Resources, Conservation & Recycling 141 (2019) 284–298

Contents lists available at ScienceDirect

Resources, Conservation & Recycling

journal homepage: www.elsevier.com/locate/resconrec

Recovery of precious metals from electronic waste and spent catalysts: A T

review
Yunji Dinga, Shengen Zhanga, , Bo Liua, Huandong Zhenga, Chein-chi Changb, Christian Ekbergc
⁎

a
Institute for Advanced Materials and Technology, University of Science and Technology Beijing, Beijing 100083, PR China
b
Department of Engineering and Technical Services, District of Columbia Water and Sewer Authority, Washington, D.C., 20032, USA
c
Nuclear Chemistry and Industrial Material Recycling, Department of Chemistry and Chemical Engineering, Chalmers University of Technology, Gothenburg 41296,
Sweden

ARTICLE INFO ABSTRACT

Keywords: Precious metals are widely applied in many industry fields due to their excellent corrosion resistance, good
Precious metals electrical conductivity and high catalytic activity. However, the reserves of precious metals falls short of the
e-Waste production globally. The rapid generation of end-of-life products has become the significant resources of pre-
Spent catalysts cious metals. Among these products, electronic waste (e-waste) and spent catalysts are more concentrated since
Recovery
they account for over 90% of precious metals in industry. This article provides an overview of various tech-
Environmental impacts
nologies on the recovery of precious metals from e-waste and spent catalysts. It shows that recycling technol-
ogies have been significantly improved in recent years. The recycling processes have transferred from leaching
by aqua regia, cyanide and chlorine in acid solution to less pollution agents leaching. Environment-oriented
technologies have been raised great attention in precious metals recycling. The advantages and environmental
impacts of these recycling technologies have been discussed in detail. However, there are still some challenges
for future promotion. In order to achieve the environment-friendly and sustainable recycling for precious metals
with high recovery rate, several considerations have been proposed.

1. Introduction
Precious metals (PMs) are widely applied in the various fields due to
the distinct physical and chemical properties, such as catalytic activity,
good electrical conductivity and corrosion resistance (Zientek and
Loferski, 2014; Richards, 2006). The most significant fields are elec-
tronics and catalysts industry, which consume over 90% of precious
metals in industry (The detailed information is shown in supplementary
materials).
In electronics industry, gold and silver are used as contacts, bonding
wires and switches, while palladium is used in computer hard disk
drives (Diaz et al., 2016). The content of main PMs in typical electronics
is shown in Table 1 (Zhang et al., 2017). In 2015, global demand for
gold, silver and palladium in the field of electronics were 254 tonnes,
12,816 tonnes and 40.18 tonnes, respectively (USGS, 2017). In recent
years, huge quantities of electronic waste (e-waste) have been gener-
ated from the electronics end of life (Kumar et al., 2017). By 2016, the
world has generated about 44.7 million tonnes (Mt) of e-waste (Yang
et al., 2017; Balde et al., 2017). Therefore, e-waste has gradually be-
come significant source of precious metals. For example, according to
National Institute for Materials Science (NIMS), over 6800 tonnes of
gold (16% of the world reserves) and 60,000 tonnes of silver (22%)
were found in urban mines (NIMS, 2015). However, only about 20% of
e-waste was recycled through appropriate channels.
In catalyst industries, precious metals are widely used as the active
components. The main catalysts are used in automobile emission pur-
ification, oil-refining, chemical engineering, pharmaceuticals and fine
chemicals. Many researchers have been studying substitute materials to
reduce the dosage of precious metals in products (Deng et al., 2014).
However, the net PGMs (platinum group metals) consumptions are still
very high due to the increasing automobiles and other catalyst in-
dustries. About 65% of palladium (182.65 tonnes), 45% of platinum
(98 tonnes), and 84% of rhodium (25.6 tonnes) were used in catalytic
converters. The concentration of precious metals varied from 200 ppm
to 100% in different kinds of catalysts (Dong et al., 2015). In addition,
the carrier materials of catalysts were also in different types, which
made their recycling difficult. The basic information of catalysts used in
chemical industries and automobiles is shown in Table 2.
However, the concentration of precious metals in Earth’s crust is
extremely low, and most of them are below 0.01 ppm. Moreover, their

⁎
Corresponding author.
E-mail address: zhangshengen@mater.ustb.edu.cn (S. Zhang).

https://doi.org/10.1016/j.resconrec.2018.10.041
Received 1 August 2018; Received in revised form 18 September 2018; Accepted 30 October 2018
Available online 06 November 2018
0921-3449/ © 2018 Elsevier B.V. All rights reserved.
Y. Ding et al. Resources, Conservation & Recycling 141 (2019) 284–298

Table 1
The content of precious metals in typical electronics (Zhang et al., 2017). AC: average content.
PM Mobile phone PC Flat screen or TV monitor Laptop
(mg/unit)
Range AC Range AC Range AC Range AC

Ag 232∼319 261 1348–11408 6378 450∼575 515 249–437 343

Au 24.1∼29 26.1 – 92.7 110∼200 161 104.5–219.8 160.8
Pd 8.7∼14.5 11.6 – 39.9 40∼44 42 – 40.2

Table 2
PMs catalysts used in the chemical industries and automobiles (Dong et al., 2015).
Application field Catalyst support Active components PM contents Lifespan/year

Automotive Catalysts Cordierite monolith ceramic pellets Pt/Rh; Pt/Pd/Rh; Pt 0.1–0.3% > 10
Diesel particulate filter SiC or cordierite Pt/Pd 0.1-0.5% > 10
Oil-refining Reforming Al2O3 Pt; Pt/Re, Pt/Ir 0.2–1% 1-12
Isomerisation Al2O3, zeolites Pt; Pt/Pd
Hydrocracking SiO2, zeolites Pd; Pt
Gas to liquid Al2O3, SiO2, TiO2 Co+(Pt; Pd; Ru; Re)
Chemical engineering Nitric acid Gauzes PtPdRh 100% 0.5
H2O2 Al2O3 Pd 0.3-0.5% 1
HCN Al2O3 or gauzes Pt; Pt/Rh 0.1%; 0.5% 0.2–1
PTA Carbon granules Pd 0.2-0.3% 0.5–1
VAM Al2O3, SiO2 Pd/Au 1–2% 4
EO Al2O3 Ag 10-15% 1-5
KAAP Activated carbon Ru – 1-3
Homogeneous Oxo Alcohols Homogeneous Rh 500–1000 g/t 1–5
Acetic acid Rh; Ir/Ru
Fine Chemicals Hydrogenation Activated carbon Pd; Pd/Pt Ru; Rh; Ir 2–10% 0.1–0.5
Oxidation
Debenzylation

distributions are not in balance, especially PGMs (Zhang et al., 2017).
98.5% of PGMs or more are found in South Africa, Russia, Zambia and
United States. PGMs are seriously constrained to most countries. For
example, only 2.5∼3 tonnes of PGMs were produced from natural re-
source in China annually (Dong et al., 2015), but demands for Pt and Pd
were over 141 tonnes, respectively. Therefore, it is necessary to recycle
PMs from end-of-life products, realizing the sustainable development of
precious metals (Izatt et al., 2014; Lu and Xu, 2016).
By 2016, only 20% of e-waste was recycled through appropriate
channels, in which about 71.2 tonnes of gold, 3276 tonnes of silver and
14 tonnes of palladium were recovered (Balde et al., 2017). For spent
catalysts, about 30% of PGMs were recovered, namely 34 tonnes of Pt,
61 tonnes of Pd and 7.2 tonnes of Rh (USGS, 2017). It indicated that
most e-waste and spent catalysts flowed into informal recycling system
or even disposed in landfills (Cao et al., 2016). E-waste and spent cat-
alysts contain precious metals, along with many hazardous materials
(e.g. heavy metals, flame retardants, organic substances) (Gu et al.,
2016). These hazardous materials may cause serious pollutions to
ground and water and affect human health (Li et al., 2007; Kohl and
Gomes, 2018). Apparently, it is crucial to recover precious metals from
e-waste and spent catalysts from perspectives of economics and en-
vironmental protection (Bigum et al., 2017).
In the early stages, simple and rough processes for precious metals
recycling were widely adopted. For example, recycling precious metals
from e-waste mainly includes manual dismantling, aqua regia leaching,
or open burning. These methods not only have low recovery rate, but
also pollute the environment (Wang and Xu, 2015). For the serious is-
sues, many less-polluted technologies, such as physical separation
pretreatments, smelting in furnaces, non-cyanide leaching, mild
leaching, have been developed over the past two decades (Zhang and
Xu, 2016; Akcil et al., 2015a). Although these technologies have special
advantages, negative effects on recovery efficiency and environment
still exist. The recycling technologies in future tend to realize the
maximum recovery of precious metals and minimum environmental
impact.
Therefore, it is necessary to summarize the current status of re-
covery technologies for precious metals from e-waste and spent cata-
lysts. This review presents the possible solutions associated with the
recycling of the precious metals. Advantages and environmental im-
pacts of these recycling technologies have been discussed in detail.
Meanwhile, the outlook on further development of precious metals
recovery is presented. Recovery of precious metals through bioleaching
or biosorption methods were not included in this review, as well as
separation and refining processes.
2. Recovery of PMs from e-waste
Technological innovation and market demand accelerate the update
of electronic applications and shorten their average lifespan. As a result,
e-waste has become one of the fastest increasing waste streams
worldwide (Kumar et al., 2017). Extensive literatures have reported
precious metals recycling from e-waste (Tanskanen, 2013; Rocchetti
et al., 2013; Khaliq et al., 2014). Various recycling technologies have
developed in the latest 20 years, and many of those have already been
employed in the industrial scale (Syed, 2016; Işıldar et al., 2018).
2.1. Mechanical pretreatment
Mechanical processing is also necessary before recycling precious
metals from e-waste. (Yoo et al., 2009). The mechanical pretreatment
includes three main steps, (1) dismantling, (2) size reduction and (3)
physical separation. Different components and devices can be selec-
tively separated by manual or automatic dismantling, such as metals,
plastics, ceramics, capacitors, batteries, LCDs, and PCBs. This process
can remove the hazardous components and increase the concentration
of precious metals (Cui and Forssberg, 2003). Then shredders and
hummer mills were used to rip and grind the waste (Dalrymple et al.,
2007). The extent of size reduction depends on following recycling
technologies. For example, the waste PCBs were cut into 4 × 4 cm
pieces and then directly smelted in Umicore, while hydrometallurgical

