化工进展 ›› 2020, Vol. 39 ›› Issue (3): 1108-1114.DOI: 10.16085/j.issn.1000-6613.2019-1016

• 材料科学与技术 • 上一篇    下一篇

微米级棒状氧化铝团簇体的合成及表征

季洪海(),凌凤香(),张会成,王少军,沈智奇   

  1. 中国石化大连石油化工研究院,辽宁 大连 116045
  • 收稿日期:2019-06-27 出版日期:2020-03-05 发布日期:2020-04-03
  • 通讯作者: 凌凤香
  • 作者简介:季洪海(1982—),男,硕士研究生,高级工程师。E-mail:jhhyd@126.com

Synthesis and characterization of micron rod-like alumina clusters

Honghai JI(),Fengxiang LING(),Huicheng ZHANG,Shaojun WANG,Zhiqi SHEN   

  1. Dalian Research Institute of Petroleum and Petrochemicals, SINOPEC, Dalian 116045, Liaoning, China
  • Received:2019-06-27 Online:2020-03-05 Published:2020-04-03
  • Contact: Fengxiang LING

摘要:

以γ-Al2O3粉末及碳酸氢铵为原料,采用水热技术成功制备微米级棒状氧化铝团簇体,考察反应温度、反应时间、物料配比等因素对微米级棒状氧化铝团簇体形貌的影响,并应用XRD、NMR、TEM、FTIR、SEM、N2吸附-脱附、吡啶吸附-脱附等技术分析其物化性质及结构。结果表明:当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6h时,合成的微米级棒状氧化铝团簇体直径为5~15μm,该微米级棒状氧化铝团簇体由直径50~100nm、长0.5~3μm的棒状氧化铝交叉堆积而成,比表面积为300m2/g、孔容为0.67mL/g,具有双重孔分布,可几孔径分别为3.5nm和26nm,表面同时含有六配位铝离子、五配位铝离子和四配位铝离子。

关键词: 氧化铝, 团簇体, 合成, 表征

Abstract:

Micron rod-like alumina clusters were successfully prepared from γ-Al2O3 powder and ammonium bicarbonate by hydrothermal method. The effects of reaction temperature, reaction time and material ratio on the morphology of rod-like alumina clusters were investigated. The physicochemical properties and structures of rod-like alumina clusters were analyzed by XRD, NMR, TEM, FTIR, SEM, N2 adsorption-desorption and pyridine adsorption-desorption techniques. The results showed that the mass ratio of γ-Al2O3 powder to ammonium bicarbonate was 1∶1.75, the reaction temperature was 140℃, the reaction time was 6h and the diameter of the synthesized micron grade rod-like alumina clusters was 5—15μm. The micron-grade rod-like alumina cluster was formed by cross-stacking of rod-like alumina with a diameter of 50—100nm and a length of 0.5—3μm. The specific surface area was 300m2/g and pore volume was 0.67mL/g with dual pore distribution. The pore sizes were 3.5nm and 26nm, respectively. It also contained six coordination aluminum ions, five coordination aluminum ions and four coordination aluminum ions.

Key words: alumina, cluster, synthesis, characterization

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