化学镀镍废液的资源回收与处理
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摘要
本文主要采用电解法,辅以化学沉淀法来实现化学镀镍废液的镍、磷资源回收及处理。
采用电解法回收镍,通过改变工艺条件,对比直流电解和脉冲电解,以及使用不同涂层阳极,考察对镍回收率、能耗的影响。研究表明:废液pH=7、温度60℃、搅拌、电流密度8.0 mA·cm-2、使用钌钛涂层阳极电解2h, Ni2+回收率达到98.93%,能耗为5.88kWh·kg -1Ni2+。同样条件,当脉冲占空比为20%,脉冲频率为1kHz,电解2h,Ni2+回收率达到99.27%,能耗为5.00kWh·kg-1Ni2+。同样脉冲电解条件,使用铱钽涂层阳极电解2h,Ni2+回收率达到99.32%,能耗为4.46kWh·kg-1Ni2+。
使用DTCR重金属捕集剂去除经电解后废液中仍残留的镍,考察了废液pH值、DTCR投加量、絮凝剂投加量、反应温度及反应时间对残留Ni2+去除率的影响,结果表明:废液pH=9,投加1.0g·L-1 DTCR,快速搅拌15min,投加6.4mg·L-1聚丙烯酰胺,缓慢搅拌5min,静置10min,镍去除率为96.91%, Ni2+浓度为0.95mg·L-1,小于1mg·L-1,达到国家排放标准。
利用次氯酸钙回收镍含量达标的废液中的磷,考察了次氯酸钙投加量、废液pH值、温度、搅拌、反应时间等对磷回收率的影响,确定出优化条件:溶液pH=8,温度60℃,向50mL废液中投加3g次氯酸钙,连续搅拌反应4h,可使磷的回收率达到99.996%,磷浓度降至0.93mg·L-1,达到国家排放标准,含磷废渣作为磷肥回收使用。
Electrolysis and assisting chemical precipitation are applied to achieve recovering and treating nickel and phosphorus resource of spent electroless nickel plating bath.
Electrolysis was adopted to recover the nickel resource. The influences of processing conditions, the direct-current power and the pulse power, different species of DSA anode on the recovery efficiency of nickel and the power consumption were studied. Research showed that the recovery rate of nickel was reduced from 98.93%, the consumed energy was 5.88kWh·kg-1Ni2+ under the conditions of the pH 7, temperature 60℃, agitate, current density 8.0mA·cm-2, Ti/RuO2-TiO2 coating anode, electrolysis time 2h. At the same conditions, when pulse duty cycle is 20%, pulse frequency is 1kHz and pulse electrolysis time 2h using Ti/RuO2-TiO2 coating anode, he recovery rate of nickel was reduced from 99.27%, the consumed energy was 5.00kWh·kg-1Ni2+. While conditions are the same as pulse electrolysis and using Ti/IrO2-Ta2O5 coating anode, electrolysis time 2h, the recovery rate of nickel was reduced from 99.32%, the consumed energy was 4.46kWh·kg-1Ni2+.
Heavy metal chelating agent DTCR was induced to removal residual nickel in waste liquid which was treated by electrolysis. Effects of pH, amount of DTCR and flocculant, temperature and time of reactions on removal efficiency of residual nickel were studied. Results showed that under condition of pH=9, adding 1.0g·L-1 DTCR, and fast mixing 15 min, then adding 6.4mg·L-1 Polyacrylamide, and followed with slow mixied for 5 min, after standing for 10min, the removal efficiency of residual nickel had reached 96.91%, and with residual nickel concentration of 0.95mg·L-1, meeted National Discharge Standard of 1 mg·L-1.
Calcium hypochlorite was used to recover phosphorus resource in the waste liquid. The influence of dosing quantity of calcium hypochlorite, pH, temperatrure and reaction time on removal efficiency of phosphorus resource were studied. The Optimum Conditions were pH=8, 60℃, added 3g calcium hypochlorite, continuous stirring for 4h, then the recover rate of phosphorus resource can reach 99.996%, with the residual concentration of 0.93mg·L-1. The sediment can be used as Phosphate Fertilizer.
采用电解法回收镍,通过改变工艺条件,对比直流电解和脉冲电解,以及使用不同涂层阳极,考察对镍回收率、能耗的影响。研究表明:废液pH=7、温度60℃、搅拌、电流密度8.0 mA·cm-2、使用钌钛涂层阳极电解2h, Ni2+回收率达到98.93%,能耗为5.88kWh·kg -1Ni2+。同样条件,当脉冲占空比为20%,脉冲频率为1kHz,电解2h,Ni2+回收率达到99.27%,能耗为5.00kWh·kg-1Ni2+。同样脉冲电解条件,使用铱钽涂层阳极电解2h,Ni2+回收率达到99.32%,能耗为4.46kWh·kg-1Ni2+。
使用DTCR重金属捕集剂去除经电解后废液中仍残留的镍,考察了废液pH值、DTCR投加量、絮凝剂投加量、反应温度及反应时间对残留Ni2+去除率的影响,结果表明:废液pH=9,投加1.0g·L-1 DTCR,快速搅拌15min,投加6.4mg·L-1聚丙烯酰胺,缓慢搅拌5min,静置10min,镍去除率为96.91%, Ni2+浓度为0.95mg·L-1,小于1mg·L-1,达到国家排放标准。
利用次氯酸钙回收镍含量达标的废液中的磷,考察了次氯酸钙投加量、废液pH值、温度、搅拌、反应时间等对磷回收率的影响,确定出优化条件:溶液pH=8,温度60℃,向50mL废液中投加3g次氯酸钙,连续搅拌反应4h,可使磷的回收率达到99.996%,磷浓度降至0.93mg·L-1,达到国家排放标准,含磷废渣作为磷肥回收使用。
Electrolysis and assisting chemical precipitation are applied to achieve recovering and treating nickel and phosphorus resource of spent electroless nickel plating bath.
