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AlCl3作为Al2O3的真空热还原-氯化-歧化反应的氯化剂,需要通过控制其升华条件以控制其进入反应体系的速率。本文研究了无水AlCl3在真空条件下的升华规律。采用研究Al2O3的真空热还原-氯化-歧化反应的三段式实验炉,在不同的温度和时间条件下进行实验。研究表明:在抽真空的条件下,温度高于室温,AlCl3开始升华。50℃后,升华速率加快。130℃后,升华速率太快。合适的升华温度为80℃左右。研究发现:AlCl3不能升华完全,残余在10%以上。残余物为粉末状、非晶物,吸水性减弱,大部分可溶解于水中,铝含量为29.14%,高于无水AlCl3的铝含量(20.24%),应当为非晶氯化铝含有聚合氯化铝和铝。
Abstract：The influence of sublimation conditions,such as the pumping speed,sublimation temperature and sublimation rate,on vacuum sublimation of anhydrous aluminum chloride was experimentally studied with the vacuum furnace used in study of carbothermic reduction chlorination disproportion of Al2O3.The results show that the sublimation temperature significantly affects the sublimation rate of the anhydrous aluminum chloride(AlCl3).For example,the sublimation of the AlCl3 starts at an elevated temperature,about 50℃,and a pressure of 1Pa.The sublimation rate increases as the temperature rises up from 50℃,However,the sublimation rate is too fast at temperature higher than 130℃.We propose that 80℃ be the optimized sublimation temperature.Interesting finding is that 10% AlCl3 was left in the residue after high temperature sublimation for a long time.The morphology of the AlCl3 in the residues was also characterized.
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基本信息:
中图分类号:TF821
引用信息:
[1]冯月斌,戴永年,刘永成,等.无水氯化铝在真空条件下的升华研究[J].真空科学与技术学报,2009,29(03):336-339.
基金信息:
973计划前期研究专项资助(No.2007CB616908);; NSF-云南联合基金(No.U0837604)
2009-05-15
2009-05-15