. 51 ›› Issue (2): 62-70.

• 基础研究 • 上一篇    下一篇

柱状碳酸铝铵团簇的合成及相变研究

季洪海,凌凤香,张会成,王少军   

  1. 中国石化大连(抚顺)石油化工研究院

  • 收稿日期:2019-07-05 修回日期:2019-10-28 出版日期:2020-02-12 发布日期:2020-02-27
  • 通讯作者: 季洪海 E-mail:jihonghai9802@163.com
  • 基金资助:
     

STUDY ON SYNTHESIS AND PHASE TRANSITION OF CYLINDRICAL ALUMINUM AMMONIUM CARBONATE CLUSTERS

    

  1.  
  • Received:2019-07-05 Revised:2019-10-28 Online:2020-02-12 Published:2020-02-27
  • Supported by:
     

摘要: 以γ-Al2O3粉末及碳酸氢铵为原料,采用水热处理技术,成功制备了柱状碳酸铝铵团簇,并以此柱状碳酸铝铵团簇为前躯体制备氧化铝。采用XRD、SEM、N2吸附-脱附、TEM等技术分析了反应温度、反应时间、物料配比等因素对柱状碳酸铝铵形貌的影响,并研究其高温相变过程及相应γ-Al2O3的结构特性。研究发现,合成柱状碳酸铝铵团簇的最佳反应条件:γ-Al2O3粉末与碳酸氢铵质量比为1:1.75,反应温度为140 ℃,反应时间为6 h。合成的柱状碳酸铝铵团簇直径为5~15 μm,该碳酸铝铵团簇由直径为50~100 nm、长为0.5~3 μm的柱状碳酸铝铵交叉堆积而成。焙烧温度为600,800,1 000,1 300 ℃时,碳酸铝铵团簇依次转变为γ,η,α相氧化铝。以柱状碳酸铝铵团簇为前躯体制备的γ-Al2O3的比表面积为300 m2/g、孔体积为0.67 mL/g,直径15 nm以上孔的体积占总孔体积的50%以上。

关键词: 碳酸铝铵, 团簇, 合成, 水热处理, 相变

Abstract: Cylindrical aluminum ammonium carbonate clusters were successfully prepared from γ-Al2O3 powder and ammonium bicarbonate by hydrothermal method. Al2O3 were also prepared from the cylindrical aluminum ammonium carbonate cluster precursor. The effects of reaction temperature, reaction time and material ratio on the morphology of cylindrical aluminum ammonium carbonate clusters and the phase transformation process and the properties of γ-Al2O3 were investigated by XRD, SEM, N2 adsorption-desorption and TEM. The results showed that the optimum reaction conditions were as following: the mass ratio of γ-Al2O3 powder to ammonium bicarbonate of 1:1.75, the reaction temperature 140 ℃, and the reaction time 6 h. The diameter of the synthesized cylindrical aluminum ammonium carbonate clusters was 5-15 μm. The cylindrical aluminum ammonium carbonate cluster was formed by cross-stacking of cylindrical aluminum ammonium carbonate with a diameter of 50-100 nm and a length of 0.5-3 μm. When the calcination temperatures were 600, 800, 1 000,1 300 ℃, aluminum ammonium carbonate clusters were successively transformed to γ,η,α aluminum. The specific surface area of the γ-Al2O3 was 300 m2/g, pore volume was 0.67 mL/g, and more than 50% of the total pore volume was over 15 nm in diameter.

Key words: aluminum ammonium carbonate, cluster, synthesis, hydrothermal treatment, phase transition

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