RARE METALS

Vol. 31, No. 4, Aug. 2012, p. 402

DOI: 10.1007/s12598-012-0528-1

Kinetics of simultaneous leaching of Ag and Pb from hydrometallurgical zinc

residues by chloride

ZHANG Yalia, YU Xianjina, and LI Xiaobinb

a
College of Chemical Engineering , Shandong University of Technology, Zibo 255081,China
b
School of Metallurgical Science and Engineering, Central South University, Changsha 410083, China
Received 11October 2011; received in revised form 27 December 2011; accepted 21 March 2012
© The Nonferrous Metals Society of China and Springer-Verlag Berlin Heidelberg 2012

Abstract

The leaching kinetics of silver and lead simultaneously from zinc residue by chloride was investigated. The effects of stirring speed, tem-
perature, sodium chloride concentration, particle size and liquid/solid ratio on Ag and Pb dissolution in sodium chloride were studied. It was
determined that the dissolution rates increased with increasing sodium chloride concentration, temperature and decreasing particle size. The
dissolution kinetics followed a shrinking core model, with inter-diffusion through gangue layer as the rate determining step. This finding is in
accordance with the apparent activation energy (Ea) of 26.8 kJ⋅mol−1 (Ag) and 26.5 kJ⋅mol−1 (Pb), and a linear relationship between the rate
constant and the reciprocal of squared particle size. The orders of reaction with respect to sodium chloride concentration, temperature and
particle size were also achieved. The rate of reaction based on diffusion-controlled process can be expressed by semi-empirical equations.

Keywords: hydrometallurgical zinc residue; chloride leaching; inner diffusion-controlled; semi-empirical equations

or hydrometallurgical routes. The low grade metals of resi-

1 Introduction
Hydrometallurgical zinc residue is the major waste mate-
rial produced from the extraction of zinc from sulfidic ores
by sulfuric acid solution, which threatens the environment
because of many heavy metals. At present, producing 1 t of
zinc electrowinning generates 300 t of residues [1−2], which
contain considerable amount of zinc, lead, iron, silver and
other minor valuable constituents. With the depletion of zinc
ores and rapid rising of the metal price, the processing of
zinc leach residue as different secondary resource rather
than waste for sustainable production because of the high
metal content has become a more attractive route for sus-
tainable production [3−4]. Therefore, the concern is not exclu-
sively environmental, but economic as well. The residue
usually contains a low grade lead of an average of 8% and
300~500 g silver per 1 t residue in weight and high grade
gangue [5].
Up to now, many researchers have carried out a lot of
studies to treat the leaching residues for recovering zinc as
well as lead and silver. The mineral and metallurgy proc-
esses are operated [6−10]. They focus on the metallurgical
technique especially, which can be either pyrometallurgical
due lead to high consumption of energy in pyrometallurgical
processing such as carbothermic reduction because of heat-
ing high contents of gangue materials, and 70%~80% total
Zn and Pb recovery can be obtained, but only 10% total Ag
can be recovered [11]. R. Raghavan [12] adopted hydro-
metallurgical processing to recover lead and silver. Two ap-
proaches have been selected. One is a simple dou-
ble-decomposition technique; the other is that the residue
was treated with brine solution. The recovery rates of lead
and silver are 90%~95% and 60%~70%. Farahmand [13]
adopted brine leaching of lead-bearing zinc plant residues,
the extractions of lead and zinc are 89.43% and 3.54%, but
cannot recover silver. These methods are introduced to re-
cover metals one by one; few literatures have been involved
in the recovery of lead and silver by chloride leaching si-
multaneously after zinc extraction. The process is simple,
easy to implement with higher recovery, cost-effective and
environmentally friendly. In this work, the leaching kinetics
by chloride was studied preliminarily to learn about the
leaching behavior and the step of rate controlling and pay
for the next remediation of the residue by chloride leaching
simultaneously.

