Study on copper kinetics in processing sulphide ore mixed with copper and zinc with sulfuric acid leaching under pressure
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1 IOP Conference Series: Materials Science and Engineering PAPER OPEN ACCESS Study on copper kinetics in processing sulphide ore mixed with copper and zinc with sulfuric acid leaching under pressure To cite this article: LUO Wen-bo et al 218 IOP Conf. Ser.: Mater. Sci. Eng View the article online for updates and enhancements. This content was downloaded from IP address on 14/6/218 at 11:55
2 Study on copper kinetics in processing sulphide ore mixed with copper and zinc with sulfuric acid leaching under pressure LUO Wen-bo a, WANG Ji-kun a,b, GAN Yin c a Faculty of Metallurgical and Energy Engineering, Kunming University of Science and Technology, Kunming, Yunnan 6593, China b Yunnan Metallurgy Group Parent Company, Kunming, Yunnan 6531, China c Yunan Gold&Mining Group CO.,LTD, Kunming, Yunnan 65224, China luowenbo@126.com Abstract. Sulphide ore mixed with copper and zinc is processed with pressure acid leaching. Research is conducted on the copper kinetic. The stirring rate is set at 6 rpm which could eliminate the influence of external diffusions. Research is conducted on the factors affecting the copper leaching kinetic are temperature, pressure, concentration of sulfuric acid, particle size. The result shows that the apparent activity energy is 5.7 KJ/mol. We could determine that the copper leaching process is shrinking core model of chemical reaction control and work out the leaching equation. 1. Introduction So far, 85% copper around the world is extracted through pyrogenic process and only 15% copper is produced through wet process. But the pyrogenic process requires that the copper content should be high and the detrimental impurity content should be low. Due to the mining of ore resources and the depletion of high-quality mineral resources, most of the resources remained are lean ore and mixed ore [1]. The mixed ore is separated through benefication, not only the metal recovery rate is low but also the content of each metal is high in the concentrate. So it is hard to meet the request of smelting. Pressure leaching is a clean and effective new metallurgy technique which has been applied to zinc sulfide ore, nickel and cobalt extraction, Gold pretreatment, etc as well as the pressure leaching of mixed ore. The results are all quite satisfying [2-4]. So far, the researches on copper leaching kinetic are: cooper leaching kinetic in ferric sulfate acid solution conducted by Misra [5], the copper leaching kinetic in chlorination system conducted by Havlik [6], the copper leaching kinetic in Hydrogen peroxide - ethylene glycol system conducted by Mahajan [7], the low grade copper oxide ore leaching kinetic in Ammonia - ammonium sulphate system conducted by Liu Zhixiong [8], the chalcopyrite dissolution kinetics conducted by Xing Weiguo [9], the pressure copper leaching kinetic in chalcopyrite concentrate by McDonld [1], the pressure copper leaching kinetic in lead matte conducted by Jin Bingjie [11], etc [12-14]. it can be seen that researches on copper leaching kinetic are mostly concentrated on leaching process under normal pressure and there are fewer researches on leaching process under intense pressure. For making clear the mineral containing copper leaching behavior in processing sulphide ore mixed with copper and zinc with sulfuric acid leaching under pressure and facilitate the leaching of copper, Content from this work may be used under the terms of the Creative Commons Attribution 3. licence. Any further distribution of this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI. Published under licence by Ltd 1
3 this paper conducts research on copper leaching kinetic in sulphide ore mixed with copper and zinc to find out the main factors affecting copper indium leaching kinetic and find out the reaction controlling steps and set up the kinetic equation. 2. Test materials and methods. 2.1 test materials The test materials are sulphide ore mixed with copper and zinc obtained in Yunnan Province, China. The chemical composition of the sample is shown in Table 1. Table1. The main components Component Zn Cu Fe S Pb Ag Au Content (%) The materials are sulphide ore containing copper, zinc, iron and a part of oxidized ore. Analysis on the chemical matter phase shows that zinc, copper and iron exist in the form of ZnS, CuFeS 2 and Fe 1- XS. 2.2 Testing method Mixed ore and Sulfuric acid leaching agent are filled in 2 L autoclave according to a certain proportion and then seal the autoclave. Fill in the oxygen till the pressure reach the set value and increase the temperature at the same time, start stirring until the temperature reaches the set value and start timing, keep stirring while keeping the pressure and temperature inside the autoclave at the set value until the set time. After the reaction is completed, fill the cool water in the autoclave to reduce the temperature to 9. Release the pressure and stop stirring. Open the autoclave cover and take out the pulp and filter it. Take the sample of filtrate and leaching residues to analyze. To make sure the concentration of leaching agent is steady, we set the liquid-solid ratio at 5:1. That is to say 1 g mineral and 5 ml sulfuric acid leaching agent are used in every test and keep the rate of temperature increase and decrease at around the same value. 