Hydrometallurgy 143 (2014) 54–59

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Hydrometallurgy
journal homepage: www.elsevier.com/locate/hydromet

Gold recovery from copper anode slime by means of magnetite

nanoparticles (MNPs)
R. Ranjbar a,⁎, M. Naderi a, H. Omidvar a, Gh. Amoabediny b,c
a
Department of Mining and Metallurgical Engineering, Amir-Kabir University of Technology, 424, Hafez Avenue, P.O. Box 15875-4413, Tehran, Iran
b
Department of Chemical Engineering, School of Engineering, University of Tehran, Tehran 14174, Iran
c
Research Center for New Technologies in Life Science Engineering, University of Tehran, Tehran, Iran

a r t i c l e i n f o a b s t r a c t

Article history: Despite cyanidation currently being the conventional gold recovery process, researchers are looking for alternative
Received 18 February 2013 methods for the recovery of gold from its sources without using cyanide. The current work attempts to study the
Received in revised form 13 January 2014 recovery of gold from copper anode slime by means of a novel process utilizing magnetite nanoparticles (MNPs).
Accepted 14 January 2014
In this process, MNPs were first synthesized by the co-precipitation method, and the characterization of the
Available online 22 January 2014
product was then carried out using the X-ray diffraction (XRD), transmission electron microscopy (TEM), and
Keywords:
vibration sample magnetometer (VSM) methods.
Recovery of gold Thiourea solution was employed as leachant. All the gold content of copper anode slime was dissolved in thiourea
Magnetite nanoparticles (MNPs) solution and a positive complex of gold and thiourea was obtained as a result. At a pH value higher than the pH of
Copper anode slime point of zero charge (PZC), the nanoparticles (NPs) were added to the gold solution. The gold complex adsorbed
Adsorption on the NPs due to their negative surface charge. At the last stage, ammonia was added to the gold-attached NP
Desorption suspension and gold was consequently precipitated in metallic form. The results obtained from the method
indicate the high efficiency of the method for the recovery of gold from copper anode slime.
© 2014 Elsevier B.V. All rights reserved.

1. Introduction
In the conventional method of copper extraction from its ores and sec-
ondary source, at the electrorefining stage, only copper and electropositive
metallic impurities such as iron, zinc, and lead are solved as ions and depos-
ited on anode. At the above mentioned stage, impurities such as gold, silver,
selenium, and tellurium, which are known as the anode slime, remain intact
and fall down as the anode corrodes gradually (Abdollahy and Shafaei,
2004). However small quantity of these metals is present in the slime, the
extraction process is advantageous due to the high value.
Zinc–dust cementation (Miller et al., 1990) carbon adsorption
(Fletcher et al., 2006; Syed, 2012; Sun et al., 1996), solvent extraction
(Luo et al., 2006; Syed, 2012; Wan and Miller, 1986), ion exchange
(Hubicki et al., 2006; Mooiman and Miller, 1991; Syed, 2012), and
recently, separation with nanoparticles (NPs) (Kim et al., 2007;
World Gold Council, 2001; Eskandari and Shariati, 2011) are among
the methods that have been employed for the recovery of precious
metals from their solutions.
The recovery of gold from waste is more appealing than that of other
metals. According to the World Gold Council, the demand for gold has
had an increasing trend during the last decade (World Gold Council,
2001). This increase is not only due to the increasing demands of the
jewelry market but also due to the increasing demands for gold in
industrial as well as medical applications. Several methods, such as
⁎ Corresponding author.
methods using resin adsorption (Donia et al., 2007; Nguyen et al.,
2010) or activated carbons, have been investigated for the recovery of
gold from slimes, waste water, and other sources.
Activated carbons are carbonaceous materials with a well-developed
porous structure consisting of hydrophobic graphene layer surface and
hydrophilic surface functional groups. These characteristics turn them
into efficient adsorbents, catalysts, and catalyst supports (Bansal et al.,
1988; Jia and Demonopolous, 2003). Hydrometallurgical processes
have been employed by many researches for extraction of gold from
anodic slime (Elkin and Tremblay, 1964; Hoffmann, 1991; Morrison,
1963; Rice, 1988; Subramanian et al., 1980). Another research work
was conducted as green technology to recover gold from non-metallic
secondary sources. The method employed in the research was based
upon heating the scrap material along with using an “eco-friendly” or
a “green” reagent (Syed, 2006).
Nowadays, NPs, nanomembranes, and nanopowders are used for
detection and removal of chemical and biological substances including
metals (e.g. cadmium, copper, lead, mercury, nickel, and zinc), nutrients
(e.g. phosphate, ammonia, nitrate, and nitrite), cyanide, organics, algae
(e.g. cyanobacterial toxins), viruses, bacteria, parasites, and antibiotics
(Tiwari et al., 2008). Their size-dependent physical and chemical prop-
erties prove efficient in various useful technologies (Kim et al., 2007).
It has been reported that metal ions such as lead, chromium, copper,
silver, and mercury can be removed/collected from diluted aqueous
solutions using TiO2 NPs (Park et al., 2005). Some other studies focused
on separation of iridium ions from aqueous solutions and indium (III)

