掺硼金刚石薄膜电极电化学还原回收炸药生产废液中的金属钯  

Metal Palladium Recovery from Explosive Production Waste Water by Electrochemical Reduction Using Boron-doped Diamond Film Electrode

作　　者：马云 王兵[1] 熊鹰[1,2] MA Yun;WANG Bing;XIONG Ying(School of Materials and Chemistry,Southwest University of Science and Technology,Mianyang 621010,Sichuan,China;State Key Laboratory of Environment-friendly Energy Materials,Southwest University of Science and Technology,Mianyang 621010,Sichuan,China)

机构地区：[1]西南科技大学材料与化学学院,四川绵阳621010 [2]西南科技大学环境友好能源材料国家重点实验室,四川绵阳621010

出　　处：《西南科技大学学报》2025年第1期36-44,共9页Journal of Southwest University of Science and Technology

基　　金：国家自然科学基金(62374140);四川省自然科学基金创新研究群体项目(23NSFTD0044)。

摘　　要：采用Hg/Hg_(2)SO_(4)/K_(2)SO_(4)电极(MSE)为参比电极,铂丝电极为对电极,掺硼金刚石薄膜电极为工作电极的三电极体系,通过恒电压还原法回收某炸药生产过程废液中的金属钯(Pd),分析了电化学还原电压和浓硫酸引入量对金属Pd的回收效率和电化学还原过程的法拉第效率的影响。结果表明:电化学还原的法拉第效率随还原电压的增大而减小,但金属Pd的回收效率随电压的增大先减小后增大。在反应电压为-1.34 V(参比电极:MSE)时,金属Pd的回收率随浓硫酸的增加先增大再减小,其最高值达到26.78%,法拉第效率也呈先增大后减小的趋势,最高值为0.1%;当反应电压调整为-0.84 V(参比电极:MSE)时,金属Pd的回收率随着浓硫酸的增加而增大,其最高值达到17.5%,但法拉第效率先增大后降低,最大值为0.76%。扫描电子显微镜-能谱和X射线光电子能谱分析表明金属Pd颗粒沉积在电极表面。当反应电压为-0.84 V(参比电极:MSE)时,加入0.3 mL和0.5 mL浓硫酸还原所得的产物中钯的质量分数在98%以上,且Pd颗粒表层有部分钯被氧化。A three-electrode system of Hg/Hg_(2)SO_(4)/K_(2)SO_(4)electrode(MSE)as the reference electrode,platinum wire electrode as the counter electrode and boron-doped diamond film electrode as the working electrode was used to recover metal palladium(Pd)from the waste water produced by an explosive production process by constant voltage reduction method.The effects of electrochemical reduction voltage and the amount of concentrated sulfuric acid on the recovery efficiency of metal Pd and the Faraday efficiency of the electrochemical reduction process were explored.The results show that the Faraday efficiency of electrochemical reaction decreases with the increase of the reduction voltage,but the recovery efficiency of metal Pd first decreases and then increases with the increase of voltage.As the reaction voltage is-1.34 V vs.MSE,the recovery rate of palladium first rises and then falls with the increase of concentrated sulfuric acid,and its maximum value is about 26.78%.The Faraday efficiency of electrochemical reduction process also shows a trend of first increasing and then decreasing with a maximum value of 0.1%.However,when the reaction voltage decreased to-0.84 V vs.MSE,the recovery efficiency of Pd increases with the increase of concentrated sulfuric acid and its maximum value reaches to 17.5%.But the Faraday efficiency of electrochemical reduction process exhibits an increase during the initial stage and a decrease in the later reaction,with a maximum value of 0.76%.The results of scanning electron microscopy and X-ray photoelectron spectroscopy reveal that palladium particles are deposited on the electrode surface.At the reaction voltage of-0.84 V vs.MSE,the mass fraction of Pd is over 98%in the products obtained by adding 0.3 mL and 0.5 mL concentrated sulfuric acid,and some palladium on the surface is oxidized.

关 键 词：电化学还原 恒电压 炸药生产废液 Pd回收 

分 类 号：TQ174.9[化学工程—陶瓷工业]