化工学报 ›› 2014, Vol. 65 ›› Issue (10): 3960-3967.DOI: 10.3969/j.issn.0438-1157.2014.10.029

• 分离工程 • 上一篇    下一篇

AlCl3·6H2O在盐酸体系中的结晶行为

郭彦霞, 杨喜, 崔慧霞, 程芳琴, 杨凤玲   

  1. 山西大学资源与环境工程研究所, 国家环境保护煤炭废弃物资源化高效利用技术重点实验室, 山西 太原 030006
  • 收稿日期:2014-03-07 修回日期:2014-05-27 出版日期:2014-10-05 发布日期:2014-10-05
  • 通讯作者: 程芳琴
  • 基金资助:

    国家高技术研究发展计划项目(2011AA06A103);山西省科技重大专项(20131101027)。

Crystallization behavior of AlCl3·6H2O in hydrochloric system

GUO Yanxia, YANG Xi, CUI Huixia, CHENG Fangqin, YANG Fengling   

  1. Institute of Resources and Environment Engineering, State Environmental Protection Key Laboratory of Efficient Utilization Technology of Coal Waste Resources, Shanxi University, Taiyuan 030006, Shanxi, China
  • Received:2014-03-07 Revised:2014-05-27 Online:2014-10-05 Published:2014-10-05
  • Supported by:

    supported by the National High Technology Research and Development Program of China (2011AA06A103) and the Shanxi Province Special Grand Science-Technology Project (20131101027).

摘要: 研究了AlCl3·6H2O在盐酸体系中的结晶行为,考察了铁、钙、镁、钾、钠等杂质对AlCl3·6H2O结晶行为的影响,并利用聚焦光束反射测量技术(FBRM)和颗粒录影显微镜(PVM)探讨了不同盐酸滴加速度下AlCl3·6H2O的结晶粒度分布及形貌。结果表明,AlCl3·6H2O的结晶量随着盐酸加入量的增加而增加,当浓盐酸加入量为AlCl3饱和溶液体积的2.25倍时,25℃时的结晶效率可达到80%。溶液中Fe的存在可促进AlCl3·6H2O的结晶,在1.5 mol·kg-1的AlCl3溶液中,当铝铁摩尔比低于3:1时,得到的AlCl3·6H2O晶体中铁的含量小于0.1%。钾、钙、镁、钠等杂质对AlCl3·6H2O的结晶影响不大。盐酸添加速度影响AlCl3·6H2O的形貌,快的盐酸添加速度易使晶体发生团聚,颗粒粒径小,盐酸添加速度较慢时,可得到颗粒较大、形貌好的单晶。

关键词: AlCl3·6H2O, 结晶, 盐酸, 杂质, 形貌, 粒度分布, 溶液

Abstract: AlCl3·6H2O, one of the most widely used inorganic compounds, is commonly prepared by leaching alumina from coal gangue and coal fly ash. Its quality depends strongly on the crystallization process. In this paper, the crystallization behavior of AlCl3·6H2O in hydrochloride system and the effect of impurities including Fe, Ca, Mg, K and Na on the crystallization were studied. The results showed that the crystallization efficiency of AlCl3·6H2O increased with the volume of concentrated HCl (36% by mass) added. The crystallization efficiency of AlCl3·6H2O reached 80% at 25℃ when the volume ratio of HCl to AlCl3 solution was 2.25. The presence of Fe improved the crystallization efficiency of AlCl3·6H2O slightly. The content of Fe in AlCl3·6H2O crystallized from 1.5 mol·kg-1 of AlCl3 solution was < 0.1% by mass when the molar ratio Al:Fe was less than 3:1. Little effects of K, Ca, Mg and Na on the crystallization of AlCl3·6H2O were observed. Furthermore, the effect of feeding speed of concentrated hydrochloride on the particle size distribution and morphology of AlCl3·6H2O crystallization was investigated by focused beam reflectance measurement and particle vision measurement. It is demonstrated that a fast feeding speed of hydrochloride results in the formation of agglomerated crystals with small size, while a slower feeding speed leads to the formation of dispersive single-crystals with larger sizes and improved morphologies.

Key words: AlCl3·6H2O, crystallization, hydrochloride, impurity, morphology, particle size distribution, solution

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