0304-386X/$ – see front matter © 2014 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.hydromet.2014.01.007
 R. Ranjbar et al. / Hydrometallurgy 143 (2014) 54–59
Fig. 1. XRD results for NPs.
from environmental samples by nano-Al2O3 and nano-sized titanium
dioxide respectively (Zhang et al., 2009, 2012). A few researchers
focused their studies on the recovery or extraction of gold from wastes
or copper anode slimes. One of such studies employed ZnO nanopowders
for collection of gold from wastewater (Park et al., 2005).
In recent years, magnetite nanoparticles (MNPs) have gained an
increasing interest because of their potential applications; instances
include their uses for cell separation (Jing et al., 2007), magnetic reso-
nance imaging (Lee et al., 2006), drug delivery systems (Neuberger
et al., 2005), protein separation (Gu et al., 2006), and cancer treatments
through hyperthermia (Ito et al., 2003).
Among the various NPs, nanomagnetites are particularly appeal-
ing for the above-mentioned purposes and due to two main reasons:
1. they behave superparamagnetically and present a relatively high
magnetic saturation and high magnetic susceptibility and biocompati-
bility; and 2. in comparison to the magnetic transition metals such as
cobalt, iron and nickel (Ferreira et al., 2010), they are less sensitive to
oxidation. In a research work, mesoporous silica-coated magnetite
nanoparticles (SCMNPs) have been used for a highly efficient removal
and recovery of Hg from water; in this work, the size of nanomagnetites
was around 50 nm, and a maximum efficiency of about 90% was reported
(Hakami et al., 2012). In another research work, adsorption of arsenic
and chromium by mixed magnetite and maghemite NPs from aqueous
solution with efficiency of about 96–99% under controlled pH condi-
tions was reported (Chowdhury and Yanful, 2010). Another work was
also carried out for on the removal of dichromate anions; in this work,
the size of magnetite NP was about 10 nm (Ozcan et al., 2009).
The current research work employs MNPs for gold recovery. MNPs
were synthesized through the co-precipitation method, and then were
coated by the method introduced by Stöber et al. (1968). TEM, XRD,
and VSM were further used to characterize the synthesized NPs. Next,
NPs were used to adsorb the positively charged complex of gold and
Fig. 2. TEM images for MNPs: A) magnetite B) SCMNPs.
55
thiourea obtained by dissolving gold in thiourea solution. In the last
step, the desorption and regeneration tests were carried out utilizing
ammonia so as to investigate whether this new type of adsorbent was
appropriate and efficient for the recovery of metallic gold.
The novelties of this work, which might be of more interest, are first
the high potential of such nanoparticles for gold recovery even at very
low concentrations; second their reproducibility after several recycling
periods, and third the introduction of a new method for gold recovery
from copper anode slime and other sources with an efficiency of 100%.
2. Experimental
2.1. Materials
The copper slime utilized for the test was obtained from the National
Sarcheshmeh Copper Company in Iran. All chemicals used in the prepa-
ration were procured from Merck (Germany).
2.2. Synthesis of MNPs
The procedure applied for the preparation of SCMNPs was of two
stages: first, the synthesis of the magnetite (Fe3O4) nanoparticles
(MNPs) and then the application of silica coating.
MNPs were first prepared using a slightly modified version of the co-
precipitation method, introduced by Kang et al. (1996).
According to this method, 10.81 g of FeCl 3 ·6H2O and 3.97 g of
FeCl2·4H2O were dissolved in water and HCl solution (37%), respec-
tively. The resultant solutions were then added to deoxidized ammo-
nia aqueous solution under vigorous stirring. The black precipitate,
or MNPs, were rinsed several times by means of a magnet, and were
dispersed in deionized water. Coating was then performed as per a
slightly modified version of a common method introduced by Stöber
et al. (1968). In this method, 100 ml ethanol (pure), 5 ml deionized
water, 8.5 ml ammonium hydroxide (28%), and 1.5 ml TEOS were
stirred for 30 min in 40°C. The resultant substance was a milky solution.
Then, 1 g of nanoparticles was added to silica and stirred for 1 h so as to
coat the magnetite core by silica. Finally, the coated nanoparticles were
rinsed and dispersed in deionized water. It is worth to note that Silica-
coating is appropriate at normal atmosphere. X-ray diffraction (XRD),
transmission electron microscopy (TEM), and vibration sample mag-
netometer (VSM) were further used to characterize the synthesized
MNPs.
2.3. Gold–thiourea solution
Leaching of gold in the copper anode slime is affected by some
elements such as silver, iron, and selenium. Therefore, copper anode
slime was first washed by concentrated nitric acid (65%). 10 ml of
 56 R. Ranjbar et al. / Hydrometallurgy 143 (2014) 54–59