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processes and physical separation always required fine particles for
high leaching rate of valuable metals (Duan et al., 2009). It was found
that metals can be completely liberated from waste PCBs when the
particle size was less than 2.0 mm (Zhang and Forssberg, 1997). Various
separation methods have been developed for the physical separation of
metals and plastics, such as gravity separation, magnetic separation,
electrostatic separation and eddy-current (Li and Xu, 2010; Wu et al.,
2008; Richard et al., 2011). The concentration of precious metals in
metal fractions has enhanced after mechanical pretreatment. The re-
moval of plastic can reduce or eliminate the generation of dioxins.
However, approximate 10–35% of valuable metals will loss during
mechanical processing due to the insufficient liberation, generation of
fines, and inefficient separation (Tuncuk et al., 2012). After mechanical
pretreatment, the enriched metal fractions are further treated by dif-
ferent metallurgical technologies for the recovery of precious metals.
2.2. Pyrometallurgical process
Pyrometallurgical processes are beneficial to segregate and con-
centrate precious metals from e-waste. The typical e-waste pyr-
ometallurgical routes include smelting in furnaces and alkali fusion.
State-of-the-art smelters and refineries can recover precious metals and
reduce environmental impact arising from large quantities of e-waste.
Precious metals are concentrated in the blister copper or lead bullion,
and then processed by acid leaching or electro-refining. Alkali fusion is
another alternative approach to remove organic compounds below
400 °C, which can avoid the formation of dioxins and furans.
2.2.1. Smelting in furnaces
Open burning in the blast furnace is always employed in the in-
formal recycling sectors. The elements form metal phase that contains
60–80% copper, as well as precious metals, lead, tin, antimony, nickel
and so on (Kang and Schoenung, 2005). The recovered black copper
was further purified by electro-refining or directly leached by H2SO4.
This process generates large amounts of hazardous gases, wastewater
and residues. The improper disposal through open burning pose serious
risks to the environment and human health. Besides, it is difficult to
recover other valuable metals except copper and precious metals.
Fortunately, pyrometallurgical processes have been significantly
improved with the consideration of maximum recovery of metals and
minimum pollution. Pyrometallurgical technologies have already suc-
cessfully applied in industry. Some typical industrial applications were
shown in Table S4 (Seen in supplementary materials). Generally, the
flow sheet of e-waste recycling by smelting is shown in Fig. 1. Before
smelting, e-waste usually needs to be treated through classification,
dismantling, shredding/grinding and sorting of metals and plastics (Lee
et al., 2012). E-waste recycling through black copper smelting is fea-
sible and economic. For example, 250,000 tonnes of different waste are
treated annually in Umicore, of which e-waste covers up to 10 wt.%.
The main processing steps contain copper smelting in Isasmelt furnace
and lead blast smelting, the copper-leaching and electro winning plant,
and precious metals refinery. The recovery rates of precious metals are
over 95% (Hagelüken, 2006). Another application for pyr-
ometallurgical process to recover metals from e-waste was at Boliden’s
Rönnskär smelter (Cui and Zhang, 2008). E-waste was firstly ground
into powder. Then they were fed into Kaldo furance to upgrade precious
metals in copper. Then it was sent to the converter to remove im-
purities. Precious metals were finally recovered by electro-refining
process (Ek and Olsson, 2005; Lennartsson et al., 2018). More than
120,000 t of e-waste were treated in Boliden every year (Cui and Zhang,
2008).
Although precious metals have been recycled via copper and/or
lead smelting, their recovery are still technologically challenging (Reck
and Graedel, 2012). E-waste is composed of 60 different substances and
the concentrations of precious metals are diverse with different kinds of
e-waste. The elements and their concentrations in e-waste are
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Resources, Conservation & Recycling 141 (2019) 284–298
Classification
Dismantling
Crushing & separation
Flux Other raw materials
PCBs
Smelting
PCBs
Blister copper Dust
PCBs
Electrorefining
Cathode copper Anode slime
Extraction & separation
Fig. 1. General flow sheet of precious metals recycling from WEEE by tradi-
tional smelting process.
significantly different with ore concentrates, which lead to a compli-
cated reaction system. Currently, the distribution behavior of associated
elements (e.g. Pb, Sn, Se, Te, As, Sb, Pd, Ag and Au) in copper ores
during primary copper smelting has been reported (Shuva et al., 2016).
However, the related thermodynamics data of trace elements (including
precious metals), or even common elements during secondary copper
processing are not available (Ghodrat et al., 2017a). The plant pro-
duction capacity has significant influence on the internal rate of return
of the process and cost to benefit ratio due to its large capital invest-
ment. It is at least 30, 000 tonnes/annum for the plant capacity of e-
waste recycling through copper smelting that can be economically vi-
able (Ghodrat et al., 2016). Therefore, advanced pyrometallurgical
technologies are limitedly employed in large enterprises in some de-
veloped countries.
E-waste processing through secondary copper smelting has sig-
nificantly higher environmental impacts than secondary copper re-
cycling without adding e-waste (Ghodrat et al., 2017b). For example, its
emission of heavy metals are 3–100 times than the later process.
Moreover, compared with 2.9 kg e-waste per dollar of capital invest-
ment for the electrochemical recovery process, the black copper
smelting process processes 1.3 kg per dollar, which is more cost-con-
suming (Diaz and Lister, 2018).
2.2.2. Alkali smelting
An alternative method of separating plastics and ceramics (Al2O3,
SiO2, etc.) is alkali fusion by using molten-salt-oxidation. Pb, Sn, other
amphoteric metals, and ceramics can react with molten alkali, which
forms soluble molten salt. Moreover, hydrocarbon chains can be broken
down by molten alkaline compounds. While copper and precious metals
remained in the solid residue and then they were separated and re-
covered by simple leaching.
Flandinet et al. (2012) recovered copper-rich metallic fraction from
waste PCBs by using molten KOH-NaOH at 300 °C under 2 L/h of Ar.
After treatment in molten KOH-NaOH and followed by washing in
Y. Ding et al.
Fig. 2. Products after washing by ultrapure water, (left) metallic fraction and (right) brown powder (Flandinet et al., 2012).
ultrapure water, a metallic fraction and a brown powder were re-
covered, as illustrated in Fig. 2. All precious metals were recovered in
the metallic fraction, with no dissolution or melting phenomena. The
similar result was also achieved by Stuhlpfarrer et al. (2016).
By using NaNO3-NaOH as fluxing agent, Guo et al. (2015) developed
an alkali fusion-leaching-separation process to recover metals in cru-
shed metal enrichment (CME) originated from waste PCBs. The re-
cycling flow sheet was shown in Fig. 3. Amphoteric metals, such as Sn,
Pb, Zn and Al, were oxidized and converted to soluble salts in the fusion
process. The residue was leached by H2SO4 to recover Cu. Precious
metals could not be dissolved by H2SO4 and were enriched in the
leaching residue. The recycling rates of Sn, Zn, Pb, Al and Cu were
96.85% 91.28%, 78.80%, 98.39% and 97.88%, respectively, under
optimal conditions of the fusion processes (mass ratio Na-
NO3:NaOH:CME of 3:4:1, fusion temperature of 500 °C, fusion time of
90 min). Meanwhile, the enrichment ratio precious metals was over 10.
Fig. 3. Flow-sheet of alkaline fusion–leaching–separation process (Guo et al., 2015).
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Resources, Conservation & Recycling 141 (2019) 284–298
2.3. Hydrometallurgical process
Compared with pyrometallurgical processes, hydrometallurgical
method has the advantages of relatively low capital cost, low tem-
perature condition and high metal recoveries with their suitability for
small scale applications. These advantages drive the development of
hydrometallurgical processes for precious metals recovery (Ghosh et al.,
2015).
Many leaching systems are exploited for extraction of precious
metals from e-waste (Akcil et al., 2015a; Cui and Anderson, 2016). Due
to the ability to form stable complexes, cyanide, thiourea, thiosulfate
and halide are widely used in the leaching of precious metals. Recovery
of precious metals from e-waste is well-established, not only in the la-
boratory scale but also industrially practiced (Shibata and Matsumoto,
1999; Quinet et al., 2005; Ha et al., 2010). Main features of these
leaching systems are summarized in Table 3 (Tuncuk et al., 2012).
Cyanide and thiosulfate leaching was conducted in the alkaline condi-
tions, while thiourea and halide leaching were in acid solution. For a
Y. Ding et al. Resources, Conservation & Recycling 141 (2019) 284–298