3. Result and discussion The main chemical reaction happened in the pressure leaching process: CuFeS + 2H SO + O = FeSO + CuSO + 2S + 2H (1) ( 1- ) ( 1- ) 2 ( 1- ) ( 1- ) Fe S + x H SO + x O = x FeSO + S + x H O (2) 1-x ZnS + H SO +.5O = ZnSO + S + H O (3) The above test (1) and (3) show that there is solid product Sulphur produced. We have reason to believe that this liquid-solid reaction process is shrinking core model with solid products generated. The reaction steps of shrinking core model include: 1). the liquid reactant diffuse externally through the liquid boundary layer. 2) The liquid reactant diffuses internally through the solid product layer. 3) Interface chemical reaction. The leaching rate is decided by the component with the lowest reaction rate [15-16]. The kinetic equation when the reaction is controlled by external diffusions reaction [15] : α = kt c (4) where α the leaching rate of solid reactant; k c the rate constant of external diffusions; t time,min; 2
4 The kinetic equation when the reaction is controlled by internal diffusions reaction [15] : 1 23α ( 1 α) 23 = kt d (5) where k d the rate constant of internal diffusions; The kinetic equation when the reaction is controlled by chemical reaction [15] : 1 ( 1 α ) 13 = kt r (6) where k r the rate constant of chemical reaction; We could get the copper leaching kinetic equation when we work out the speed constant K The effect of stirring rate on copper leaching When the particle size is 8~96 μm, the temperature is 13, the liquid-solid ratio is 5 ml/g, the concentration of sulfuric acid is 5 g/l, the pressure is 1. Mpa, the time is 1 h, a small amount of Surfactant lignin is added, the effect of stirring rate on the copper leaching rate is shown in Fig. 1. Fig. 1. shows that when the stirring speed is over 6 rpm, it has no effect on the rate of copper leaching. It means that when the stirring rate is over 6 rpm, therefore, in the future test, we set the stirring speed at 6 rpm to eliminate the effect of stirring rate on copper leaching. 3 Leaching rate of copper(%) Mixing speed(r/min) Figure.1. Effect of mixing speed on leaching rate of copper 3.2 The effect of temperature on copper leaching rate When the particle size is 8~96 μm, the concentration of sulfuric acid is 5 g/l, the pressure is 1. Mpa, the stirring rate is 6 rpm, a small amount of surfactant lignin is added, the effect of temperature on the copper leaching rate is shown in Fig. 2. Leaching rate of copper(%) C 13 C 14 C 15 C Figure. 2. Effect of temperature 3
5 1-(1-α) 1/ y 12 C = x y 13 C = x y 14 C = x y 15 C = x. Time/min Figure. 3. Relationship of temperature 1 ( 1 α ) 13 with time We could work out the relationship of 1 ( 1 α ) 13 and 1 2α 3 ( 1 α) 23 with time. The result shows in Fig. 3 and 4. From Fig. 3 and Fig. 4, we could see the coefficient all bigger than.991 and the line fitting is good. Fig. 4 shows that the smallest coefficient is.935 and the line fitting is bad. The preliminary result shows that the leaching process is controlled by chemical reaction. 1-2/3α-(1-α) 2/ y 12 C = x y 13 C = x y 14 C = x y 15 C = x. Figure.4. Relationship of temperature ( ) α 3 1 α with time y= x -7. lnk /T Figure.5. Arrhenius plot of chemical reaction control Fig. 3 the straight slope of the logarithm of different temperature. The results are shown in Fig. 5. According to Arrhenius theorem [15] : 2 d lnk dt = Ea RT 4
6 The integration is as follows: ln K = Ea RT + C The apparent activation energy of chemical reaction control is 5.7kJ/mol according to Fig.6. According to the shrinking core model kinetic theory, when the apparent activation energy is 8~2 kj/mol, the leaching process is internally diffusions control. When the apparent activation energy is over 4 kj/mol, the leaching process is chemical reaction control. It can be estimated that the leaching process is chemical reaction control. We could set up the kinetic equation which shows the temperature s effect on copper leaching according to the result in Fig ln K = T (7) 3.3. The effect of particle size on copper leaching efficiency. The sulfuric acid is 5 g/l, pressure 1. MPa, temperature 13, stirring rate 6 rpm, a small amount of lignin is added, the effect of particle size on the copper leaching rate shown in fig. 6. We work out the relationship between different 1 ( 1 α ) 13 of particle size and time. The result is shown in Fig. 7. Leaching rate of copper(%) µm 8-96µm 75-8µm 53-58µm Figure. 6. Effect of mineral grain-size 1-(1-α) 1/ µm y= x 8-96µm y= x 75-8µm y= x 53-58µm y= x. Figure. 7. Relationship between different 1 ( 1 α ) 13 of particle size and time According to Fig. 7, we could work out the relationship between ln Kand lnr. The result is shown in Fig. 8. 5
