DOC《doi:10》

doi:10.

3969/j.issn.1007-7545.2016.05.005 皂化P204优化钒萃取工艺研究 刘红1,2,张一敏1,2,3,刘涛1,2,3,黄晶1,2,3,师启华1,3 (1.武汉科技大学 资源与环境工程学院,武汉 430081;

2.钒资源高效利用湖北省协同创新中心,武汉 430081;

3.湖北省页岩钒资源高效清洁利用工程技术研究中心,武汉 430081) 摘要:采用皂化P204有机相优化高酸多杂质含钒石煤浸出液萃取工艺.在萃原液pH=1.

4、相比1U

2、有机相皂化率80%、搅拌时间8 min的条件下,钒单级萃取率可达92.31%,较未皂化有机相提高17.16个百分点.未皂化有机相逆流萃取平衡级数为6级,皂化后缩短至4级,铁离子的萃取率由11.49%降低至6.46%.对皂化后P204提高钒萃取率的原因进行了阐述. 关键词:P204;

皂化;

萃取;

钒;

石煤 中图分类号:TF841.3 文献标志码:A 文章编号:1007-7545(2016)05-0000-00 Optimization Study on Vanadium Extraction Process by Saponified P204 LIU Hong1,2, ZHANG Yi-min1,2,3, LIU Tao1,2,3, HUANG Jing1,2,3, SHI Qi-hua1,3 (1.School of Resources and Environmental Engineering, Wuhan University of Science and Technology, Wuhan 430081, China;

2. Hubei Provincial Collaborative Innovation Center for High Efficient Utilization of Vanadium Resources, Wuhan 430081, China;

3. Hubei Provincial Engineering Technology Research Center of High Efficient Cleaning Utilization for Shale Vanadium Resource, Wuhan 430081, China) Abstract:Optimization of vanadium extraction process by saponified P204 from stone coal acid leaching solution with various impurity ions was studied. The results show that single-stage extraction rate of vanadium is 92.31% with 17.16 percent point higher than that of non-saponified under the optimum conditions including pH value of aqueous of 1.4, phase ratio of 1U2, saponification percentage of organic phase of 80%, and extraction time of

8 min. Series of counter-current extraction of vanadium drop from six of saponified to four of non-saponified. Extraction rate of iron ion drops from 11.49% to 6.46%. The reason for saponification of P204 to improve vanadium extraction rate is elaborated. Key words:P204;

saponification;

extraction;

vanadium;

stone coal 目前,石煤提钒通常采用焙烧―酸浸―萃取(离子交换)―沉钒―煅烧工艺[1-6].溶剂萃取以其适应性强、选择性高、平衡速度快等优点受到广泛应用[7].工业生产中采用的钒萃取剂主要为P204.魏昶等[8-9]研究表明,萃原液pH对P204萃取钒有较大影响.由于P204是一种酸性萃取剂,萃取过程中会交换出大量H+,导致萃取效率下降.P204经皂化后,生成了一种油包水型的微乳分散体系[10-11],不再释放出H+,使萃取效率得到大幅度提高.胡建锋[12]等用皂化P204有机相对杂质离子与钒的萃取行为进行了初步研究,表明P204萃取前须进行皂化处理,以提高萃取率;

陈兴龙[13]等以含钒石煤酸浸液为研究对象,在pH 2.1~2.

3、相比1U(1~1.5)、单级萃取7 min条件下钒铁分离效果较好,产品铁含量达到相关标准. 传统P204萃取高酸多杂质含钒溶液存在调pH过程固液分离难度大、萃取效率低、杂质离子萃取率高的问题,而有机相经过皂化后既可以在较低pH下获得较高的萃取率,又增强了对目的离子的选择性,因此本研究采用皂化P204有机相处理高酸多杂质含钒溶液,以优化P204萃取钒工艺.

1 试验原料及方法 1.1 原料制备 1.1.1 萃原液制备 试验原料取自湖北通山沸腾炉焙烧样,按液固比1.5U1(mL/g)加入20%硫酸,助浸剂氟化钙用量5%,在95 ℃下浸出6 h,固液分离得到含钒石煤酸浸液.酸浸液先用石灰乳调至一定pH,固液分离后再用亚硫酸钠还原得到萃原液. 收稿日期:2015-11-23 基金项目:国家自然科学基金资助项目(51474162,51404174);