Table 3
Main features for leaching gold from e-waste by different reagents (Tuncuk et al., 2012).
Lixviants Reagents Chemistry reactions Species and stability Conditions

− − − −
Cyanide CN , Air (O2) 4Au+8CN +O2+2H2O = 4Au(CN)2 +4OH Au(CN)2− logK = 38.3 E° = 0.67V
Ag(CN)2− logK = 20.3 pH > 10, 25 °C
Thiosulfate S2O32−, NH3, Cu 2+ 2
4Au+8S2O3 +O2+2H2O = 4[Au(S2O3)2] 3−
+4H2O Au(S2O3)23− logK = 28.7 E° = 0.274-0.038V
Ag(S2O3)23− logK = 13 pH 8-10, 25 °C
Thiourea CSN(NH2)2, Fe3+ 2Au+4CS(NH2)2+2Fe3+ = 2Au(CS(NH2)2)++2Fe3+ Au(CS(NH2)2)+ logK = 22 E° = 0.38V
Ag(CS(NH2)2)+ logK = 13 pH 1-2, 25 °C
Halide Cl/Cl2, Br−/Br2, I−/I2 2Au+11HCl+3HNO3 = 2HAuCl4+3NOCl+6H2O AuCl4− logK = 29.6 E° = 1.00V
pH < 4, 25 °C

Table 4
The leaching rate of precious metals from e-waste by various lixiviants.
Materials Leaching conditions Recovery rate References

Reagents Temp. (°C) Time (h) S:L ratio

PCBs I2 0.1%, I−1.0%, H2O21.5%, pH=7 25 4 1:10 Au 97.5% Xu et al. (2009)

PCBs Copper was removed before experiment. Iodine 35 4 3:20 Au 99.98% Sahin et al. (2015)
3%, H2O21%, pH=7
PCBs Thiourea 24 g/L, Fe3+ 0.6%, H2SO4 0.5 mol/L, 25 2 _ Au 89.67%; Ag 48.3% Li et al. (2012a,b,c,d,e)
particle size 100 mesh
PCBs (NH4)2S2O3 0.1 mol, CuSO4 40 mmol, pH 10-10.5, 25 8 3:50 Au 57.6%; Tripathi et al. (2012)
pulp density: 10 g/L
PCBs thiosulfate 72.71 mmol, Cu2+ 10.0 mmol, NH3 40 5min — Au 91% Ha et al. (2014)
0.266 mol
PCBs thiosulfate 20 mmol, Cu2+ 0.12 mmol, NH3 0.2 25 2 1:15 Au 98% Ha et al. (2010)
mol
ICs Thiourea 20 g, ferric sulfate 2.6 g, H2SO4 3.6 mol/ 20 3 1:100 Au 69.36%, Ag100% Lee et al. (2011)
L
Aqua regia 5-40% 27 1 1:100 Au 100%, Ag 88.51%
NH3 5-30%, 27 1 1:100 Au 12.76%, Ag 100%
(NH4)2S2O8 45.6 g
H2SO4 0.001-6 mol/L 27 3 1:75-200 Au 6.05%, Ag 90.37%
Waste cell phones e-waste 7 g, SC(NH2)2 0.2 mol, HCl 0.5 mol, FeCl3 25 2 — Au 54.81%, Ag 20.72%, Pd Diaz et al. (2016)
0.1 mol 29.6%
Waste PCBs H2O2(30%) 20 ml, H2SO4 20 ml 25 2 1:4 Au 98.75% Zhu and Gu (2002)
Waste PCBs HNO3 1 mol/L 25 96 ∼100% Jadhav and Hocheng
HCl 1 mol/L 25 22 ∼100% (2015)
H2SO4 1 mol/L 25 96 Au ∼0, Ag 32.4%, Pd ∼0
C2H4O2 1 mol/L 25 96 Au < 1%, Ag 13.2%,
Pd < 1%
C6H8O7 1 mol/L 25 364 Au < 0.1%, Ag 4.2%,
Pd < 0.5%
Waste PWBs HNO3 20-40%, aqua regia 20%. 80 1.5 1:200 Au 87%, Ag 40%, Pt 23% Luyima et al. (2011)
PCBs Copper was leached out by H2SO4 and H2O2 1st 25 1st3 1:10 1stAu 84.31%, Ag 71.36%, Behnamfard et al. (2013)
before experiment. 2st 63 2st3 Pd 2.13%;
1st SC(NH2)2 20 g/L, Fe3+ 6 g/L, H2SO4 10 g/L 2stAu 6%, Ag 16.48, Pd
2stH2O2 1%, NaClO 10%, HCl 2 mol/L 97.87%
PCBs aqua regia 20 3 1:20 Au 97%, Ag 98%, Pd 93% Park and Fray (2009)
Copper anode slime from e- NaClO3 3.75 g/L, NaCl 0.02 mol/L, H2SO4 80 3 1:5 Au 98.1% Ding et al. (2017)
waste 0.5 mol/L
PCBs (1)CuSO4+NaCl (Cu/Cu2+≥1.4) (1) 60 (1) 0.5 — Pd 96.9% Zhang and Zhang (2014)
(2)CuSO4+NaCl (Cu/Cu2+≤0.9) (2) 60 (2) 0.5
Waste PCBs (1)Ag iodine/iodide 1:6 25 (1) 1.5 (1)1:8 (1) Ag 99%, Xiu et al. (2015)
(2)Au, Pd iodine/iodide 1:5; (2) 2 (2)1:10 (2)Au 98.5%, Pd 97.2%
pH=9
Waste memory sticks H2SO4 100 g/L, NaCl 75 g/L, NaClO3 25 g/L 40 2 1:8 Au 99.6% He and Xu (2015)

certain lixiviant, reaction equilibrium constant (K) showed that Au has been discussed in detail in following sections.
complex was more stable than Ag complex. Moreover, the linear cor-
relations of stability constants of Au complexes follow the order
2.3.1. Traditional leaching methods
CN− > Cl− > S2O32- > CSN(NH2)2 (Cui and Anderson, 2016).
Traditional hydrometallurgy processes include cyanide and aqua
Hydrometallurgical leaching of precious metals from e-waste by
regia leaching. Au, Ag and even PGMs can be leached in cyanide so-
various lixiviants has been summarized, as shown in Table 4. Consistent
lution. The leaching efficiency depends on the oxidant dosage, cyanide
with the stability constants, the leaching rates of Au by halide and
concentration, pH, temperature, and other physiochemical features (Xie
cyanide were higher than by thiosulfate and thiourea. Under the proper
et al., 2014). CN− is the active ingredient, which dissolves precious
circumstances, more than 97% of Au can be recovered in aqua regia,
metals by complexation. The optimal pH of cyanide solution is 10–10.5
H2O2-H2SO4, NaClO3-HCl, H2O2, iodine solutions. In most cases, Au
since CN- is stable at pH 10.2. When the pH value is below 8.2, highly
leaching efficiencies were lower than 80% in thiourea, (NH4)2S2O3 and
volatile HCN can be formed, causing serious harmfulness to operators’
SC(NH2)2. Precious metals recovery by hydrometallurgical technologies
health (Marsden and House, 2006). A number of environmental

