高等学校化学学报 ›› 2002, Vol. 23 ›› Issue (5): 751.

• 研究论文 •    下一篇

Al13形态的分离纯化与表征

赵华章1, 栾兆坤1, 苏永渤2   

  1. 1. 中国科学院生态环境研究中心环境水化学国家重点实验室, 北京 100085;
    2. 东北大学理学院应用化学系, 沈阳 110004
  • 收稿日期:2001-07-27 出版日期:2002-05-24 发布日期:2002-05-24
  • 通讯作者: 赵华章(1974年出生),男,博士研究生,主要从事环境水化学及水处理药剂的研究.E-mail:hzzhao@263.net. E-mail:hzzhao@263.net.
  • 基金资助:

    国家自然科学基金重点项目(批准号:59838300);国家自然科学基金(批准号:50178087)资助.

Purification and Characterization of A113 Species

ZHAO Hua-Zhang1, LUAN Zhao-Kun1, SU Yong-Bo2, WANG Shu-Guang1   

  1. 1. State Key Laboratory of Environmental Aquatic Chemistry, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China;
    2. Department of Applied Chemistry, School of Science, Northeastern University. Shenyang 110004, China
  • Received:2001-07-27 Online:2002-05-24 Published:2002-05-24

摘要: 采用乙醇-丙酮沉淀法提取了聚合氰化铝(PAC)中的Al13形态并采用Al-Ferron逐时络合比色法、27AlNMR,SEM,TEM和XRD等方法对所获得的水溶性Al13形态进行了分析表征.结果表明,通过向聚合氯化铝溶液中不断加入乙醇和丙酮,聚合氯化铝中各形态组分便会按照在混合溶剂中溶解度由小到大的顺序,依次从溶液中析出.截取中间组分得到Al13形态.Al-Ferron逐时络合比色法和27AlNMR的鉴定结果表明,采用该方法分离提纯得到的样品中Al13的含量达95%以上.SEM和TEM的鉴定结果表明,固体Al13聚集体主要为棱柱、单斜长方体和四面体等多面晶粒,小的聚集体粒径约200mm,大的可达2μm.溶液中的Al13形态聚集成束并以枝状排列.XRD结果表明,Al13的特征衍射峰出现在2θ为5°~25°的范围内.

关键词: Al13形态, 分离纯化, 形态结构表征, 聚合氯化铝(PAC)

Abstract: The polynuclear Keggin species, AlC4Al12(OH)24(H2O)127+(Al13),was firstly separated and purified from polyaluminum chloride (P AC) by the precipitation method, which involved adding ethanol and acetone continuously to the PACsolution.The solid Al13 obtained with excellent dissolubility was characterized by Al-Ferron timed complexation spectrophotometry, 27A1 NMRspectroscopy, SEM, TEM and XRD.The results show that the components of PAC would be separated out in soluble sequence from low to high when ethanol and acetone were added continuously to the PACsolution, and that Al with a high purity would be obtained by taking out the middle precipitate.From Al-Ferron timed complexation spectrophotometry and 27A1 NMR spectroscopy, it was found that the sample obtained contained more than 95% of Al13.The SEM and TEM results showed that the small Al13 aggregates were about 200 nm and the big one were about 2 um in diameter.The Aln aggregates were mainly polyhedron such as prism, monoclinic rectangle and tetrahedron in solid sample and showed a branch type in solution.In the XRD spectra, the signal of Al13 appeared in the range of 2θfrom 5°to 25°

Key words: Al13 species, Separation and purification, Characterization of morphology and structure, Polyaluminum chloride (PAC) (Ed.: M, G)

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