Corresponding author: YU Xianjin, LI Xiaobin E-mail: xjy@sdut.edu.cn, xbli@csu.edu.cn

ZHANG Yali, et al., Kinetics of simultaneous leaching of Ag and Pb from hydrometallurgical zinc residues by chloride 403

Table 1 Chemical composition of residue after zinc extraction

Elements Percentage / % Elements Percentage / % Elements Percentage / % Elements Percentage / %

Pb 12.2600 Ag 0.0651 Mg 1.3000 Ti 0.0341
Zn 1.0800 Mn 0.0310 Al 0.4210 Sb 0.1310
N 0.5650 S 4.9900 Si 15.3000 Ba 0.1190
O 44.5000 Cu 0.0991 P 0.0500 Ca 1.2000

2 Experimental
2.1 Materials
The representative samples of residues were obtained
from a plant in Shandong province. Prior to use in this study,
the samples were washed, dried and sieved to obtain a re-
quired fraction. These samples were subjected to detailed
analyses before experiments. The chemical composition by
X-ray fluorescence (XRF) and atomic absorption spectros-
copy (AAS) are given in Table 1 and chemical phase com-
positions of lead and silver are shown in Tables 2 and 3. The
pattern of X-ray diffraction analysis (XRD) is given in Fig. 1 XRD pattern of residue after zinc extraction
Fig. 1. The XRF and AAS analyses show that the samples
contain 12.26% Pb, 651 g⋅t−1 Ag, 2.78% Fe, 15.30% Si and the water-soluble substance and enrich lead and silver, and
4.99% S. XRD analysis shows Anglesit (PbSO4), Anhydrite the slurry was filtered. The cake was laid in a drying cabinet
(CaSO4) and Quartz (SiO2) as major components; there is no for 10 min, then the materials were dry-screened to obtain
obvious diffraction peak of silver because of its trace four different sizes to examine the possible effect of particle
amounts in the residues. size. The leaching experiments were performed in a 500 ml
2.2 Experimental procedure vessel with two opening set up in a thermostatically con-
The secondary hydrometallurgical zinc residuals after trolled oil bath and the temperature controlling accuracy was
zinc extraction were washed four times by water to scour off ±0.5 K. To minimize aqueous loss when the system was
heated, a reflux condenser was mounted on the top of one
Table 2 Mineral phase constitutes of silver opening. The mechanical stirrer used had a controller unit
and its agitator shaft was made of glass to avoid corrosion
Components Repartition of silver / (g⋅t−1) Percentage/% and cementation by iron. 500 ml of clear brine solution with
Silver in lead silicate 336 51.62 known concentration was added to the reaction vessel.
Native silver 177 27.14 When the temperature of the solution system reached the
Silver sulfide 48 7.37 predetermined value, 10.00 g sample was introduced into
the flask, the acidity was adjusted to the desired value by
Silver in silicate 33 5.02
using a small amount of HCl, and H2O2 was used as additive.
Rests 57 8.85 After maintaining for a preset reaction period, the leach
TAg 651 100.00 slurry was filtered immediately and washed for three times
and the filtrate was diluted with distilled water. The cake
Table 3 Mineral phase constitutes of plumbum was dried and analyzed for Pb and Ag.