288
Y. Ding et al.
accidents at various gold mines around the world have raised wide-
spread concern over the use of cyanide as a leach reagent. The accidents
have restricted its use. Several non-cyanide lixiviants (thiourea, thio-
sulfate, halide and etc.) have been proposed as substitutes for recovery
of precious metals.
Aqua regia was used for non-selective dissolution of both base and
precious metals from e-waste. Park and Fray (2009) used aqua regia for
leaching Au, Ag, and Pd. The results showed that 98% of Ag and 93% of
Pd could be recovered. Au was extracted selectively by using toluene as
solvent and about 97% was finally recovered. Fontana et al. (2018)
recovered Pd from monolithic ceramic capacitors (MCCs) by aqua regia,
followed by solvent extraction with Aliquat 336 in limonene. 100% of
Pd was dissolved under the following leaching condition: solid/liquid
ratio of 1/10, at 25 °C for 24 h.
Lee et al. (2011) have compared sulfuric acid, ammonia, aqua regia
and thiourea used as leaching solutions to recover Au, Ag and Cu from
scrap integrated circuits (ICs). The best result for aqua regia was that it
could achieve a 100% recovery for Au and Cu and an 88.51% recovery
for Ag. The leaching rates in other systems were not optimistic.
Although the leaching rates of Au and Ag were relatively high in
aqua regia, it was strongly oxidative, corrosive, and toxic (Petter et al.,
2014).
2.3.2. Non-cyanide extraction technologies
In order to reduce environmental impact, modified and new hy-
drometallurgical technologies have studied by several researches. Some
non-cyanide leaching agents such as thiosulfate, thiourea and thiocya-
nate were proposed.
Compared to cyanide and aqua regia leaching, thiosulfate leaching
showed relatively low recovery of gold. To improve the leaching effi-
ciency, Cu2+ was added as catalyst (Breuer and Jeffrey, 2000; Jeffrey
et al., 2001). Thiosulfate leaching is performed in the presence of am-
monia to stabilize Cu2+ since Cu2+ can increase the decomposition of
thiosulfate (Akcil et al., 2015a).
Tripathi et al. (2012) studied the effects of ammonium thiosulfate
concentration, copper sulfate concentration, pH, and pulp density on
gold leaching rate. Results showed that only 56.7% of gold was leached
out under the optimal condition of 0.1 mol/L ammonium thiosulfate,
40 mmol/L copper sulfate, and pH 10∼10.5 at room temperature. The
complete and shredded PCBs granules leaching behavior has also stu-
died. Under the same leaching conditions, gold leaching rate of com-
plete PCBs and shredded ones were 78.8% and 30.35%, respectively.
For complete and shredded PCBs granules, the dissolved copper was
1.53 g/L and 11.8 g/L, respectively. The dissolution of copper resulted
in higher losses of thiosulfate ions, which decreased in the recovery of
gold. Therefore, it is necessary to remove copper before thiosulphate
leaching. Ha et al. (2010) found that solution chemistry had more in-
fluence on gold extraction from PCB scraps. Gold leaching rate in-
creased with the concentration of thiosulfate after reaching maximum
leaching and then decreased with increasing thiosulfate concentration.
The stable region of the gold species was changed by the variation of
thiosulfate concentration since the pH value was affected by thiosulfate
concentration. Gold cannot be dissolved if the potentials of the copper-
ammoniacal thiosulfate system are too low (Aylmore and Muir, 2001).
In order to optimize the thiosulfate leaching of gold, response surface
methodology based on central composite design was used (Ha et al.,
2014). The quadratic mathematical model was established using sets of
experimental data and analysis of variance. The optimum conditions for
gold leaching were 72.71 mmol/L thiosulfate, 10.0 mmol/L Cu2+ and
0.266 mol/L ammonia. The kinetic model for metal dissolution fol-
lowed by the pseudo-second order kinetic model with chemical control.
Thiourea (CS(NH2)2) is a promising gold extracting agent for its
high leaching rate and eco-efficiency (Wronski and Luczak, 2010). The
electron pairs between nitrogen and sulphur atoms have a better po-
tential for a coordination bond between gold and silver during thiourea
leaching (Lacoste-Bouchet et al., 1998; Deschênes and Ghali, 1988).
289
Resources, Conservation & Recycling 141 (2019) 284–298
Fe3+can increase the redox potential of the solutions, resulting in
higher leaching rate of gold and silver (Birloaga et al., 2013).
Li et al. (2012a) conducted thiourea leaching of gold and silver from
the PCBs collected from waste mobile phones. 89.67% of Au and 48.3%
of Ag were recovered in the conditions: 24 g/L CS(NH2)2, 0.6% Fe3+
concentration at 25 °C for 2 h. To recycle value metals from waste PCBs,
two chemical leaching systems were developed by Birloaga et al.
(2014). The leaching rates of Zn, Cu, Fe, Ni and Sn were 100%, 100%,
58%, 81% and 94%, respectively in H2SO4-H2O2 solution. However, the
highest gold extraction rate was about 70% in thiourea acid leaching
process. Behnamfard et al. (2013) developed a multi-step hydro-
metallurgical processes to selectively recover Cu, Ag, Au and Pd. First,
by using two consecutive H2SO4-H2O2 leaching systems, almost all
copper was removed. Second, the residue was treated by thiourea in the
presence of Fe3+, which dissolved 85.76% of Au and 71.36% of Ag.
Last, the remaining Au and Pd were leached out in NaClO-HCl-H2O2.
This consecutive leaching process is low toxic and highly efficient, and
can selectively recover Cu, Ag, Au and Pd.
Gold can be leached by thiocyanate by using Fe3+ as oxidizing
agent and forms stable and soluble Au(SCN)2- and Au(SCN)4-. Li et al.
(2012a,b,c,d,e) have studied the thermodynamics and kinetics of acid
thiocyanate leaching of gold. The mechanism showed that Fe3+ was
reduced to Fe2+ while oxidizing SCN− during gold dissolution. The
leaching kinetics indicated that gold leaching in acid thiocyanate so-
lutions is the limiting step for the leaching process. Followed by the
above studies, the leaching of gold in mixed solutions (CS(NH2)2−-
SCN−-Fe3+) has been studied (Yang et al., 2011). They found that the
addition of small amounts of thiourea to thiocyanate-ferric solutions
revealed a synergistic effect on the dissolution of gold. Gold leaching
rate was higher than both ferric-thiocyanate and ferric-thiourea solu-
tions. The synergistic effect was attributed to the formation Au(CS
[NH2]2)2SCN.
2.3.3. Halide leaching
Chlorine, bromine, iodine have been used for gold extraction by
forming Au+ and Au3+ complexes. Chlorination is a feasible method
for gold recovery from waste PCBs with the advantages of higher
leaching rate, less pollution and selective leaching of different metals by
controlling the redox potential. He and Xu (2015) used chloride/so-
dium chlorate to recover Au from waste PCBs and reached 99% gold
recovery. Ball milling and supercritical process pretreatments were
necessary to separate metallic and non-metallic parts, and enlarge the
specific surface and decompose crystalline structure (Tan and Li, 2015).
Gold leaching rate increased from 48.25% to 89.98% after a 10 min ball
milling. However, it decreased to 43.75% after 60 min ball milling
treatment. The leaching rate of gold could reached more than 99%
under the optimal supercritical conditions (400 °C, 23 MPa, 60 min).
Gold and silver were selectively recovered from copper anode slime
(from e-waste smelting) by NaClO3-NaCl-H2SO4 solution. By controlling
the concentration of H+ (1.0 mol/L) and Cl− (0.02 mol/L), the leaching
yield of gold could reach 98.1%, and the impurities (e.g. Ag and Pb)
were hardly leached out (Ding et al., 2017).
Au, Ag, and Pd were recovered from waste PCBs by iodine-iodide
leaching with supercritical water oxidation (SCWO) pre-treatment (Xiu
et al., 2015). The leaching rates of Au, Ag, and Pd increased from
63.3%, 81.5%, and 60.5% to 98.5%, 97.2% and 99%, respectively when
SCWO time increased from 15 min to 60 min (the pressure was 22 MPa).
In the iodine-iodide leaching system, the reaction mechanisms were
illustrated as follows:
Anode reaction:
Au + I− = AuI2− + e- (2-1)
−
Ag + 2I = AgI2− + e- (2-2)
− −
Pd + 3I = PdI3 + 2e- (2-3)
Y. Ding et al.
Cathode reaction:
I3− −
+2e = 3I -
(2-4)
Therefore, the leaching rates of Au, Ag, and Pd strongly depends on
the iodide concentration and the iodine concentration. Other para-
meters (e.g. leaching time, solid to liquid ratio, and pH) were also
important for high recovery efficiency of Au, Ag, and Pd.
2.3.4. Electrochemical methods
Electrochemical technology is a promising method to recover pre-
cious metals from e-waste due to its high energy efficiency, low en-
vironmental impact and minimal chemical usage. Kim et al. (2011)
recovered gold from waste PCBs by using electro-generated chlorine as
an oxidant. This process is environmental friendly because it can op-
erate in the closed system and chlorine can be reduced during the
leaching of precious metals. The leaching efficiency of gold was 93% in
