盐酸溶液中双氧水浸出黄铜矿（英文）
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摘要
本文旨在研究以双氧水为强氧化剂的黄铜矿精矿的盐酸浸出过程。研究搅拌速度、固液比、温度、HCl和H_2O_2浓度等浸出参数对金属浸出率的影响。室温下,用3.0 mol/L H_2O_2和0.5 mol/L HCl溶液与黄铜矿反应180 min后,获得33%的最大铜浸出率。结果表明,在反应的前60 min,铜的浸出率增大;此后,由于双氧水的快速催化分解,铜浸出率基本上保持不变。此外,固液比对铜的浸出率影响显著,而且在最稀的悬浮液中(即固液比1:100)铜的浸出率最高。溶出过程可用一级动力学方程描述,表观活化能为19.6 kJ/mol,表明溶出过程受扩散控制,对于HCl和H_2O_2的反应级数分别为0.30和0.53。浸出渣的XRD和SEM/EDS分析结果表明,矿物表面生成单质硫,抑制浸出率的提高。
The aim of this work was to investigate the leaching of chalcopyrite concentrate in hydrochloric acid with hydrogen peroxide as a strong oxidizing agent. The effects of the leaching variables on metal extraction, such as stirring speed, solid-to-liquid ratio, temperature and HCl and H_2O_2 concentrations, were studied. The maximum final copper extraction of 33% was attained with 3.0 mol/L H_2O_2 in 0.5 mol/L HCl at room temperature after 180 min of the reaction. The results showed that the copper extraction was increased in the first 60 min of reaction, after which it essentially ceased due to the fast catalytic decomposition of hydrogen peroxide. Further, solid-to-liquid ratio affected the copper extraction significantly and the highest copper extraction was obtained in the most dilute suspension(i.e., S/L ratio of 1:100). The dissolution process was described by the first order kinetics equation. The apparent activation energy of 19.6 k J/mol suggested that the dissolution process was under diffusion control. The reaction orders for HCl and H_2O_2 were established to be 0.30 and 0.53, respectively. The results of the XRD and SEM/EDS analysis of the leaching residue indicated the generation of the elemental sulphur on mineral surfaces which tended to inhibit the leaching rate.
The aim of this work was to investigate the leaching of chalcopyrite concentrate in hydrochloric acid with hydrogen peroxide as a strong oxidizing agent. The effects of the leaching variables on metal extraction, such as stirring speed, solid-to-liquid ratio, temperature and HCl and H_2O_2 concentrations, were studied. The maximum final copper extraction of 33% was attained with 3.0 mol/L H_2O_2 in 0.5 mol/L HCl at room temperature after 180 min of the reaction. The results showed that the copper extraction was increased in the first 60 min of reaction, after which it essentially ceased due to the fast catalytic decomposition of hydrogen peroxide. Further, solid-to-liquid ratio affected the copper extraction significantly and the highest copper extraction was obtained in the most dilute suspension(i.e., S/L ratio of 1:100). The dissolution process was described by the first order kinetics equation. The apparent activation energy of 19.6 k J/mol suggested that the dissolution process was under diffusion control. The reaction orders for HCl and H_2O_2 were established to be 0.30 and 0.53, respectively. The results of the XRD and SEM/EDS analysis of the leaching residue indicated the generation of the elemental sulphur on mineral surfaces which tended to inhibit the leaching rate.
引文
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[24]TURAN M D,ALTUNDOGAN H S.Leaching of chalcopyrite concentrate with hydrogen peroxide and sulphuric acid in an autoclave system[J].Metallurgical and Materials Transactions B,2013,44:809-819.
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[27]UCAR G,BOYRAZLI M,AYDOGAN S.Dissolution of fine particle chalcopyrite concentrate in acidic potassium dichromate solution[C]//Proceedings of 7th International Scientific Conference of Modern Management of Mine Producing,Geology and Environmental Protection.Albena:SGEM,2007:44-51.
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[30]KERTALLI E,van RIJNSOEVER L S,PAUNOVIC V,NEIRA D'ANGELO M F,SCHOUTEN J C,NIJHUIS T A.Propylene epoxidation with hydrogen peroxide in acidic conditions[J].Chemical Engineering Science,2016,156:36-43.
