钾系亚熔盐法钒渣多元体系分离应用基础研究
文献类型：学位论文
| 作者 | 杨娜 |
| 学位类别 | 硕士 |
| 答辩日期 | 2012-05-22 |
| 授予单位 | 中国科学院研究生院 |
| 导师 | 郑诗礼 |
| 关键词 | 钒酸钾 冷却结晶 钒产品转化 阳离子置换 |
| 其他题名 | Applied Fundamental Research on the Separation of the Multi-component Systemin Potassium-based Sub-molten Salt Method for Processing Vanadium-slag |
| 学位专业 | 化学工程 |
| 中文摘要 | 针对传统钒渣钠化焙烧提钒工艺反应温度高、钒提取率低、三废污染严重等问题，中国科学院过程工程研究所采用钾系亚熔盐介质化学场强化钒渣分解，实现了温和反应条件下钒的高效提取。本论文针对钾系亚熔盐分解钒渣产生的强碱性含钒溶液，通过对多元复杂KOH介质中不同组分相平衡数据测定和钒化合物结晶规律研究，建立了钒酸钾高效结晶分离方法，获得了分离最佳条件；通过研究不同阳离子与钒酸根作用规律，获得了多级阳离子置换实现钒产品清洁转化及碱高效循环方法，为亚熔盐钒渣提钒清洁工艺的建立提供了设计依据。论文取得的创新性成果主要如下： 1）确定了KOH介质中K3VO4高效结晶分离的方法。通过测定KOH-K2CO3-K3VO4-H2O体系及其子体系KOH-K3VO4-H2O在不同温度下的溶解度数据，基于K3VO4、K2CO3溶解度随温度及碱浓度变化规律的差异，确定了通过分步冷却结晶方法实现碳酸钾及钒酸钾的分离。 2）获得了KOH介质中钒酸钾高效结晶分离的最优工艺条件。通过系统研究钒酸钾的结晶行为随KOH介质浓度、温度、搅拌机制、诱导机制等关键工艺操作条件的影响，获得了高碱介质中钒酸钾冷却诱导结晶分离的最佳工艺条件，得到了颗粒大、纯度高的钒酸钾晶体。 3）开发了钙化沉钒实现钒酸钾中间体钾、钒分离的新方法。通过系统研究氢氧化钾浓度、氧化钙添加量、反应温度及反应时间等主要因素对钙化沉钒的影响，建立了通过阳离子置换实现钾钒高效分离的新方法，获得了可直接应用于钒铁冶炼的初级工业原料Ca10V6O25，并实现了钾的完全循环。 4）形成了钒酸钙碳酸化清洁转化生产V2O5的新方法。通过系统研究液固比、反应温度、NH4HCO3添加量及反应时间等因素对碳化效果的影响，掌握了少铵体系中钒酸钙向钒酸铵转化的调控规律，获得了碳化/铵化实现钒酸钙清洁转化的最佳工艺操作条件，实现了95%以上的钒转化率及母液的循环利用，达到了全过程无废水排放。 |
| 英文摘要 | Against disadvantages in the traditional salt roasting technology, such as high reaction temperature, low vanadium extraction efficiency, serious environmental pollution and etc., a new clean vanadium slag treatment process has been created by the Institute of Process Engineering, Chinese Academy of Sciences. Such treatment was developed using KOH sub-molten salt and enhanced with chemical field, which realizes efficient extraction of vanadium under mild reaction conditions. Based on the researches of phase equilibrium data and vanadate crystallization principle of different components in the multi-component KOH solution, this paper established a high-efficiency crystallization and separation method of potassium vanadate as well as optimizing the separation condition. Thus, according to the interaction principle between different cations and vanadate, clean conversion of vanadium product and efficient circulation of KOH was finally achieved via a multi-step cation exchange method. Innovative achievements in this paper including: 1) The method for the high-efficiency crystallization and separation of K3VO4 in the KOH solution was determined. The method of cooling crystallization step-by-step was determined to separate K2CO3 and K3VO4 by measuring the solubility of KOH-K2CO3-K3VO4-H2O and KOH-K3VO4-H2O. 2）The optimial crystallization and separation technology of K3VO4 from KOH solution was obtained. By examination the key effect of KOH concentration, temperature, stirring mechanism and introduction mechanism in the crystallization process, the optimal experimental conditions for separating K3VO4 by cooling induced crystallization was achieved and shape-controlled K3VO4 crystal of high purity was obtained. 3）A new technology was developed for the potassium and vanadium separation of K3VO4 intermediate. By examination the effect of KOH concentration, CaO addition, reaction temperature and reaction time on calcification process, cation exchange was realized to separate potassium and vanadium with high efficiency and reaction product of Ca10V6O25 was obtained, which can be used as primary industrial raw for the ferrovanadium smelting. Moreover, KOH can be completely recycled. 4）A new clean production processof V2O5 was established from calcium vanadate carbonation. By examination of liquid- solid ratio, NH4HCO3 addition, reaction temperature and reaction time, the regulation mechanism is revealed especially in the system with less-ammonium and the optimal carbonization/ammoniation conditions was obtained. The conversion of vanadium was more than 95%. The completely recycle of mother solution was realized with none waste water emission. |
| 语种 | 中文 |
| 公开日期 | 2013-09-25 |
| 源URL | [http://ir.ipe.ac.cn/handle/122111/1850]  |
| 专题 | 过程工程研究所_研究所（批量导入） |
| 推荐引用方式 GB/T 7714 | 杨娜. 钾系亚熔盐法钒渣多元体系分离应用基础研究[D]. 中国科学院研究生院. 2012. |
入库方式： OAI收割
来源：过程工程研究所
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