0.1 mol/L HCl by electro-generated chlorine at the current density of
714 A/m2. The leaching of gold was increased with higher temperature,
higher initial concentration of chlorine, and lower concentration of
acid.
Fogarasi et al. (2014) developed a chemical-electrochemical process
for the simultaneous recovery of copper and enrichment of gold from
waste PCBs. This process was performed by employing two different
types of reactors coupled in series. One was for the dissolution of base
metals with a perforated rotating drum, the other one was for the re-
generation of the leaching solution with the parallel electro-winning of
copper. After dissolution of base metals and recovery of Cu, the gold
concentration in the residue was 25 times higher than in the initial
waste PCB samples.
The minimal chemical input to recover metals was one of the ad-
vantages of the electro-recycling process. Oxidizing agents were gen-
erated to dissolve metals at the anode while reducing dissolved metals
at the cathode (Lister et al., 2014). Two stages of electro-recycling were
proposed: (1) about 97% of Cu, Sn and Ag were recovered with Fe3+ in
sulfate, (2) then Pd and Au were dissolved using Cl2 generated in dilute
HCl solution.
2.3.5. Other leaching methods
Other lixiviants such as inorganic acid/oxidizing reactive systems
were also investigated for leaching precious metals. Zhang and Zhang
(2014) successfully developed a non-acid process for selective recovery
of Pd from waste PCBs. The process contained three stages, as shown in
Fig. 4. The process included enrichment, dissolution and extraction of
Pd. Results showed that the dissolution percentage of Pd reached 98%
when Cu/Cu2+ ≤ 0.9 while less than 1.5% of Pd was dissolved when
Cu/Cu2+ ≥ 1.4. Under the optimum conditions (10% S201, A/O ratio 5
and 2 min extraction), 99.4% of Pd2+ was extracted from the solution.
In most cases, an amount of 10–35% of precious metals was lost
during the physical separation between metals and non-metals frac-
tions. Jadhav and Hocheng (2015) proposed an efficient hydro-
metallurgical process using large pieces of PCBs. In their study, HCl,
HNO3, H2SO4, C2H4O2 and C6H8O7 were used as lixiviants for leaching
metals. It was found that 100% of Ag, Au and Pd were dissolved in HCl
solution for 22 h from the size of 4 cm × 4 cm pieces. To achieve this
goal, HNO3 took 96 h. Less than 10% of precious metals were dissolved
in H2SO4, C2H4O2, and C6H8O7 for over 100 h. Hence, HCl is a suitable
lixiviant for leaching metals from large PCB pieces.
3. Recovery of PMs from spent catalysts
Recovery of precious metals from spent catalyst has the advantages
including the simple process, short production cycle, and low invest-
ment and environmental impact comparing with mining production.
However, the concentration of PMs in spent catalysts varies from
100 ppm to 100%, and the catalyst carriers also diverse in different
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Resources, Conservation & Recycling 141 (2019) 284–298
applications. Many researchers have made efforts on precious metals
recycling from spent catalysts (Dong et al., 2015; Jha et al., 2013).
Among the recycling technologies, the most practical ones are con-
centrating precious metals by the pyrometallurgical process or by the
selectively leaching process.
3.1. Pyrometallurgical process
The contents of PMs in spent catalysts are always less than 1%. To
enhance the recycling efficiency and reduce reactants consumption,
concentrating PMs by the pyrometallurgical process is a good choice.
PMs can be enriched in the metal or metal alloy phase by pyr-
ometallurgical treatment, and then recovered by refining technologies
(Akcil et al., 2015b).
Copper, iron, lead, nickel, and matte are good collectors of PMs. In
the pyrometallurgical process, crushed spent catalysts mixed with
fluxes (Al2O3, CaO, or SiO2), collector and reductant were smelted.
Mutual solubility, chemical properties, melting point, and environment
impact between collector materials and PMs have to be taken into
consideration (Peng et al., 2017).
3.1.1. Metal trapping methods
Lead is a traditional collector which has been applied to treat sec-
ondary resources before 1980s. Using blast furnace or electric furnace,
lead oxides were reduced to lead bullion, while PMs formed alloy and
stayed in the metal phase. The supporting materials were oxidized or
directly entered into the slag phase. The PMs in lead bullion were en-
riched by selective oxidation in a blast furnace or converter. Lead col-
lection has the advantages of easy operation, low working temperature,
the mature subsequent refining process. However, the disadvantages
are the long processing period, low recovery rate of Rh (about
70%–80%), and emission of volatile leads to the workers and en-
vironment.
With a target towards higher recovery rate and less pollution,
copper and iron trapping technologies have been studied and applied in
industry. Kolliopoulos et al. (2014) studied the behavior of PGMs
during their recovery with copper smelting. They raised “wetting” and
“settling” mechanisms on metal recovery in this process. Wetting me-
chanism shows that micro-dispersed particulates of PGMs in the slag
were wetted by molten copper and form copper droplets. Settling me-
chanism means that solid PGMs micro-particles settle through the
molten slag and form a solid solution with copper. Results showed that
the heavier Pt was recovered primarily (almost 88%) through “settling”
mechanism. Meanwhile, Pd and Rh were recovered following by both
mechanisms. But the “settling” one is more significant (66% for Pd and
57% for Rh). After enrichment of PGMs into the molten copper, the
molten copper is then casted into anode plate for electrolysis. The
overall recovery of PMs by copper collection may approach as high as
99% (Fornalczyk and Saternus, 2013).
An industrial application of copper collection was at Tanaka
Precious Metals. Spent automobile catalysts, copper oxide, flux and
reducing agent were mixed and fed into closed electric furnace. PGMs
were collected in the copper phase during smelting stage. After se-
paration of slag and metal phase, the total content of PGMs (Pt, Pd, Rh)
was less than 1.0 g/t (Yamada et al., 2006).
Iron is one of the most promising collectors due to its low-costing
and strong chemical affinity with PGMs to form a solid solution. Plasma
melting technology is most extensively used method for recycling PGMs
from spent catalysts, concentrating PGMs in the molten the iron phase.
The Fe-PGMs alloy and slag can be separated easily because of their
large densities difference (6.0∼7.0 g/cm3 versus 3.0∼3.5 g/cm3).
Through industrial test on plasma melting iron capture technology, the
recovery rates of Pt, Pd and Rh were over 98%, 98% and 97%, re-
spectively (He et al., 2016).
Benson et al. (2000a) found that PGMs recovery cannot be simply
explained by the gravity model. The diameter of PGM particles needed
Y. Ding et al.
Fig. 4. Flow chart of Pd recovery by non-acid process from waste PCBs (Zhang and Zhang, 2014).
to be above 200 μm for their settling by gravity. However, the particles
were in nanoscale in spent catalysts. By using a model based on com-
putational fluid dynamics and diffusion-controlled mass-transfer, the
migration coefficient of PGMs during the process was calculated and
the influences of temperature, droplet size, slag composition on col-
lector-metal droplets settling were also discussed (Benson et al.,
2000b). The model initially focused on the determining factors on the
settling rate of PGMs and their recovery in the molten iron. Calculation
with data under Stocks’ law for iron droplet setting showed that the
recovery rate of PGMs would reach over 90% within 1 h when droplet
diameter was 0.1∼0.3 mm. Plasma melting technology has the ad-
vantages of high recovery rate, short process, high efficiency, no gen-
eration of wastewater and gas. However, it is high energy consumption
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Resources, Conservation & Recycling 141 (2019) 284–298
and works at high temperature (> 2000 °C). The high temperature can
reduce silicon dioxide into monatomic silicon and form ferrosilicon
alloy. However, the ferrosilicon alloy is extremely difficult to dissolve,
and resulting recovery of PGMs challenging.
To solve this problem, Dong et al. (2014) investigated PGMs re-
covery by the iron trapping method based on solid state. The results
showed that Pt, Pd, and Rh recovery rate were 98.6%, 91.7% and
97.6%, respectively when the reducing temperature was only 1220 °C.
They found PGMs transformed to atomic state or atomic cluster and
bonded with free electrons in iron metal during reduction process. The
iron atoms kept together and formed crystal nucleus particle, and the
crystal grain grew up, after which the iron containing PGMs can be
recovered by ball grinding-magnetic separation.
Y. Ding et al. Resources, Conservation & Recycling 141 (2019) 284–298