Components Repartition of plumbous / % Percentage / %

Anglesite 7.50 61.17
3 Results and discussion
Lead sicicon 2.42 19.74 3.1 Leaching kinetics analysis
Galenite 0.24 1.96 The leaching of the secondary residue after zinc extrac-
tion with sodium chloride solution is a typical liquid/solid
Rests 2.10 17.13
heterogeneous reaction. The main chemical reactions that
TPb 12.26 100.00
occur between residue and sodium chloride solution are
404
listed as follows [14]:
2+
PbSO 4 ⇔ Pb + SO 4 2−
(1)
2+ 2−i
Pb + iCl− = PbCli (i =1, 2, 3, 4, 5) (2)
Ag − e = Ag + (3)
Ag + + jCl− = AgCl j1− j ( j =1, 2, 3, 4) (4)
The particle of slags after dissolution was detected, and
the average diameter of leached slags was 13.79 μm com-
pared with 14.9 μm of those before leaching; the particle
diameter hardly changed. The leaching rates of Pb and Ag
were 94.75% and 82%, respectively, when 10.00 g samples
were leached by 350 g⋅L−1 solution chloride for 2 h at a liq-
uid/solid ratio of 15, temperature of 368.15 K, stirring rate
of 400 r⋅min−1, HCl of 12 ml, and H2O2 of 15 ml. The con-
centration of solution chloride decreased less than 10%, the
amount largely exceeded the theoretical amount, so the
concentration was considered as constant during the whole
process, which was consistent with the hypothesis of the
pseudo-stationary state. Therefore, the leaching process can
be analyzed with the shrinking core model [15]. According
to this model, the rate of reaction between solid particle and
solution may be controlled by one of the following steps
[13]: diffusion controlled, chemical reaction controlled and
combination controlled of diffusion and chemical reaction.
The rate-controlling step of the leaching process depends on
experimental kinetics data.
3.2 Effect of stirring speed
Among the effective factors, stirring speed was taken into
consideration first while the reaction time, temperature, liq-
uid/solid ratio, initial sodium chloride concentration and
particle size were kept constant as 2 h, 368 K, 15, 300 g⋅L−1
and 0.080~0.098 mm. The experiments were carried out at
stirring speeds of 100, 200, 300, 400, 500 and 600 r⋅min−1
(12.5, 25.0, 37.5, 50.0, 62.5 and 75.0 m⋅s−1), respectively.
The results are presented in Fig. 2.
Fig. 2 Effect of stirring rate on leaching efficiency (HCl, 12 ml;
H2O2, 15 ml)
RARE METALS, Vol. 31, No. 4, Aug. 2012
It can be seen from Fig. 2 that the extraction rate of Ag
or Pb increases steadily with stirring speed increasing from
100(12.5 m⋅s−1) to 400 r⋅min−1 (50 m⋅s−1) and afterwards it
remains constant. This suggests that the influence of exter-
nal diffusion control to the leaching process is eliminated
when the stirring speed is above 400 r⋅min−1 (50 m⋅s−1) [16].
Thus, 400 r⋅min−1 (50 m⋅s−1) is chosen as an invariable
quantity for the subsequent experiments.
3.3 Effect of sodium chloride concentration
The sodium chloride concentration was varied in a range
from 200 g⋅L−1 to 350 g⋅L−1 while keeping reaction tem-
perature, duration time, liquid/solid ratio and stirring speed
at 368 K, 2 h, 15, and 400 r⋅min−1 (50 m⋅s−1), respectively.
Figs. 3 (a) and (b) illustrate the influence of sodium chloride
concentration on leaching rate. It is indicated that increasing
sodium chloride concentration could promote extraction rate.
Excess sodium chloride is necessary to maintain higher ex-
traction rate and ensure sufficient reactions, yet the extra so-
dium chloride is not economical in industrial production
practice. Therefore, to investigate the effects of other pa-
rameters, 350 g⋅L−1 was chosen.
When the diffusion through the gangue layer is rate con-
trolling, the kinetics may be correlated graphically using the
equation (Eq. 5) [17−18]:
Fig. 3 Effect of chloride concentration on leaching efficiency
(HCl, 12 ml; H2O2, 15 ml)
ZHANG Yali, et al., Kinetics of simultaneous leaching of Ag and Pb from hydrometallurgical zinc residues by chloride 405