[31]HE Mei-feng,WANG Hao,JIANG Hong,ZHAO Su,PAN Deng.Effect of hydrogen peroxide concentration on surface properties of Ni-Cr alloys[J].Transactions of Nonferrous Metals Society of China,2016,26:1353-1358.
[32]LI Qian,RAO Xue-fei,XU Bin,YANG Yong-bin,LIU Ting,JIANG Tao,HU Long.Extraction of manganese and zinc from their compound ore by reductive acid leaching[J].Transactions of Nonferrous Metals Society of China,2017,27:1172-1179.
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[35]ADEBAYO A O,IPINMOROTI K O,AJAYI O O.Dissolution kinetics of chalcopyrite with hydrogen peroxide in sulphuric acid medium[J].Chemical and Biochemical Engineering Quarterly,2003,17:213-218.
[36]MAHAJAN V,MISRA M,ZHONG K,FUERSTENAU M C.Enhanced leaching of copper from chalcopyrite in hydrogen peroxide–glycol system[J].Minerals Engineering,2007,20:670-674.
[37]TURAN D,SARI Z A,MILLER J D.Leaching of blended copper slag in microwave oven[J].Transactions of Nonferrous Metals Society of China,2017,27:1404-1410.
[38]SOLIS-MARCíAL O J,LAPIDUS G T.Improvement of chalcopyrite dissolution in acid media using polar organic solvents[J].Hydrometallurgy,2013,131-132:120-126.
[39]RUIZ-SáNCHEZ A,LAPIDUS G T.Study of chalcopyrite leaching from a copper concentrate with hydrogen peroxide in aqueous ethylene glycol media[J].Hydrometallurgy,2017,169:192-200.
[40]VAZARLIS H G.Hydrochloric acid-hydrogen peroxide leaching and metal recovery from a Greek zinc-lead bulk sulphide concentrate[J].Hydrometallurgy,1987,19:243-251.
[41]BABA A A,ADEKOLA F A.Comparative analysis of the dissolution kinetics of galena in binary solutions of HCl/Fe Cl3 and HCl/H2O2[J].International Journal of Minerals,Metallurgy and Materials,2011,18:9-17.
[42]HE Gui-xiang,ZHAO Zhong-wei,WANG Xiao-bo,LI Jiang-tao,CHEN Xing-yu,HE Li-hua,LIU Xu-heng.Leaching kinetics of scheelite in hydrochloric acid solution containing hydrogen peroxide as complexing agent[J].Hydrometallurgy,2014,144-145:140-147.
[43]DIMITRIJEVI?M,ANTONIJEVI?M M,JANKOVI?Z.Kinetics of pyrite dissolution by hydrogen peroxide in perchloric acid[J].Hydrometallurgy,1996,42:377-386.
[44]ANTONIJEVI?M,DIMITRIJEVI?D,JANKOVI?Z.Leaching of pyrite with hydrogen peroxide in sulphuric acid[J].Hydrometallurgy,1997,46:71-83.
[45]AYDOGAN S.Dissolution kinetics of sphalerite with hydrogen peroxide in sulphuric acid medium[J].Chemical Engineering Journal,2006,123:65-70.
[46]SHU Chi-Min,YANG Yuh-Joang.Using VSP2 to separate catalytic and self-decomposition reactions for hydrogen peroxide in the presence of hydrochloric acid[J].Thermochimica Acta,2002,392-393:259-269.
[47]VOLL F A P,PALU P,SANTOS J B O.Influence of catalyst treatments on the decomposition of hydrogen peroxide on supported palladium catalysts[J].Latin American Applied Research,2011,41:305-310.
[48]EARY L E.Catalytic decomposition of hydrogen peroxide by ferric ion in dilute sulfuric acid solutions[J].Metallurgical Transactions B,1985,16:181-186.
[49]CARRILLO-PEDROZA F R,DAVALOS-SANCHEZ A,SORIAAGUILAR M,PECINA-TREVINO E T.Coal desulfurization in oxidative acid media using hydrogen peroxide and ozone:A kinetic and statistical approach[J].Energy&Fuel,2009,23:3703-3710.
[50]CHIRITA P.Hydrogen peroxide decomposition by pyrite in the presence of Fe(III)-ligands[J].Chemical and Biochemical Engineering Quarterly,2009,23:259-265.