3.1.2. Matte trapping methods

Chen and Huang (2006)

Aberasturi et al. (2011)

Kuczynski et al. (1992)

Hammadi et al. (2017)

Kizilaslan et al. (2009)

Nogueira et al. (2014)
Due to the close affinity of matte for PGMs, matte is a good collector

Marinho et al. (2011)

Barakat et al. (2006)

Shams et al. (2004)
(Jones and Geldenhuys, 2011). He et al. (2012) adopted the high nickel

Chen et al. (2014)

Mahmoud (2003)

Sarioğlan (2013)
matte (Ni2S3-CuS) trapping-aluminothermic activation method to re-
cover rhodium from spent organic rhodium catalysts. In the melting

References
state, the materials have low melting point (about 1000 °C) and good
liquidity. The recovery rate of Rh reached 94.65% in this enrichment
process. You et al. (2016) used nickel and sulfur as collectors to smelt

Pt 96%, Pd 97.8%, Rh 92%

spent catalysts in the presence of Na2CO3 and Na2B4O7 at 1050 °C for
30 min. The recovery rates of Pt, Pd, and Rh were 90%, 93%, and 88%,
respectively.

95%, Rh 86%
Due to the unique chemical composition of copper and nickel ore in

PGMs 85-90%
Recovery rate
Jinchuan Group Co, Ltd., PGMs were concentrated in FeS-Ni2S3-CuS

(1) Rh 56%
(2) Rh 80%
PGMs 95%
PGMs 90%

Pt 97.58%
Pt > 95%
matter. The smelting atmosphere is important in this system since

99%
99%
95%
Pt 99%
Pt 85%
Pt 97%
oxidation of nickel will cause refining difficulty after separation of

Pd
Pd
Pd
Pd
PGMs-containing matte from slag. The performance of smelting slag
determined the distribution behavior of precious metals. In general, the

S:L ratio

1:100

1:2.5
slag was composed of FeO-CaO-MgO-SiO2. The high basicity of slag will

1:20

1:10

1:20

1:10
1:20
1:4
1:4

1:2
1:4

1:3
enhance desulfurization reactions and form Na2S that has the potential
to enrich PMs in slag. Too low basicity will increase viscosity of slag and

Time (h)

20 min
decrease its fluidity, inhibiting the separation of matte and slag. All of

10 h

6h
2h
precious metals can recovered in matter once slag and matter phases

1
1

4
3
2
2
were separated effectively.

Temp. (°C)

160
160

125
180

100
3.2. Hydrometallurgical process

75

90
90

80
90
60
80
(1) Without any pretreatment; (2) Pretreatment: 300 °C, 3 h, flow rate of CO 150 ml/
In the hydrometallurgical process, precious metals are dissolved in
cyanide, aqua regia and strong acids, such as HCl, HNO3 and H2SO4.
The oxidizing agents (such as H2O2, O2, Cl2 and I2) are also added to
increase the leaching efficiency. Some typical leaching of PGMs from
spent catalysts are listed in Table 5. In general, Pd was most likely to be
leached, while Rh was hard to achieve a high recovery rate (90%). The
recovery rate of PGMs was high by cyanide leaching. However, it re-
quired high temperature and the cyanide was highly toxic. The situa-

HCl 3 mol/L, H2SO4 5 mol/L, H2O2 3 ml, NaClO3 2 mol/L

tion is similar to aqua regia leaching. High leaching efficiency can be
also achieved in environmentally friendly leaching agents (HCl/H2SO4
+ H2O2/Cu2+) under optimal conditions. In some cases, PGMs were HCl 12 mol/L, H2O2 7% and H2SO4 2.0 mol/L

transformed into inert compound because of oxidation or sulfuration,

resulting low recovery rate. Therefore, it is necessary to reduce them
into metallic state before leaching experiments.
NaCN 6.25 g/L, O2 pressure 1.5 MPa
NaCN 1 wt.%, NaOH 0.1 mol/L

HCl 6 mol/L, Cu2+ 0.3 mol/L

3.2.1. Cyanide leaching 10 HCl (37%): 1 H2O2 (36%)

H2SO4 60%, NaCl 0.1 mol/L

Sodium cyanide has been widely employed to recover PGMs (Chen

NaCN 1 wt.%, pH=9

and Huang, 2006; Allen et al., 1992). Dissolution of PGMs in cyanide

Leaching conditions

HCl 10%, H2O2 5%

HCl 7%, H2O2 5%

solution was shown as follows.

2 Pt + 8NaCN + O2+ 2H2O → 2Na2[Pt(CN)4] + 4NaOH (3-1)

Aqua regia
Aqua regia
Reagents

2Pd + 8NaCN + O2+ 2H2O → 2Na2[Pd(CN)4] + 4NaOH (3-2)

min

Rh + 24NaCN + 3O2+ 6H2O → 4Na3[Rh(CN)6] + 12NaOH (3-3)

Some typical leaching of PGMs from spent catalysts.

Selective linear paraffin dehydrogenation spent catalyst

The cyanide reaction mechanism was mainly controlled by a surface

chemical reaction of precious, and the leaching rate was the function of
cyanide and oxygen concentration (Naghavi et al., 2016). The cyanide
leaching of PGMs requires higher temperatures than gold since the
metallic bonding strength of PGMs is higher. Chen and Huang (2006)
automotive catalytic converters

recovered PGMs from spent auto-catalysts by pressure cyanide

alumina-supported catalyst
carbon-supported catalysts

leaching. With an oxygen pressure 1.5 MPa, NaCN 6.25 g/L, solid: li-
quid = 1:4, and 160 °C, the recovery of Pt, Pd and Rh were 96%, 98%
catalytic converters
Spent bulky catalysts
Spent pellet catalysts

Car catalytic converters

and 92%, respectively. Due to the metal bonding strength of their

Virgin bulky catalysts

Spent auto-catalysts

Spent auto-catalysts

complexes, the leaching order in cyanide solution was Pt > Pd > Rh.
Industrial catalyst