k p t =1− 2/3 x − (1− x)1/3 (5) plots of lnkp versus lnco are shown in Figs. 4 (c) and (d). The
reaction orders are calculated to be 0.2114 for Pb and 0.0759
When the reaction rate is controlled by chemical reaction,
for Ag, which indicates that the dependency of Ag leaching
the following expression of shrinking core model can be
used to describe the kinetics: Table 4 Apparent rate constant and correlation coefficient
kc t =1− (1− x)1/3 (6) values (R2)
where kp = chemical rate constant (h−1); kc = reaction rate Reaction Chemical Diffusion through
constant (h−1); t = time(h); x = fraction reaction of Ag or Pb; condition reaction (Ag) the gangue layer (Ag)
On the basis of the experimental data in Figs. 3 (a) and K’a / min−1 R2 Ka / min−1 R2
(b), the rate constants and their correlation coefficients are 200 g·L−1 0.0824 0.9125 0.0092 0.9991
given in Tables 4 and 5 for the diffusion through the product 250 g·L−1 0.0882 0.9063 0.0175 0.9861
layer and the chemical reaction controlled model. Also, Figs. 300 g·L−1 0.0927 0.8832 0.0262 0.9957
4 (a) and (b) show the data plots according to diffusion con- 350 g·L−1 0.0966 0.8658 0.0356 0.9721
trol process.
The results in Tables 4 and 5 reveal that the values of the Table 5 Apparent rate constant and correlation coefficient
correlation coefficients for the diffusion through the product values
layer are closer to 1 than those of the chemical reaction con- Reaction Chemical Diffusion through
trolled model. Therefore, Eq. (5) was found to fit the data condition reaction (Pb) the gangue layer(Pb)
best. Figs. 4 (a) and (b) show that, during the whole reaction K’a/min−1 R2 Ka/min−1 R2
time, the data are linear, and zero point intercepts are ob-
200 g·L−1 0.1022 0.9158 0.0281 0.9806
tained. The linear relationship between 1− 2/3 x − (1− x)1/3
250 g·L−1 0.1153 0.8956 0.0468 0.9763
and leaching time is significant and indicates that the rates −1
300 g·L 0.1366 0.9186 0.0634 0.9934
of leaching reactions are controlled by diffusion through the
gangue layer [19]. The slope of these straight lines is kp. The 350 g·L−1 0.1524 0.9247 0.0760 0.9945

Fig. 4 Plots of leaching kinetics at different chloride concentration(a) and (b) and plots of lnKp against lnC0 (c) and (d)
406 RARE METALS, Vol. 31, No. 4, Aug. 2012

