摘要
从含钒溶液中分离提纯钒是制备高纯钒的关键,普通萃取提纯需要消耗大量试剂,废水产生量大,且对设备耐酸性要求较高,而且离子选择性较差;而Cyanex272萃取pH值主要为2.5~4.0,对设备的耐酸度要求较低,且萃取产生的废水对环境的危害较小。本文以某企业钒渣钙化焙烧-酸浸后钒液为原料,采用Cyanex272为萃取剂、硫酸为反萃剂提纯钒,制备了V_(2)O_(5),并借助表征分析探究了Cyanex272萃取机理,得到以下主要结论。Cyanex272在酸性条件下对V(Ⅳ)具有良好的选择性,在有机相组成为Cyanex272∶TBP∶磺化煤油=4∶0.5∶5.5、溶液pH=3.0、萃取时间10 min、萃取温度30℃、相比O/A=1∶1的条件下,单级萃取的钒萃取率为78.06%,三级萃取的钒萃取率达到98.80%;在反萃剂硫酸浓度3.0 mol/L、反萃时间6 min、反萃取温度30℃、反萃相比O/A=1∶1的条件下,单级反萃的钒反萃取率为80.70%,三级反萃取的钒反萃取率达到98.38%,煅烧后的V_(2)O_(5)的纯度达到99.36%;钒液中经过亚硫酸钠还原的钒主要以VO^(2+)形式存在,Cyanex272的磷酸基团通过断裂P—O—H键与VO^(2+)发生螯合反应形成稳定金属配合物,从而实现对钒离子的分离萃取。
The separation and purification of vanadium from vanadium-containing solutions is the key to preparing high-purity vanadium.Conventional extraction and purification require a large amount of reagents,generate a large amount of wastewater,have high requirements for the acid resistance of equipment,and have poor ion selectivity.The pH value of Cyanex272 extraction is mainly between 2.5 and 4.0,which has a relatively low requirement for the acid resistance of the equipment.Moreover,the wastewater generated during extraction causes less harm to the environment.In this paper,the vanadium solution after calcification roasting and acid leaching of vanadium slag from a certain enterprise was used as the raw material.Cyanex272 was used as the extractant and sulfuric acid as the stripping agent to purify vanadium and prepare V_(2)O_(5).The extraction mechanism of Cyanex272 was explored through characterization analysis,and the following main conclusions were obtained.Cyanex272 exhibits excellent selectivity for V(Ⅳ)under acidic conditions.Under the conditions of organic phase composition of Cyanex272∶TBP∶sulfonated kerosene=4∶0.5∶5.5,solution pH=3.0,extraction time 10 min,extraction temperature 30℃,and O/A ratio of 1∶1,The vanadium extraction rate of single-stage extraction was 78.06%,and that of three-stage extraction reached 98.80%.Under the conditions of A sulfuric acid concentration of 3.0 mol/L as the stripping agent,a stripping time of 6 min,a stripping temperature of 30℃,and a stripping ratio of O/A=1∶1,the vanadium stripping rate of single-stage stripping was 80.70%,that of three-stage stripping reached 98.38%,and the purity of V_(2)O_(5)after calcination was 99.36%.The vanadium reduced by sodium sulfite in the vanadium solution mainly exists in the form of VO^(2+).The phosphate group of Cyanex272 undergoes chelation reaction with VO^(2+)by breaking the P-O-H bond to form a stable metal complex,thereby achieving the separation and extraction of vanadium ions.
作者
杨志
李京伟
林银河
王大龙
张林
YANG Zhi;LI Jingwei;LIN Yinhe;WANG Dalong;ZHANG Lin(School of Materials Science and Technology,Hefei University of Technology,Hefei 230009,China;School of Chemistry Engineering,Yangtze Normal University,Chongqing 408000,China;Pangang Group Xichang Vanadium Production Co.,Ltd.,Xichang 615000,China)
出处
《中国有色冶金》
北大核心
2025年第4期51-59,共9页
China Nonferrous Metallurgy
基金
国家自然科学基金项目(51874272)
凉山州重点研发计划(23ZDYF0173,23ZDYF0156)
西昌市科技项目(JSYJ-2023-16)。
作者简介
第一作者:杨志(2000-),男,安徽淮北人,主要从事钒冶金工艺研究;通信作者:李京伟(1985-),男,研究员,主要从事钒钛资源选冶及综合利用。