Kuczynski et al. (1992) compared the leaching behavior of Pt from

Spent catalysts
Auto-catalysts

virgin and spent monolith catalysts in NaCN-NaOH solutions. More

Materials

than 95% and 90% of PGMs were dissolved from virgin bulky and used
Table 5

Spent
Spent
Spent
Scrap

pellet catalysts respectively by leaching twice with 1 wt.% NaCN and

0.1 mol/L NaOH solution at 160 °C. The dissolution differences between

292
Y. Ding et al.
virgin and used monolith catalyst were due to contamination from
combustion and sintering of substrate materials, decreasing the reaction
surface and activity. By using this process, 95–97% of Pt was recovered
from spent pellet catalysts in a pilot scale (45 kg), recovery rates of Pd
and Rh were 94∼95% and 64∼81%, respectively (Kuczynski et al.,
1995).
3.2.2. HCl(aq)+oxidants leaching
In order to reduce the environmental impact caused by cyanide.
Precious metals are leached in HCl medium with oxidizing agents
(Grumett, 2003; de Sá Pinheiro et al., 2004). PGMs are mostly oxidized
and form soluble complexes (e.g. [PtCl6]2−, [PdCl4]2−, [RhCl6]3-) with
chloride.
Green (2004) reported that over 95% of PGMs were recovered from
roasted concentrates in 6.0 mol/L HCl solution by using chlorine gas.
However, chlorine gas are highly corrosive and toxic, which is the
major obstacles to be overcome. Waste chlorine gas must be turned into
harmless chloride for discharge.
Kim et al. (2013) and Upadhyay et al. (2013) developed an eco-
friendly electro-generated chlorine leaching method for leaching PGMs
from spent automotive catalysts. The generated Cl2 was fed into HCl
solution, forming Cl2(aq), Cl3−, HClO. Cl3- species seemed to be the
most effective chlorine species for dissolving Pt, which enhanced Pt
dissolution by an increase of Cl3- at the certain HCl concentration.
Leaching rates of Pt, Pd and Rh were 71%, 68%, and 60%, respectively
under the optimized conditions of HCl 6.0 mol/L, current density
714 A/m2, temperature 90 °C, and pulp density 20 g/L. The activation
energies for Pt, Pd, and Rh were 29.6, 26.4, 20.6 kJ/mol, respectively.
Therefore, PGMs extraction dissolution kinetics in this process were
followed ash diffusion control. The deposits of carbon or sulfur-con-
taining substances on the surface of spent catalysts may hinder the
dissolution of PGMs. Based on thermodynamic analysis, the metallic
PGMs were much easier to be chlorinated and converted to soluble
chlorides compared with their oxides (Bezuidenhout et al., 2013). Chen
et al. (2014) found Rh extraction rate increased from 56% to 82% H2
reduction pretreatments (300 °C for 3 h and flow rate 150–200 ml/min).
The use of chlorine requires special attention due to its poisoning
effect. The reactions with aqua regia and other HCl/HNO3 mixtures
involve the emission of nitric oxide (e.g. NO and NO2) and Cl2
(Massucci et al., 1999). Therefore, more environmentally friendly oxi-
dants are essential to precious metals extraction. Nogueira et al. (2014)
developed a leaching process using Cu2+ as the oxidizing agent in HCl
solution for recovery of Pd and Rh from spent catalysts. The chloride
media allow the adequate conditions for oxidizing and solubilizing the
metals. Under the optimal conditions (HCl 6.0 mol/L, Cu2+ 0.3 mol/L,
80 °C, 4 h), the maximum recovery rates of Pd and Rh were 95% and
86%, respectively. The concentrations of HCl and Cu2+ were the most
determinant factors, which influenced the leaching efficiencies. For
example, the leaching rates of Pd and Rh were about 70∼80% and
35∼40%, respectively when the concentrations of HCl and Cu2+ were
2.0 mol/L and 0.05 mol/L.
Safer and cheaper HCl-H2O2 solution was also widely used as an
alternative to aqua regia (Aberasturi et al., 2011). Kizilaslan et al.
(2009) compared the leaching efficiency of HCl+H2O2 solution with
aqua regia for Pd recovery. It was found that Pd was more easily ex-
tracted in aqua regia solution. Temperature was the most important
parameter affecting the efficiency of Pd dissolution for both solutions.
The highest leaching rates in room temperature were 67% and 52% in
aqua regia and HCl+H2O2 solution, respectively. More than 95% of Pd
was dissolved at 80 °C for 2 h in HCl+H2O2 solution when the ratio of
liquid/solid was 20.
Sarioğlan (2013) studied the recovery of Pd from spent activated
carbon-supported palladium catalysts using dilute HCl and H2O2. The
leaching was carried out at 90 °C for 180 min A maximum leaching rate
of Pd was 99% in a mixture solution of 10% HCl and 5% H2O2. The
leaching efficiency increased with both temperature and time, and the
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Resources, Conservation & Recycling 141 (2019) 284–298
optimal condition was 10% HCl and 5% H2O2 at 90 °C for 3 h. Spent
alumina supported palladium catalyst was also leached by 7% HCl and
5% H2O2 solution at 60 °C for 2 h with an extraction rate of 99% of Pd
(Barakat et al., 2006).
In order to enhance the selectivity for Pd and decrease the Al con-
tamination, MgCl2 or NH4Cl was used to reduce acidity in the process of
leaching Pd from spent industrial catalysts (Paiva et al., 2017). The
partly replacement of HCl does not affect Pd leaching efficiency
(95–100%) in the solution of HCl-MgCl2/NH4Cl-H2O2 when the con-
centration of HCl is not below 1.0 mol/L. But the content of Al de-
creased from 3.3 g/L to 2.2 g/L by using HCl/NH4Cl mixture for 0.5 h.
Significantly, high Al3+ concentrations may affect the following liquid-
liquid extraction efficiency and the extraction-stripping cycles of sol-
vents due to accumulation in the organic phases.
In order to avoid the toxic leaching agents, spent catalysts were
roasted with alkali metal salts at 600–800 ℃ in air. Complex oxides of
Pt (M2PtO3, M = Na, Li) were prepared and then dissolved in HCl so-
lution directly (Kasuya et al., 2016). The result showed that the solu-
bility of Li2PtO3 was higher than Na2PtO3. The leaching efficiency of
Li2PtO3 was nearly 100% in 12.0 mol/L HCl at 180 °C for 2 h.
3.2.3. Supercritical fluids extraction
Supercritical fluids have the advantages of good selectivity, facile,
easily recycled process, low surface tension, and low energy con-
sumption and nontoxicity (Laintz et al., 1992), which are currently used
as unique solvents for different types of reactions (Eckert et al., 1996;
Phelps et al., 1996). By controlling pressure and temperature, metal
ions can be easily dissolved and efficiently extracted from supercritical
fluids according to their size, boiling point, polarity, and molecular
weight.
Faisal et al. (2008) studied the recovery of Pd, Pt and Rh from spent
automobile catalytic converters by supercritical carbon dioxide
(SCCO2) containing a tributyl phosphate (TBP). They found that the
addition of chelating ligand was necessary to extract the PGMs because
no metal was extracted with pure SCCO2. SCCO2 with TBP-HNO3 was
not effective for extracting Pt and Rh, of which the extraction efficiency
was less than 3%. More than 96% of Pd was extracted at 60 °C, 20 MPa
for 60 min of extraction time. Iwao et al. (2007) compared the effect of
different chelating agents (Cyanex 302, acetyl acetone, or TBP/HNO3/
H2O) on Pd extraction by using SCCO2. Among those chelating agents,
Cyanex 302 obtained the maximum extraction efficiency of more than
99%. Under the optimal condition, the highest extraction rates of Pd for
acetyl acetone and TBP/HNO3/H2O were around 80% and 60%, re-
spectively. The difference was owing to a decreased ability to form a
complex of acetyl acetone and TBP/HNO3/H2O with palladium. Wang
and Wai (2005) used HNO3 as an oxidizing agent and a fluorinated β-
diketone as a chelating agent, and Pd can be easily dissolved in SCCO2
with a recovery rate of 99% after 30 s extraction. Collard et al. (2006)
recovered precious metals from organic compositions such as hetero-
geneous (e.g. Pt/C) or homogeneous precious metal catalysts by using
supercritical water. The leaching rates of Pd, Pt, and Rh from organic
compositions were over 95% at 500∼600 °C and 25∼30 MPa with
oxygen injection (0–15%).
3.2.4. Other leaching methods
Microwave-assisted leaching: Microwave-assisted leaching has been
used to improve the extraction efficiency and reduce process time,
especially with the increasing demand for more environmental-friendly
processes. Jafarifar et al. (2005) studied two alternative methods for
leaching PGMs from spent catalysts. One was direct leaching with aqua
regia at a liquid/solid ratio of 5 for 2.5 h, and the other one was per-
formed by microwave radiation at a liquid/solid ratio of 2 for 5 min.
The maximum leaching rate of Pt was 96.5% for the conventional
process. For microwave-assisted leaching, the extraction rate could
reach 98.3% after only 5 min. Suoranta et al. (2015) studied the re-
covery of Pd, Pt, and Rh by microwave-assisted leaching with cloud
Y. Ding et al.
point extraction. More than 90% of Pd, Pt, and Rh could be recovered
both in aqua regia and HCl solution at temperatures above 150 °C.
However, over 95% of the matrix elements (Al, Ce, Zr) were leached out
simultaneously. By using the cloud point extraction method, less than
5% of the matrix elements were transferred to the surfactant rich phase,
which indicated that precious metals were separated efficiently. The
similar results were also obtained by other researchers (Niemelä et al.,
2012).
Substrates leaching: In order to reduce consumption of lixiviant, some
authors studied the dissolution of the catalyst substrates for con-
centrating PGMs in the leach residue. Kim et al. (2010) recovered Pt
and Pd from spent petroleum catalysts by dissolving substrate in sul-
furic acid. They found that the dissolution of substrates containing only
γ-Al2O3was higher than that of containing the mixture of γ-Al2O3 and α-
Al2O3. The dissolutions of both substrates were higher than 90% under
the optimal leaching condition: H2SO4 6.0 mol/L, temperature 100 °C,
leaching time 2–4 h, and pulp density 220 g/L. Alkali dissolution was
another method to dissolve the supported materials Al2O3, which was
only suitable for γ-Al2O3. It is important to control the pH value since
aluminates possibly forms colloid due to alumina hydrolysis, making it
hard to separate solid and liquid. However, the disadvantage of sub-
strates leaching methods was that a small amount of PGMs that could
be dissolved meanwhile.
3.2.5. Liquid-liquid extraction and solid phase extraction
Precious metals were dissolved in aqueous solution after hydro-
metallurgical processes. The metals from the leaching solution are then
separated and recovered by different methods, such as liquid-liquid
extraction, solid phase extraction, precipitation and crystallization.
Compared with chemical precipitation, liquid-liquid extraction and
solid phase extraction have the advantages of low environmental im-
pact, high efficiency and selectivity (Bernardis et al., 2005).
In the liquid-liquid extraction process, different organic extractants
(e.g. cationic, anionic or solvating type) are applied for the recovery of
precious metals depending on their characteristics in the solution. Some
extractants have been employed in industry. For example, high purity
Pd and Ir have been extracted by using liquid-liquid extraction with
