碳酸氢铵溶液中偏钒酸铵的冷却结晶

doi:10.16085/j.issn.1000-6613.2017-1092

化工进展 ›› 2018, Vol. 37 ›› Issue (03): 853-860.DOI: 10.16085/j.issn.1000-6613.2017-1092

碳酸氢铵溶液中偏钒酸铵的冷却结晶

郭雪梅^1,2,3, 王少娜², 杜浩^2,4, 冯曼^2,4, 郑诗礼², 张懿²

1 天津大学化工学院, 天津 300350;
2 中国科学院过程工程研究所绿色过程与工程重点实验室, 北京 100190;
3 精馏技术国家工程研究中心, 天津 300350;
4 中国科学院大学, 北京 100083

收稿日期:2017-06-07 修回日期:2017-08-23 出版日期:2018-03-05 发布日期:2018-03-05
通讯作者: 王少娜,副研究员,长期从事冶金物化方面的基础研究工作。
作者简介:郭雪梅(1991-),女,硕士研究生。
基金资助:
中国科学院STS计划（KFJ-SW-STS-148）及国家重点基础研究发展计划（2013CB632605）项目。

Cooling crystallization of ammonium metavanadate from ammonium bicarbonate solution

GUO Xuemei^1,2,3, WANG Shaona², DU Hao^2,4, FENG Man^2,4, ZHENG Shili², ZHANG Yi²

1 School of Chemical Engineering and Technology, Tianjin University, Tianjin 300350, China;
2 Key Laboratory of Green Process and Engineering, Institute of Process Engineering, CAS, Beijing 100190, China;
3 National Engineering Research Center of Distillation Technology, Tianjin 300350, China;
4 University of Chinese Academy of Sciences, Beijing 100083, China

Received:2017-06-07 Revised:2017-08-23 Online:2018-03-05 Published:2018-03-05

摘要/Abstract

摘要： 针对钒渣空白焙烧-铵化浸出新工艺产生的浸出液，在对NH₄HCO₃-NH₄VO₃-H₂O溶解度数据进行分析的基础上，采用冷却结晶分离方法分离溶液中偏钒酸铵。采用程序控温冷却方式考察了碳酸氢铵浓度、降温速率、搅拌速率、晶种添加量等因素对偏钒酸铵从70℃冷却结晶至40℃时结晶率、产品粒度、形貌等的影响，明确了偏钒酸铵冷却结晶规律，建立了偏钒酸铵从碳酸氢铵母液中高效结晶分离方法，获得了结晶最佳工艺条件。在碳酸氢铵浓度10g/L、降温速率0.36℃/min、搅拌速率200r/min、晶种添加量1.0%时偏钒酸铵结晶率可达94.28%，得到的偏钒酸铵晶体纯度为99.5%，产品粒度均匀，平均粒径约为152μm，晶体成规则棱柱状结构。

关键词: 偏钒酸铵, 碳酸氢铵, 结晶, 晶种

Abstract: Based on the solubility data of NH₄HCO₃-NH₄VO₃-H₂O ternary leaching solution which obtained from the vanadium slag roasting-ammonium leaching reaction,the present study established a high-efficiency crystallization and separation method of ammonium metavanadate from ammonium bicarbonate solution by programmed temperature controlling method when ammonium metavanadate solution cooling from 70℃ to 40℃. The effects of ammonium bicarbonate concentrations,cooling rate,agitation speed and seed load on crystallization rate,particle size and micro-structure of crystallized ammonium metavanadate were studied and discussed. The optimized separation condition showed that when ammonium bicarbonate concentration was 10g/L,cooling rate was 0.36℃/min,agitation speed was 200r/min and seed load was 1.0%,crystallization rate reached to 94.28% while the purity increased to 99.5%. The average particle size of the epigranular crystal was 152μm with a shape of prismatic structures.

Key words: ammonium metavanadate, ammonium bicarbonate, crystallization, seed

中图分类号:

TQ113.7

郭雪梅, 王少娜, 杜浩, 冯曼, 郑诗礼, 张懿. 碳酸氢铵溶液中偏钒酸铵的冷却结晶[J]. 化工进展, 2018, 37(03): 853-860.

GUO Xuemei, WANG Shaona, DU Hao, FENG Man, ZHENG Shili, ZHANG Yi. Cooling crystallization of ammonium metavanadate from ammonium bicarbonate solution[J]. Chemical Industry and Engineering Progress, 2018, 37(03): 853-860.

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碳酸氢铵溶液中偏钒酸铵的冷却结晶

Cooling crystallization of ammonium metavanadate from ammonium bicarbonate solution

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