acidic buffer with pH 5 and water and then were re-used for gold
adsorption process.

3. Results and discussion

3.1. Characterization of MNPs

The crystal structure, morphology, and magnetic properties of the

NPs were characterized by XRD, TEM, and VSM, respectively. The XRD
pattern was obtained using a Rigaku RINT-2000 diffractometer using
CuKα radiation (λ = 1.5418 Å). The pattern obtained for the observed
peaks was the same as the standard pattern for magnetite (JCPDS 19-
629); this indicates the inverse spinel structure of the MNPs (Fig. 1).
TEM images for MNPs and SCMNPs were obtained using a Philips,
EM 208 instrument at 100 kV acceleration voltage.
According to the TEM images obtained for MNPs (Fig. 2a) and
SCMNPs (Fig. 2b), it can be concluded that the NPs are almost spherical
with average diameters of around 8 and 15 nm, respectively (determined
Fig. 3. Room temperature VSM magnetization curves for Fe3O4 NPs and SCMNPs.
by a statistical measurement and averaging 50 particles, with particle
size distribution of about 1.2).
The size reduction results in an increase in superparamagnetic prop-
concentrated nitric acid was added to 5 g of copper anode slime, and the
erties (Rice, 1988). In the current paper, the least particle size for
obtained mixture was then stirred for 15 min. As a result, gold and resid-
obtaining the best magnetic properties was achieved by optimizing
ual barite was deposited.
the conditions of synthesizing. It is significant that the important
The gold and silver content of the residue was measured after leaching
parameters including type of the base, reaction temperature, stirring
by atomic absorption spectroscopy (AAS), methyl iso-butylketone
speed and time were set in away to have the desired characteristics
(MIBK), and XRF.
for the obtained MNPs. The magnetic behavior of the synthesized
Leaching tests were carried out by thiourea in a 500-ml round
MNPs was characterized using a vibrating sample magnetometer
bottomed flask. Mixing was performed by an adjustable speed stirrer.
(VSM). Fig. 3 presents the results confirming the above statements.
All of the experiments were carried out at ambient temperature. Thio-
As shown in Fig. 3, the curves for both MNPs and SCMNPs exhibit
urea powder, hydrogen peroxide (30%) (as the oxidizing agent), and
zero remanence and coercivity, demonstrating superparamagnetic
sulfuric acid (98%) (for pH adjustment) were used for gold leaching
property of these particles. Besides, it can be concluded that they are
with thiourea. In the next step, 5 g of the pretreated copper anode
sufficient for magnetic separation with a conventional magnet due to
slime was added to the thiourea solution, and the resulting solution
their high magnetic saturation.
was then stirred for 24 h at 500 rpm. Finally, residue was removed
This property is suitable for industrial applications and is a signif-
from gold thiourea solution by filtration.
icant finding on MNPs. A similar observation has been reported by Zhao
et al. (2008).
2.4. Gold adsorption on to NPs
Fig 3 also shows that saturation magnetization of the Fe3O4 NPs is
