摘要
针对失活硫酸催化剂直接酸浸、碱浸工艺选择性差,后续分离代价高、介质难回用的问题,使用两步法选择性提钒新工艺,利用钾、硫的强水溶性特点,研究了水洗温度、pH值对钾、硫浸出的影响,发现在温度40~60℃、pH值3~5水洗条件下,钾、硫的浸出率分别达到80%、96%以上,而钒的损失率控制在10%以内,实现了钒与钾、硫的选择性分离;第二步利用钒、硅在碱介质中的溶出特性,研究了碱浸温度、时间、液固比及碱液浓度对提钒效果的影响,发现采用5%NaOH溶液在80℃、L/S=5条件下反应30 min可实现失活硫酸催化剂中钒95%以上的浸出,而硅基本不浸出,实现了钒、硅的选择性分离。含钒浸出液可经钙化-铵化工艺制备得到偏钒酸铵产品,NaOH介质返回提钒阶段循环使用,介质封闭。
Based on the limited selectivity exhibited by current direct acid leaching and alkaline leaching processes for deactivated sulfuric acid catalysts,resulting in costly subsequent separation and challenging medium reuse,a new two-step process for selective extraction of vanadium was adopted.Using the strong water solubility of potassium and sulfur,the influence of washing temperature and pH value on leaching of potassium and sulfur was studied.It was found that potassium and sulfur can be removed more than 80%and 96%respectively by water washing under the condition of temperature 40~60℃and pH 3~5,while the loss rate of vanadium was controlled within 10%.Thus,the selective separation of vanadium from potassium and sulfur was realized.In the second step,based on the leaching characteristics of vanadium and silicon in an alkali medium,the effects of leaching temperature,time,liquid-solid ratio and alkali concentration on vanadium extraction were studied.It was found that after reaction with 5%NaOH solution at 80℃and L/S=5 for 30 min,more than 95%vanadium was deactivated from the sulfuric acid catalyst,while the silicon leaching rate kept almost zero.The vanadium-containing leaching solution can be handled by calcification and ammonium process to obtain ammonium metavanadate products.The NaOH solution can be recycled to vanadium extraction step and wastewater zero emission was achieved.
作者
贾美丽
杜浩
张懿
王少娜
李兰杰
祁健
周冰晶
赵备备
Jia Meili;Du Hao;Zhang Yi;Wang Shaona;Li Lanjie;Qi Jian;Zhou Bingjing;Zhao Beibei(School of Metallurgy,Northeastern University,Shenyang 110004,Liaoning,China;Institute of Process Engineering,Chinese Academy of Sciences,National Engineering Research Center of Green Recycling for Strategic Metal Resources,Beijing 100190,China;Hebei He Steel Material Technology Research Institute Co.,Ltd.,Chengde 067102,Hebei,China;Chengde Vanadium Titanium New Material Co.,Ltd.,Chengde 067102,Hebei,China)
出处
《钢铁钒钛》
CAS
北大核心
2024年第5期9-16,共8页
Iron Steel Vanadium Titanium
基金
河北省科技重大专项项目(23293801Z)。
关键词
失活硫酸催化剂
提钒
碱浸
偏钒酸铵
deactivated sulfuric acid catalyst
extraction of vanadium
alkaline leaching
ammonium metavanadate