[51]ETO I,AKIYOSHI M,MIYAKE A,OGAWE T,MATSUNAGA T.Hazard evaluation of runaway reaction of hydrogen peroxide–Influence of contamination of various ions[J].Journal of Loss Prevention in the Process Industries,2009,22:15-20.
[52]LU Z Y,JEFFREY M I,LAWSON F.An electrochemical study of the effect of chloride ions on the dissolution of chalcopyrite in acidic solutions[J].Hydrometallurgy,2000,56:145-155.
[53]HABASHI F,TOOR T.Aqueous oxidation of chalcopyrite in hydrochloric acid[J].Metallurgical Transactions B,1979,10:49-56.
[54]LI Y,KAWASHIMA N,LI J,CHANDRA A,GERSON A.A review of the structure,and fundamental mechanisms and kinetics of the leaching of chalcopyrite[J].Advances in Colloid and Interface Science,2013,197:1-32.
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[2]ZHAO Hong-bo,HU Ming-hao,LI Yi-ni,ZHU Shan,QIN Wen-qing,QIU Guan-zhou,WANG Jun.Comparison of electrochemical dissolution of chalcopyrite and bornite in acid culture medium[J].Transactions of Nonferrous Metals Society of China,2015,25:303-313.
[3]DENG J,WEN S,YIN Q,WU D,SUN Q.Leaching of malachite using 5-sulfosalicylic acid[J].Journal of the Taiwan Institute of Chemical Engineers,2017,71:20-27.
[4]BOGDANOVI?G D,STANKOVI?V D,TRUMI?M S,ANTI?D V,TRUMI?M?.Leaching of low-grade copper ores:A case study for“Kraku Bugaresku-Cementacija”Deposits(Eastern Serbia)[J].Journal of Mining and Metallurgy A,2016,52:45-56.
[5]WANG S.Copper leaching from chalcopyrite concentrates[J].JOM,2005,57:48-51.
[6]DREISINGER D.Copper leaching from primary sulfides:Options for biological and chemical extraction of copper[J].Hydrometallurgy,2006,83:10-20.
[7]QIU Ting-sheng,NIE Guang-hua,WANG Jun-feng,CUI Li-feng.Kinetic process of oxidative leaching of chalcopyrite under low oxygen pressure and low temperature[J].Transactions of Nonferrous Metals Society of China,2007,17:418-422.
[8]PAN Hao-dan,YANG Hong-ying,TONG Lin-lin,ZHONG Cong-bin,ZHAO Yu-shan.Control method of chalcopyrite passivation in bioleaching[J].Transactions of Nonferrous Metals Society of China,2012,22:2255-2260.
[9]DUTRIZAC J E.Elemental sulphur formation during the ferric chloride leaching of chalcopyrite[J].Hydrometallurgy,1990,23:153-176.
[10]HARMER S,THOMAS J E,FORNASIERO D,GERSON A R.The evolution of surface layers formed during chalcopyrite leaching[J].Geochimica et Cosmochimica Acta,2006,70:4392-4402.
[11]LI J,KAWASHIMA N,KAPLUN K,ABSOLON V J,GERSON A R.Chalcopyrite leaching:The rate controlling factors[J].Geochimica et Cosmochimica Acta,2010,74:2881-2893.
[12]LU J,DREISINGER D.Copper leaching from chalcopyrite concentrate in Cu(II)/Fe(III)chloride system[J].Minerals Engineering,2013,45:185-190.
[13]LUNDSTROM M,LIIPO J,TASKINEN P,AROMAA J.Copper precipitation during leaching of various copper sulfide concentrates with cupric chloride in acidic solutions[J].Hydrometallurgy,2016,166:136-142.
[14]MIKI H,NICOL M.The dissolution of chalcopyrite in chloride solutions:IV.The kinetics of the auto-oxidation of copper(I)[J].Hydrometallurgy,2011,105:246-250.
[15]VELáSQUEZ-YéVENES L,NICOL M,MIKI H.The dissolution of chalcopyrite in chloride solutions:Part 1.The effect of solution potential[J].Hydrometallurgy,2010,103:108-113.
[16]WATLING H R.Chalcopyrite hydrometallurgy at atmospheric pressure:2.Review of acidic chloride process options[J].Hydrometallurgy,2014,146:96-110.