about 50 EMU/g at room temperature, while it is 40 EMU/g in the
At this step, MNPs were utilized for recovering gold from the gold-
case of SCMNPs.
containing solution. Since the surface charge of the NPs changes by vary-
This reduction is due to the presence of nonmagnetic silica layers on
ing pH (Faraji et al., 2010), MNPs in ammonia solution were dispersed in
the magnetite particles. A similar magnetic behavior with the same
order to obtain more negatively charged MNPs. NPs were then collected
amount of magnetization for MNPs, which have a similar diameter,
by a magnet. At the next step, 0.1 g of the negatively charged MNPs was
has been reported by Mahdavian and Mirrahimi (2010).
added to 25 ml and 50 ml of the gold–thiourea solutions, and the
The magnetically separated MNPs and SCMNPs are not permanently
solutions were stirred for 15 min using a mechanical stirrer. Gold-
magnetized, and can be re-dispersed without any signs of re-aggregation
adsorbed MNPs were collected by applying a magnetic field. The
when the external magnetic field is removed. This property is due to the
thiourea solution lost its gold color at this stage. MIBK and AAS were
super-paramagnetic NPs. Both MNPs and SCMNPs show similar charac-
conducted on the remaining solution to determine the amount of gold.
teristics. Because of the higher saturation magnetization for MNPs rela-
tive to SCMNPs, and working in aqueous phase, it can be concluded
2.5. Gold desorption from NPs
that Fe3O4 NPs are most suitable for gold recovery from solution.
By mixing 10 ml of ammonia and 30 ml of ionized water, a solution
with a pH of over 8 was obtained. Then, 1 g of the gold-adsorbed MNPs 3.2. Anodic slime characterization
was added to the solution and was stirred for 15 min by a mechanical
stirrer. Hence, metallic gold and MNPs were precipitated. At last, by Table 1 presents the chemical composition of the delivered copper
applying a magnetic field, NPs were separated from the black sediment anodic slime from the National Sarcheshmeh Copper Company before
containing gold. After desorption process, MNPs were washed by an and after the washing process with nitric acid obtained by XRF and

t1:1 Table 1
t1:2 Chemical analysis of the main elements of the delivered copper anode slime.

t1:3 Elements CuO SeO2 Ag2O Sb2O3 BaO PbO SrO Au Re IrO2

t1:4 Before washing (wt %) 5.4 10.2 4.8 2.58 34.1 3.81 0.98 0.12 0.028 0.12
t1:5 After washing (wt %) 0.128 0.42 0.2 3.72 64.7 3.81 1.82 0.12 0.03 0.12
t1:6 After dissolving (wt %) 0.128 0.42 0.2 3.72 65 3.81 1.82 ~0 0.04 0.12
 R. Ranjbar et al. / Hydrometallurgy 143 (2014) 54–59 57

t2:1 Table 2 Table 3 t3:1

t2:2 The amount of gold in thiourea solution. The amount of gold remained in thiourea solution after gold recovery. t3:2

t2:3 pH The amount of dissolved gold (ppm) The percentage of dissolved gold (%) pH The remained gold in solution Absorbed gold (%) t3:3

t2:4 1.2 66 ~100 (ppm) % t3:4

t2:5 1.4 66 ~100
1.2 b0.01 0≈ N99.999 t3:5
1.4 b0.01 0≈ N99.999 t3:6

was precipitated (Farinha et al., 1992; Hilson and Monhemius, 2006;