on sodium chloride concentration is less than that of Pb. Table 7 Apparent rate constant and correlation coefficient
However, all the dependency is slight, as can be seen in Fig. values
4, which indicates that a solid gangue layer forms and pre- Chemical Diffusion through
vents the mobilization of Ag and Pb from residuals. Reaction Reaction (Pb) the gangue layer (Pb)
condition
K’a/min−1 R2 Ka/min−1 R2
3.4 Effect of reaction temperature
The influence of reaction temperature on the Pb and Ag 318 K 0.0944 0.9936 0.0329 0.9815
leaching rates under the following conditions: time 2 h, liq- 338 K 0.1274 0.9789 0.0387 0.9926
uid/solid ratio 15, sodium chloride concentration 350 g⋅L−1, 353 K 0.1587 0.9748 0.0499 0.9948
stirring speed 400 r⋅min−1 (50 m⋅s−1), is investigated. The
results are presented in Figs.5 (a) and (b). The rate constants 368 K 0.1865 0.9666 0.0576 0.9947
and their correlation coefficients are given in Tables 6 and 7.
The plots of the right-hand side of Eq. (5) against time are It can be seen in Figs. 5 (a) and (b) that the temperature
obtained by substituting the experimental data into Eq. (5) has a noticeable influence on the extraction of Ag and Pb.
and given in Figs. 6 (a) and (b). About 47.15% for silver and 69.12% for lead in the fine
fraction of the residuals are extracted after 3.5 h at a reaction
temperature of 318 K; at 368 K, the leaching rate are
82.05% for silver and 97.29% for lead. The metal extraction
increased with increasing the temperature, which is mainly
because high temperature can increase the numbers of acti-
vated molecule and diffusion coefficient, the metal dissolu-
tion can be improved.
The experimental data in Figs. 6 (a) and (b) are approxi-
mately linear and almost goes through the origin, which also
suggests that an inner diffusion-controlled model is suitable
for this reaction process, as can be also seen from the value
of correlation coefficient values in Tables 6 and 7. The acti-
vation energy [19] of an inner diffusion-controlled process is
characterized to be 8-30 kJ·mol−1, while for a chemically
controlled process, it is usually greater than 40 kJ·mol-1. The
apparent activation energy was determined based on Ar-
rhenius equation [20]:
⎛ −E ⎞
K a = K 0 exp⎜ a ⎟ (7)
⎝ RT ⎠
where: K0 is frequency factor (min−1), Ea is apparent activa-
tion energy (kJ⋅mol−1), R is ideal gas constant (8.314
J·mol−1·K−1), T is leaching temperature (K).
To calculate the apparent activation energy, the values of
lnkp against 1000/T are plotted in Figs. 6 (c) and (d). The ac-
Fig. 5 Effect of leaching temperature on leaching efficiency tivation energy of the overall reaction is calculated to be
(HCl, 12 ml, H2O2, 15 ml)
about 26.8 kJ·mol−1 for Ag and 26.5 kJ·mol−1 for Pb. The
Table 6 Apparent rate constant and correlation coefficient frequency factor (K0) is calculated to be about 0.0399 for Ag
values
and 0.0412 for Pb. The energy values fall in the range of
Chemical Diffusion through typical inner diffusion controlled process, which supports
Reaction
reaction (Ag) the gangue layer (Ag) the conclusion that the leaching process is controlled by the
condition
K’a/min−1 R2 Ka/min−1 R2 mass transfer through the gangue product layer [21].
318 K 0.0498 0.9292 0.0227 0.999
338 K 0.0708 0.9007 0.0254 0.9966 3.5 Effect of particle size
353 K 0.0909 0.883 0.0286 0.9967 The influence of particle size on the extraction of Pb and
368 K 0.1118 0.8769 0.0329 0.9941 Ag was examined with four different size fractions (0.075~
ZHANG Yali, et al., Kinetics of simultaneous leaching of Ag and Pb from hydrometallurgical zinc residues by chloride
Fig. 6 Plots of leaching kinetics at different temperatures (a) and (b) and plots of lnKa against 1/T (c) and (d)
0.090 mm, 0.090~0.106 mm, 0.106~0.125 mm, 0.125~0.150
mm) at 368 K under a stirring speed of 400 r⋅min−1 (50 m⋅s−1)
and sodium chloride concentration of 350 g⋅L−1. The kinetic
data are fitted well with Eq.(1) and the results are given in
Figs. 7 (a) and (b).
It can be seen from Figs. 7 (a) and (b) at the same leach-
ing time that the smaller is the particle size , the faster is the
metal dissolution. The reason is likely that, when the total
weight is kept constant, decreasing the particle size can in-
crease numbers and the contact area of particles with the
fluid. The results for the effects of particle size on dissolu-
tion were applied to this kinetic model, the apparent rate
constant was determined. According to lnKd–lndo curve
shown in Figs. 7 (c) and (d), the orders of reaction with re-
spect to particle size (d0) were found to be inversely propor-
tional to a 0.5678 power for Pb and a 0.5108 power for Ag.
Calculations show that activation energy and the orders
of reaction values with respect to sodium chloride concen-
tration and particle size confirm to the shrinking core model
for a diffusion controlled process. K can be expressed as the
following equation [22−23]:
⎛ −E ⎞
K = K 0 C1α ⋅C2β ⋅⋅⋅d 0Kd ⋅exp⎜ a ⎟ (8)
⎝ RT ⎠
407
where: Ci is bulk fluid concentration (mol/L), α, β, Kd is re-
action order of variable C1, C2 and d0, respectively.
Thus, the leaching of Pb and Ag can be presented by Eqs.
(9) and (10):
2 2
−26800 ⎞
1− x − (1− x) 3 = 0.0399C 0.2114 d 0−0.5678 exp⎛⎜ ⎟t (9)
3 ⎝ RT ⎠
2
2 −26500 ⎞
1− x − (1− x) 3 = 0.0412C 0.0759 d 0−0.5108 exp⎛⎜ ⎟t (10)
3 ⎝ RT ⎠
3.6 Effect of solid concentration(liquid/solid ratio)
To make the leaching process analyzed with the shrink-
ing core model, the liquid/solid ratio of 15 was selected.
However, this low solid concentration can result in more
consumption and large liquid circulation. In this work, sev-
eral experiments were performed at other optimal leaching
conditions (stirring speed of 400 r⋅min−1 (50 m⋅s−1), particle
size of 0.075~0.090 mm and sodium chloride concentration
of 350 g⋅L−1, time of 2 h, temperature of 368 K), and the ap-
propriate liquid/solid ratio was determined. The results are
presented in Fig. 8.
As seen from Fig. 8, below liquid/solid ratio of 5, the
leaching efficiency of Ag increased significantly with the
408 RARE METALS, Vol. 31, No. 4, Aug. 2012