Electrolysis was adopted to recover the nickel resource. The influences of processing conditions, the direct-current power and the pulse power, different species of DSA anode on the recovery efficiency of nickel and the power consumption were studied. Research showed that the recovery rate of nickel was reduced from 98.93%, the consumed energy was 5.88kWh·kg-1Ni2+ under the conditions of the pH 7, temperature 60℃, agitate, current density 8.0mA·cm-2, Ti/RuO2-TiO2 coating anode, electrolysis time 2h. At the same conditions, when pulse duty cycle is 20%, pulse frequency is 1kHz and pulse electrolysis time 2h using Ti/RuO2-TiO2 coating anode, he recovery rate of nickel was reduced from 99.27%, the consumed energy was 5.00kWh·kg-1Ni2+. While conditions are the same as pulse electrolysis and using Ti/IrO2-Ta2O5 coating anode, electrolysis time 2h, the recovery rate of nickel was reduced from 99.32%, the consumed energy was 4.46kWh·kg-1Ni2+.
Heavy metal chelating agent DTCR was induced to removal residual nickel in waste liquid which was treated by electrolysis. Effects of pH, amount of DTCR and flocculant, temperature and time of reactions on removal efficiency of residual nickel were studied. Results showed that under condition of pH=9, adding 1.0g·L-1 DTCR, and fast mixing 15 min, then adding 6.4mg·L-1 Polyacrylamide, and followed with slow mixied for 5 min, after standing for 10min, the removal efficiency of residual nickel had reached 96.91%, and with residual nickel concentration of 0.95mg·L-1, meeted National Discharge Standard of 1 mg·L-1.
Calcium hypochlorite was used to recover phosphorus resource in the waste liquid. The influence of dosing quantity of calcium hypochlorite, pH, temperatrure and reaction time on removal efficiency of phosphorus resource were studied. The Optimum Conditions were pH=8, 60℃, added 3g calcium hypochlorite, continuous stirring for 4h, then the recover rate of phosphorus resource can reach 99.996%, with the residual concentration of 0.93mg·L-1. The sediment can be used as Phosphate Fertilizer.
引文
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[2]姜晓霞,沈伟.化学镀理论及实践[M].北京:国防工业出版社,2000.2-4,26-35,181,472-476
[3]崔国峰,李宁,黎德育.化学镀镍和镍/金在微电子领域中的应用及展望[J].电镀与环保.2003(4):7-9
[4]李异.化学镀镍在五金工具防护中的应用[J].材料保护.2002(2):57-58
[5]刘曦,高加强,胡文彬.化学镀Ni-P合金在电子工业中的应用[J].电镀与精饰.2006(1):30-34
[6]贾韦,宣天鹏.化学镀镍在微电子领域的应用及发展前景[J].稀有金属快报.2007(3):1-6
[7]智建辉,陈芳,唐雪娇等.化学镀镍在高科技领域中的应用[J].天津化工.2004(4):1-3
[8]闻洪.现代化学镀镍和复合镀新技术[M].北京:国防工业出版社,1999.2
[9]沃尔夫冈·里德尔.化学镀镍[M].上海交通大学出版社,1996.
[10]陈勇生,孙启俊,陈钧等.重金属的生物吸附技术研究[J].环境科学进展.1997,5(6):34-43
[11]孟祥和,胡国飞.重金属废水处理[M].北京:化学工业出版社,2000,5:14
[12]张笑一,潘渝生.重金属致毒的化学机理[J].环境科学研究.1997,10(2):45-49
[13]王忠玉,姚重华(译).水环境的金属污染[M].北京:海洋出版社,1987.3-55
[14]上海金属网.2009年有色金属镍现货价格走势图.EB/OL.http://www.shmet.com/tubiao/ x_ni. htm,2009.4.18
[15]张庆明.中国水利百科全书(第4卷)[M].北京:水利电力出版社,1990.12:2366
[16]李朝林,周定,唐彩虹.国外化学镀镍老化液处理现状[J].环境保护科学.1997,23(3):8-11.
[17]孙红,赵立军,杨永生.化学沉淀法处理化学镀镍废液中镍的研究[J].黑龙江大学自然科学学报.1999,26(2):102-105.
[18]王利,黄英,王艳丽等.玻璃纤维化学镀镍钴磷合金废液的处理与回用[J].工业用水与废水.2006,37(3):41-44.
[19]陈志勇,刘彦明,王辉.化学镀镍液的循环利用及废水处理研究(II)﹡——废水处理[J].信阳师范学院学报(自然科学版).1996,9(3):296-299.
[20]于秀娟,赵南霞,周力等.化学镀镍老化液中镍、磷的处理与回收[J].环境保护科学.2001,29(2):15-18.
[21] Teruyoshi Izawa ,Kasugai, et al. Recovery of Valuable Substances[P]. US patent. 5665324. 1997.
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