MIBK. As shown, the gold and silver contents in the slime have been örgul and Atalay, 2002).
0.12 and 5 wt.%, respectively.
þ −
It can be inferred from the results that a large amount of copper, 2Au CSðNH2 Þ2 2
þ 2OH →Au þ 2CSðNH2 Þ2 þ H2 O þ ½ O2 : ð1Þ
selenium, and silver were eliminated.
Thiourea can also be dissociated according to reaction 2.
3.3. Gold containing thiourea solution characterization
þ −
CSðNH2 Þ2 b ¼ NNH4 þ SCN : ð2Þ
Table 2 shows the amount of dissolved gold in the thiourea solution
(dissolution efficiency) in ppm scale. Furthermore, thiourea can be hydrolyzed, and have reaction with
According to Farinha et al. (1992), the maximum amount of gold dis- H2O according to the following reaction:
solved in thiourea solution can be obtained with thiourea to hydrogen
peroxide ratio of 2 and pH value of between 1 and 1.5. The results CSðNH2 Þ2 þ H2 Ob ¼ NCOðNH2 Þ2 þ H2 S: ð3Þ
obtained also confirm this fact that under the following leaching condi-
tions, the gold contained in the copper anodic slime dissolved almost Another reversible reaction that may occur is the formation of
completely (99.99%) at CS(NH2)2/H2O2 = 60 (g/l)/30 (g/l) = 2. The formamidine disulfide. Formamidine disulfide oxidizes to produce
tests were carried out at pH values between 1.2 and 1.4. cyanamide, hydrogen sulfide, and elemental sulfur.
þ −
3.4. Adsorption process 2CSðNH2 Þ2 b ¼ NNH2 ðNHÞCSSCðNHÞ:NH2 þ 2H þ 2e ð4Þ

Gold in thiourea solution is in the form of the Au(CS(NH2)2)+
2
positive complex. The adsorption process involves coulombic attraction
between the negatively charged NPs and the positive complex. Around
the isoelectric point, Fe-OH is the dominating surface species for MNPs.
However, the dominating sites can be altered in the presence of H+ and
OH− ions from dissolved acids or bases. Under the pH(PZC), the dominat-
ing surface species changed to Fe-OH+2, and the surface charge of the
particles became positive. Increasing pH above the isoelectric point
caused formation of Fe–O− and a negative surface charge. Hence, after
dispersing MNPs in ammonia, more negatively charged particles were
obtained due to enhancement of hydroxide ions (Illés and Tombácz,
2006). The obtained pH(pzc) for MNPs was about 6 (Faraji et al., 2010;
Ferreira et al., 2010). Thus, when MNPs were placed in ammonia solu-
tion, Fe–O− formed on the NP surfaces. Upon addition of MNPs to gold–
thiourea solution, a layer of gold complex formed around the MNP
surface, and this layer prevented dissolution of MNPs in the acidic
solution. After adsorption, MIBK was carried out on the remaining
thiourea solution to determine the percentage of gold adsorption.
Table 3 presents the results obtained from the MIBK test. The effect
of time was investigated as well, the results of which are shown in
Fig. 4. It is notable that the adsorption amount of Au-cations on
MNPs increases with time, and Au-cation concentration in the solu-
tion decreases until it disappears or is completely removed from
the solution. This shows the high separation potential and efficiency
of the synthesized superparamagnetic magnetite nanoparticles.
Morphology of gold on the surface of NPs was studied by TEM at
100 kv (Fig. 5).
TEM images show spherical NPs with an average diameter of around
25 nm, demonstrating adsorption of gold onto the magnetite.
NH2 ðNHÞCSSCðNHÞ:NH2 b ¼ NNH2 CSNH2 þ Sulfinic compound ð5Þ
0
Sulfinic Compound→CNNH2 þ S : ð6Þ
Also, to confirm the elemental gold precipitation, XRD test was
carried out on the residue; the results of the test without any noise
filtration and numerical normalization are shown in Fig. 6. The XRD dif-
fraction pattern shows two diffraction peaks related to gold which dem-
onstrates pure gold particle precipitates. It can be concluded from the
seven observed diffraction peaks emphasizing the magnetite structure
that they are recovered without any change. Hence, they can be used
for several times.
Finally, after washing the precipitate with deionized water, gold was
separated from MNPs by applying a magnetic field. In fact, the XRD anal-
ysis of results shows that there are no metallic impurities besides gold.
They also indicate the successful recovery of gold.
3.6. MNPs recycling
After desorption process, MNPs were separated from gold by apply-
ing magnetic field. MNPs were then washed by acidic buffer with a pH of
about 5 as well as water to remove all impurities. The obtained recycled