7 y= x -6.9 lnk lnr Figure. 8. The relationship ln Kwith lnr We could set up the kinetic equation which shows the particle size s effect on copper leaching according to the result in Fig. 8. ln K = ln r (8) 3.4. The effect of pressure on copper leaching efficiency. Particle size 8~96 μm, the sulfuric acid 5 g/l, temperature 13, stirring rate 6 rpm, a small amount of lignin is added. Test the effect on copper leaching rate when the pressure is within the range of.8~1.4 Mpa. We work out the relationship between different 1 ( 1 α ) 13 of pressure and time. The result is shown in Fig Leaching rate of copper(%) Mpa 1.Mpa 1.2Mpa 1.4Mpa Figure. 9. Effect of pressure 1-(1-α) 1/ y.8mpa = x y 1.Mpa = x y 1.2Mpa = x y 1.4Mpa = x. Figure. 1. Relationship of pressure 1 ( 1 α ) 13 with time According to Fig. 1, we could work out the relationship between ln Kand lnp. The result is shown in Fig
8 y= x lnk lnp Figure. 11. Relationship ln Kwith lnp We could set up the kinetic equation which shows the pressure s effect on copper leaching according to the result in Fig. 11. ln K = ln P (9) 3.5. The effect of initial acidity on copper leaching efficiency. Particle size 8~96 μm, pressure 1. MPa, temperature 13, stirring rate 6 rpm, a small amount of lignin is added, the effect of initial acidity on copper leaching rate shown in fig.12. We work out the relationship between different 1 ( 1 α ) 13 of sulfuric acid and time. The result is shown in Fig. 13. Leaching rate of copper(%) g/L 7g/L 9g/L 12g/L Figure. 12. Effect of sulfuric acid 1-(1-α) 1/ y 5g/L = x y 7g/L = x y 9g/L = x y 12g/L = x. Figure. 13. Relationship between different 1 ( 1 α ) 13 of sulfuric acid and time According to Fig. 13, we could work out the relationship between ln Kacid and ln C. The result is shown in Fig
9 y= x lnk lnc Figure. 14. Relationship ln Kwith lnp We could set up the kinetic equation which shows the sulfuric acid s effect on copper leaching according to the result in Fig. 14. ln K = ln C (1) 4. Establish Kinetic equation The test above shows that the equations (7),(8),(9),(1) are all linear relationship. Multiple linear regression analysis is conducted on dependent variable ln kand independent variable 1/T ln P ln C ln r with SPSS software. The regression equation is obtained: 1 ln K = ln P.542ln C 1.223ln r T Therefore, we could work out the copper leaching kinetic equation in the process of pressure acid leaching of sulphide ore mixed with copper and zinc. 3 1 α = 1 1 t exp ln P.542ln C 1.223ln r T 5. Conclusions (1) The test using 2 L autoclave to simulate practical production.when the stirring rate is over 6 rpm, it almost has no effect on copper leaching rate. Therefore under this condition, the external diffusions process is not the copper leaching reaction controlling steps. (2) In the process of pressure acid leaching of sulphide ore mixed with copper and zinc, the apparent activation energy of copper leaching chemical reaction control is 5.7 kj/mol. We could determine that the copper leaching reaction is shrinking core model controlled by chemical reaction. (3) The influence of temperature, initial acidity, pressure, particle size on copper leaching. The kinetic equation of copper leaching in the process of pressure acid leaching of sulphide ore mixed with copper and zinc is listed as follows: 3 1 α = 1 1 t exp ln P.542ln C 1.223ln r T (4) In fact, this kinetic equation of copper has deviation with practical production. This result occurred because the stirring rate is lower than 6 rpm and the initial acidity value change with time in practical production. 8
10 References [1] Xie K Q, Yang X W, Shu Y Z and Shen Q F 26 China Nonferrous Metallurgy vol 4 p 19 [2] F Habashi 24 The Canadian Institute of Mining, Metallurgy and Petroleum p 3 [3] F Habashi 1997 Proc. Of the XX IMPC (Aachen) vol 1 p 129 [4] Mike Anthony and Doug Flett 2 England Mineral Industrial Research Organization vol 2 p 55 [5] Misra M and Fuerstenau M. C 25 Minerals Engineering vol 18 p 293 [6] Havlik T, Skrobian M, Balaz P and et al 1995 INT J M INER PROCESS vol 43 p 61 [7] Mahajan V, Misra M, Zhong K and et al 27 Minerals Engineering vol 2 p 67 [8] Liu Z X, Yin Z L, Hu H P and et al 212 J. Cent. South Univ vol 19 p 77 [9] Xing W G, Zhong Z Q, Mei G G 199 Nonferrous Metals(Extractive Metallurgy) vol 5 p 27 [1] McDonald R G, Muir D M 27 Hydrometallurgy vol 86 p 191 [11] Jin B J, Yang X W, Shen Q F 29 Hydrometallurgy vol 99 p 119 [12] FAN X X, PENG J H, HUANG M Y and et al 25 Precious Metals vol 26 p 15 [13] Arslan F, Bulut G, Kangal M O and et al 24 Scandinavian Journal of Metallurgy vol 33 p 6 [14] Qiu T, Nie G, Wang I and et al 27 Trans Nonferrous Met Soc China vol 17 p 418 [15] Hua Y X 24 An Introduction to Kinetics of metallurgical processes (Bei Jing: Metallurgical Industry Press) p [16] Mo D C 1987 Kinetics of metallurgical (Chang Sha: Central south university press) p 173 9
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