Fig. 7 Plots of leaching kinetics at different particle sizes (a) and (b) and plots of lnKd against lnd0 (c) and (d)

3.7 Characterization of solid residuals after leaching

Fig. 8 Effect of liquid/solid ratio
increasing of liquid/solid ratio, and the same regularity of Pb
was below 7. Therefore, it was decided that a solid–liquid
ratio of 7 could be the best choice available so that both Ag
and Pb had the desired leaching effects.
The solid residuals, reacted at 368 K for 2 h under the
conditions of stirring speed of 400 r⋅min−1 (50 m⋅s−1), parti-
cle size of 0.075-0.090 mm and sodium chloride concentra-
tion of 350 g⋅L−1, were characterized by XRD and chemical
analysis.
The chemical composition of solid residuals is shown in
Table 8. Compared with Table 1, it can be seen that the
content of Pb varied from 12.26% to 0.414%, and the con-
tent of Ag decreased to 117 g⋅L−1 from 651 g⋅L−1. The
leaching rates of Pb and Ag can reach 96.6% and 82.1%.
The XRD (Fig. 9) patterns of solid residuals after leaching
indicate that the major mineral phase is quartz(SiO2). Zne-
site(Ca2Mn7Si10O28(OH)2·5H2O) and jahnsite(Ca, Mn, Mg)
(Ca2MnMg2Fe2(PO4)·8H2O) are the minor phases. The dif-
fraction peaks of anglesite (PbSO4) is not observed, which

Table 8 Chemical compositions of slags after extraction

Elements Percentage / % Elements Percentage / % Elements Percentage / % Elements Percentage / %
Pb 0.4140 Ag 0.0117 O 51.1000 Si 28.5000
C 5.4300 Cr 0.0084 Fe 1.9900 As 0.2580
Ca 2.8600 Mn 0.0227 Mg 2.0900 Sr 0.0078
ZHANG Yali, et al., Kinetics of simultaneous leaching of Ag and Pb from hydrometallurgical zinc residues by chloride
Fig. 9 XRD pattern of residue after chloride leaching
indicates the technology of chloride leaching of silver and
lead simultaneously is effective.
4 Conclusion
The first chemical step of an integrated process for re-
covering Ag and Pb by chloride leaching from zinc plant
residues was tested. Taking into account the parameters used in
the experiments, stirring speed, temperature, sodium chloride
concentration, particle size and liquid/solid ratio and their
levels, a kinetic model has been assigned to simultaneous
leaching of Ag and Pb from hydrometallurgical zinc residues
by chloride, which is found to fit the shrinking core model
for an inner diffusion through the gangue layer controlled
process, when the stirring speed is above 400 r⋅min−1 (50
m⋅s−1), it can eliminate the influence of external diffusion.
The activation energy of Pb and Ag is determined to be
26.5 and 26.8 kJ·mol−1 and the leaching rate can be ex-
pressed by Eqs. (9) and (10), which is a semi-empirical
mathematical model symbolizing the process. The model
can proclaim the leaching mechanism better and describe
actual reaction process by experimental verification.
Acknowledgement
This project was financially supported by the Natural
Science Foundation of Shandong Province, China (No.
ZR2010EL006); High Education Science Technology Pro-
gram of Shangdong Province (No. J12LA04).
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