3.5. Desorption study

At this step, for the desorption process, ammonia solution was added
to the magnetite-gold NP suspension, and as a result, a black sediment
containing gold and MNPs was deposited. The gold complex was stable
in the pH range from 1 to 1.5, and therefore, by adding ammonia to NPs,
pH reached a level of over 8, and the complex disassociated according to Fig. 4. The changes in adsorption of gold cation with residence time at room temperature
the following reaction. Therefore, gold along with other components and pH 9.
58 R. Ranjbar et al. / Hydrometallurgy 143 (2014) 54–59
Fig. 5. TEM images of gold adsorbed on MNPs.
products were used for separation of gold complex. The adsorption
capacity (qe, mgg−1), i.e. the amount of gold adsorbed at equilibrium,
was calculated by the following equation (Hakami et al., 2012):
qe ¼ VðC0 −Ce Þ=m
where C0 is the initial gold concentration in solution (mg l−1), Ce is the
equilibrium concentration (mg l−1) after adsorption, V is the solution
volume (l) and m is the mass of NPs adsorbent (g). Fig. 7 presents the
results pertaining to separation of gold. The results reveal that the
recycled products have still preserved their capability for separation.
The capacity of gold adsorption is reduced about 2–4% during each
recycling period which may be due to gold complex or thiourea not
being released from adsorption sites between cycles; this actually
suggests the stability of superparamagnetic MNPs after separation and
recycling procedure. It can also be concluded that the electrostatic
(physical) bonding between gold complex and MNPs is the most impor-
tant cause of easy separation of gold from the surface of MNPs and
capacity retention of MNPs.
4. Conclusions
1. MNPs were prepared using the co-precipitation method, and the
silica-coating process was carried out according to the Stöber
method (1968). NP characterization suggested that the process
produced a uniform structure and uniform properties. TEM im-
ages illustrated that the particle size for MNPs and SCMNPs was
about 8 and 10 nm, respectively. Moreover, both of them show
Fig. 6. XRD results for the precipitate.
superparamagnetic properties according to their magnetization
curves.
2. Due to various reasons such as higher saturation of magnetization of
MNPs relative to SCMNPs, working in aqueous phase as well as eco-
ð7Þ nomic reasons, it can be concluded that Fe3O4 NPs are the most suit-
able and profitable method for the recovery of gold from the solution.
3. Gold solution was prepared using thiourea as solvent. Gold ions
appeared in the solution in the Au(CS(NH2)2)+ 2 form.
4. Gold adsorption onto the NPs occurred according to the electrostatic
attraction between the negative charged MNPs and positive complex
of gold.
5. Gold-attached MNPs were successfully prepared in an aqueous solu-
tion with pH control. In fact, this was achieved by using copper anode
slime as Au source. Au ions attached the MNP surfaces as per the
ionic surface charge force as well as the zeta potential or pH(pzc) of
the MNPs.
6. Au complex adsorbed on MNPs could be desorbed effectively using
ammonia for increasing pH, and this is because of the low stability
of gold complex in alkaline solution.
7. The capacity of gold adsorption was reduced about 2–4% during each
recycling step and this shows the stability of MNPs after separation
and recycling process.
8. The results suggest that MNPs can be an effective alternative to
conventional adsorbents for the adsorption of gold complex from
Fig. 7. The changes in capacity of MNPs for adsorption of gold complex with residence time
and recycled sample (Recy) at room temperature and pH of over 8.
 R. Ranjbar et al. / Hydrometallurgy 143 (2014) 54–59
its solution at high recovery efficiency of about 100% and in a very
short time.
9. The advantage of MNPs is their ease of separation by an external
magnetic field and possibility of simple recovery after washing
with acidic aqueous solution and water. The method for synthesis
of MNPs and gold collection process addressed in this work is viable
for obtaining gold with high purity from anode slime and other
secondary sources.
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