[17]HAVLIK T,SKROBIAN M,BALAZ P,KAMMEL R.Leaching of chalcopyrite concentrate with ferric chloride[J].International Journal of Mineral Processing,1995,43:61-72.
[18]TURKMEN Y,KAYA E.Acidified ferric chloride leaching of a chalcopyrite concentrate[J].The Journal of Ore Dressing,2009,11:16-24.
[19]NICOL M,MIKI H,VELáSQUEZ-YéVENES L.The dissolution of chalcopyrite in chloride solutions:Part 3.Mechanisms[J].Hydrometallurgy,2010,103:86-95.
[20]LUNDSTROM M,AROMAA J,FORSEN O,HYVARINEN O,BARKER M H.Leaching of chalcopyrite in cupric chloride solution[J].Hydrometallurgy,2005,77:89-95.
[21]TURKMEN Y,KAYA E,YAVUZHAN O.Leaching of chalcopyrite flotation concentrate with Cu Cl2-Na Cl-HCl[C]//Proceedings of the XIII International Mineral Processing Symposium.Bodrum,2012:361.
[22]AGACAYAK T,ARAS A,AYDOGAN S,ERDEMOGLU M.Leaching of chalcopyrite concentrate in hydrogen peroxide solution[J].Physicochemical Problems of Mineral Processing,2014,50:657-666.
[23]ANTONIJEVI?M M,JANKOVI?Z D,DIMITRIJEVI?M D.Kinetics of chalcopyrite dissolution by hydrogen peroxide in sulphuric acid[J].Hydrometallurgy,2004,71:329-334.
[24]TURAN M D,ALTUNDOGAN H S.Leaching of chalcopyrite concentrate with hydrogen peroxide and sulphuric acid in an autoclave system[J].Metallurgical and Materials Transactions B,2013,44:809-819.
[25]ANTONIJEVI?M M,JANKOVI?Z D,DIMITRIJEVI?M D.Investigation of the kinetics of chalcopyrite oxidation by potassium dichromate[J].Hydrometallurgy 1994,35:187-201.
[26]AYDOGAN S,UCAR G,CANBAZOGLU M.Dissolution kinetics of chalcopyrite in acidic potassium dichromate solution[J].Hydrometallurgy,2006,81:45-51.
[27]UCAR G,BOYRAZLI M,AYDOGAN S.Dissolution of fine particle chalcopyrite concentrate in acidic potassium dichromate solution[C]//Proceedings of 7th International Scientific Conference of Modern Management of Mine Producing,Geology and Environmental Protection.Albena:SGEM,2007:44-51.
[28]HAVLIK T,SKROBIAN M.Acid leaching of chalcopyrite in the presence of ozone[J].Canadian Metallurgical Quarterly,1990,29:133-139.
[29]PEDROZA F R C,AGUILAR M J S,TREVINO T P,LUEVANOS A M,CASTILLO M S.Treatment of sulfide minerals by oxidative leaching with ozone[J].Mineral Processing and Extractive Metallurgy Review,2012,33:269-279.
[30]KERTALLI E,van RIJNSOEVER L S,PAUNOVIC V,NEIRA D'ANGELO M F,SCHOUTEN J C,NIJHUIS T A.Propylene epoxidation with hydrogen peroxide in acidic conditions[J].Chemical Engineering Science,2016,156:36-43.
[31]HE Mei-feng,WANG Hao,JIANG Hong,ZHAO Su,PAN Deng.Effect of hydrogen peroxide concentration on surface properties of Ni-Cr alloys[J].Transactions of Nonferrous Metals Society of China,2016,26:1353-1358.
[32]LI Qian,RAO Xue-fei,XU Bin,YANG Yong-bin,LIU Ting,JIANG Tao,HU Long.Extraction of manganese and zinc from their compound ore by reductive acid leaching[J].Transactions of Nonferrous Metals Society of China,2017,27:1172-1179.
[33]DIMITRIJEVI?M,ANTONIJEVI?M M,DIMITRIJEVI?V.Investigation of the kinetics of pyrite oxidation by hydrogen peroxide in hydrochloric acid solutions[J].Minerals Engineering,1999,12:165-174.
[34]GREENWOOD N N,EARNSHAW A.Chemistry of the elements[M].New York:Pergamon Press,1984.
[35]ADEBAYO A O,IPINMOROTI K O,AJAYI O O.Dissolution kinetics of chalcopyrite with hydrogen peroxide in sulphuric acid medium[J].Chemical and Biochemical Engineering Quarterly,2003,17:213-218.
[36]MAHAJAN V,MISRA M,ZHONG K,FUERSTENAU M C.Enhanced leaching of copper from chalcopyrite in hydrogen peroxide–glycol system[J].Minerals Engineering,2007,20:670-674.
[37]TURAN D,SARI Z A,MILLER J D.Leaching of blended copper slag in microwave oven[J].Transactions of Nonferrous Metals Society of China,2017,27:1404-1410.
[38]SOLIS-MARCíAL O J,LAPIDUS G T.Improvement of chalcopyrite dissolution in acid media using polar organic solvents[J].Hydrometallurgy,2013,131-132:120-126.
[39]RUIZ-SáNCHEZ A,LAPIDUS G T.Study of chalcopyrite leaching from a copper concentrate with hydrogen peroxide in aqueous ethylene glycol media[J].Hydrometallurgy,2017,169:192-200.
[40]VAZARLIS H G.Hydrochloric acid-hydrogen peroxide leaching and metal recovery from a Greek zinc-lead bulk sulphide concentrate[J].Hydrometallurgy,1987,19:243-251.
[41]BABA A A,ADEKOLA F A.Comparative analysis of the dissolution kinetics of galena in binary solutions of HCl/Fe Cl3 and HCl/H2O2[J].International Journal of Minerals,Metallurgy and Materials,2011,18:9-17.
[42]HE Gui-xiang,ZHAO Zhong-wei,WANG Xiao-bo,LI Jiang-tao,CHEN Xing-yu,HE Li-hua,LIU Xu-heng.Leaching kinetics of scheelite in hydrochloric acid solution containing hydrogen peroxide as complexing agent[J].Hydrometallurgy,2014,144-145:140-147.
[43]DIMITRIJEVI?M,ANTONIJEVI?M M,JANKOVI?Z.Kinetics of pyrite dissolution by hydrogen peroxide in perchloric acid[J].Hydrometallurgy,1996,42:377-386.
[44]ANTONIJEVI?M,DIMITRIJEVI?D,JANKOVI?Z.Leaching of pyrite with hydrogen peroxide in sulphuric acid[J].Hydrometallurgy,1997,46:71-83.
[45]AYDOGAN S.Dissolution kinetics of sphalerite with hydrogen peroxide in sulphuric acid medium[J].Chemical Engineering Journal,2006,123:65-70.
[46]SHU Chi-Min,YANG Yuh-Joang.Using VSP2 to separate catalytic and self-decomposition reactions for hydrogen peroxide in the presence of hydrochloric acid[J].Thermochimica Acta,2002,392-393:259-269.
[47]VOLL F A P,PALU P,SANTOS J B O.Influence of catalyst treatments on the decomposition of hydrogen peroxide on supported palladium catalysts[J].Latin American Applied Research,2011,41:305-310.
[48]EARY L E.Catalytic decomposition of hydrogen peroxide by ferric ion in dilute sulfuric acid solutions[J].Metallurgical Transactions B,1985,16:181-186.
[49]CARRILLO-PEDROZA F R,DAVALOS-SANCHEZ A,SORIAAGUILAR M,PECINA-TREVINO E T.Coal desulfurization in oxidative acid media using hydrogen peroxide and ozone:A kinetic and statistical approach[J].Energy&Fuel,2009,23:3703-3710.
[50]CHIRITA P.Hydrogen peroxide decomposition by pyrite in the presence of Fe(III)-ligands[J].Chemical and Biochemical Engineering Quarterly,2009,23:259-265.
[51]ETO I,AKIYOSHI M,MIYAKE A,OGAWE T,MATSUNAGA T.Hazard evaluation of runaway reaction of hydrogen peroxide–Influence of contamination of various ions[J].Journal of Loss Prevention in the Process Industries,2009,22:15-20.
[52]LU Z Y,JEFFREY M I,LAWSON F.An electrochemical study of the effect of chloride ions on the dissolution of chalcopyrite in acidic solutions[J].Hydrometallurgy,2000,56:145-155.
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