amines, beta-hydroxyxime with an amine accelerant for palladium and
amide extractants for iridium (Jha et al., 2014). Lee et al. (2009) re-
ported the extraction of PtCl62− and RhCl63- from acidic solutions by
using tri-iso-octylamine (Alamine 308) as an extractant diluted in ker-
osene. The extraction rates of PtCl62− and RhCl63- were 98% and 36%,
respectively with 0.01 mol/L Alamine 308 at 1.0 mol/L HCl. The mixed
solution of 5.0 mol/L HCl and 0.75 mol/L thiourea was good stripping
reagents. The recycling capacity of Alamine 308 decreased slightly after
12 cycles of extraction and stripping. Phosphonium ionic liquids are
prospective methods for separation of PGMs. Cieszynska and
Wisniewski (2011) have successfully extracted over 99% of PdCl42- with
Cyphos®IL 101 and Cyphos®IL 104 from 0.1 mol/L HCl in the presence
of Ni2+, Cu2+, Pb2+, Fe3+, and RhCl63-. However, the separation of
PdCl42- from Pt-containing solution is not effective and both of ex-
traction efficiencies were appropriate 70%. Pd(II) can be effectively
separated from the loaded organic phase through stripping with
0.5 mol/L NH3 solution.
Although liquid-liquid extraction has the advantages of high se-
lectivity and excellent extraction efficiency, the defects such as volatile,
inflammable, toxic, and not recyclable in long term limit its application.
In order to avoid the defects of liquid-liquid extraction, solid-phase
extraction methods have been raised great attentions. It consists of an
inert solid support and a complexing agent impregnated on the solid
support. The characteristic of the complexing agent decide the se-
lectivity towards a specific metal ion and the solid support influences
the adsorption capacity, chemical stability and mechanical strength
(Sharma et al., 2017). Some solid-phase extractants have been widely
used in commercial scale, such as Amberlite IRA 400 and Superlig®
series of media (Bernardis et al., 2005).
294
Resources, Conservation & Recycling 141 (2019) 284–298
Strongly basic anion exchange resins with styrene or acrylic poly-
mers cross-linked with divinylbenzene show a high selectivity for PGMs
(Pyrzyńska, 1998). Pd(II) complexes has high affinity for Lewatit MP-
500, of which the equilibrium adsorption capacity was in the range
from 8.48 to 9.99 mg/g in the chloride solutions containing 1.0 mol/L
NaCl (Wołowicz and Hubicki, 2009). Nikoloski et al. (2015) in-
vestigated the applicability and performance of the different ion ex-
changers to recover Pt, Pd and Rh simultaneously (Nikoloski et al.,
2015). Three ion exchangers including Lewatit MonoPlus (+) MP600
with a quaternary ammonium functional group, Purolite S985 with a
polyamine functional group and XUS 43,600.00 with thiouronium
functional group. The leaching solution contained 2.35 mol/L HCl and
the concentrations of Pt, Pd, and Rh were 0.13, 0.13, and 0.03 mmol/L,
respectively. XUS 43,600.00 has the best overall absorption recovery of
PGMs when compared with other two ion exchangers. The absorption
recovery rates of Pt and Pd were over 99%, whereas absorption of Rh
was 75.3%. Purolite S985 had the highest recovery rate of Rh (87.8%).
Molecular recognition technology is one kind of solid phase ex-
traction by using SuperLig® products. The advantages of molecular re-
cognition technology contain large ligand-target metal binding en-
ergies, fast reaction rate, high selectivity, environmental friendly, and
separation of selective metal and recovery of pure metals directly (Izatt
et al., 2015). SuperLig® products can selectively absorb specified metal
ion of PGMs. For example, SuperLig® 2 is selective for the recovery of
the cation (Pd2+) from remaining PGMs solution. Pt and Rh are then
separated by using SuperLig® 133 and SuperLig® 190, respectively (Izatt
et al., 2012).
Compared with liquid-liquid separation, solid-phase method has
advantages in terms of good recovery efficiency, facile adsorption and
desorption mechanism, regenerability, none organic pollution.
However, the cost of extractants is expensive. It is also challenging to
achieve the extractants with performances of high adsorption capacity,
excellent selectivity and recyclable.
4. Advantages and environmental impacts of recycling
technologies
As described in Sections 2 and 3, the recycling technologies for
precious metals from e-waste and spent catalysts have been improved
with the aims of enhancing recovery rate and reducing environmental
pollution.
For e-waste, pyrometallurgy can recycle precious metals as well as
base metals (e.g. Cu, Pb, Sn, etc.) with high purity through the smelting
and refining process. The state-of-the-art smelting technologies have
already been applied in some enterprises in developed countries (shown
in Table S4). Although these pyrometallurgical plants have achieved
the requirement of strict pollution emission, most smelting plants in
developing countries still cannot meet the emission standards.
However, over 80% of e-waste is disposed in developing countries
(Balde et al., 2017). Pollution problems are still inevitable although
smelting technologies have been improved and upgraded in developing
countries. Much attention needs to be paid on the disposal of waste gas
and slags (Ghodrat et al., 2017a). The generation and release of dioxins
and particulate matter (PM) 2.5 should be considered. Smoke treating
devices are indispensable to disposal ash and toxic gases. The occupa-
tional safety is very critical due to high working temperature, emission
of hazardous gases and PM 2.5. Moreover, the equipments are ex-
pensive and the investment is huge, which is not suitable for small and
medium-sized enterprises. Alkali smelting can separate plastics, cera-
mics, and metals effectively at low temperatures. However, much toxic
gas (e.g. bromide) would generated during smelting, as well as waste-
water containing heavy metal ions during the leaching process. Cur-
rently, alkali smelting was only studied in the laboratory stage.
Compared with pyrometallurgical technologies, hydrometallurgical
processes are more widely employed in developing countries and areas.
With the purpose to reduce the environmental impacts caused by
Y. Ding et al.
Table 6
Basic assessment indices of different leaching methods (Akcil et al., 2015a,b; Li et al., 2018; Awasthi and Li, 2017).
Methods Economic feasibility
Leaching rate Reagent costs
Cyanide 3 5
Aqua regia 4 4
Thiourea 4 4
Thiosulfate 2 2
Chloride 5 4
Bromide 5 2
Iodide 5 3
Scale is between 0 and 5.
traditional leaching methods, some modified hydrometallurgical tech-
nologies have been developed. The detailed assessments of different
leaching methods based on economic feasibility and environmental
impacts are shown in Table 6. The most reliable methods are cyanide
and aqua regia leaching, but both are highly corrosive and toxic. The
thiourea and thiosulfate have moderate environmental impacts, but
they are not economically feasible. In addition, the technologies are not
reliable when compared with other leaching methods. The halide
leaching have the advantages of high recovery rate and moderate
toxicity. However, the corrosion issues and technological reliability
need to be considered.
Compared to e-waste recycling, recovery of precious metals from
spent catalysts was easier due to their simple components for certain
kind of catalyst. Several pyrometallurgical methods have been devel-
oped for concentrating PGMs. The distinct advantages are high re-
covery rate, efficiency, and no generation of wastewater. The defects of
pyrometallurgy are similar to e-waste smelting.
Hydrometallurgical leaching of PGMs from spent catalysts was
carried out in different lixiviants. Cyanide leaching shows poor effi-
ciency at room temperature and atmospheric pressure. The toxicity of
cyanide must be considered seriously. Aqua regia leaching was em-
ployed on the commercial scale to recover PGMs. However, during the
leaching period, serious environmental pollution has caused by the
generations of NOx, Cl2, and acid fumes. Moreover, the dissolution of
alumina matrix materials makes PGMs separation difficult. High
leaching rate of PGMs in cyanide solution required high temperature
and pressure. The potential emission of toxic cyanide may cause serious
environmental problems and threaten the health of workers. H2O2 also
has potential to be used for the leaching of PGMs. However, Cl2 can be
formed during the leaching process, as well as by using NaClO and
NaClO3 as oxidants.
The environmental benefits of supercritical fluids extraction and
microwave-assisted leaching technologies have been validated. SCCO2
with chelating ligand was highly efficient for Pd extraction, but not
effective for extracting Pt and Rh. And the cost is too expensive.
Microwave-assisted leaching can improve PGMs recovery rate with less
time and agents. However, it still needs to be improved for further
promotion since this technology is currently only suitable for treating
the small amount of materials. Table 7 shows the technologies status for
recycling precious metals from e-waste and spent catalysts.
In fact, almost all efforts are for better cost-effectiveness, higher
recovery rate, and less environmental impact. With the continuous re-
search and development of recycling technologies, environment-or-
iented concept has been gradually formed. Consequently, to realize this
goal, combinative recycling methods need to be put forward.
5. Outlook and conclusions
Precious metals are widely applied in many fields of industries. Due
to the conflicts of limited natural resources and increasing demands, as
well as their economic value, it is essential to recycle precious metals
295
Resources, Conservation & Recycling 141 (2019) 284–298
Environmental impacts Research level
Corrosive Toxicity Reliability
5 5 5
5 5 5
3 4 3
4 4 2
5 3 4
2 3 2
5 5 3
from secondary resources. Throughout the past decade, the amount of
recycled precious metals was estimated to be approximately 30% of
global mine production. During the last decade, there has been an in-
tensification of research activities for developing effective recycling
methods for precious metals, especially e-waste and spent catalysts.
Environment-oriented technologies for recycling precious metals have
been formed gradually.
Based on the traditional technologies for recycling precious metals,
various methods have been significantly improved. As the precious
metals dominate the most value for e-waste recycling, the loss of these
metals should be minimum. However, precious metals are dispersed in
each output fraction in e-waste mechanical processing (Ueberschaar
et al., 2017). Direct smelting without mechanical treatment can recover
almost all of precious metals, as well as other valuable metals. The fume
treatment should be payed special attention since hazardous gases (e.g.
dioxins and bromide) may be generated during this process. As for
spent catalysts, concentrating precious metals in metal phase can re-
duce the reagents consumption in further dissolution and purification.
Hydrometallurgical, cost-effective, and innovative technologies
have been developed to drastically decrease the environmental impact.
Non-cyanide lixiviants, such as thiosulfate, thiourea, chlorination, io-
dine-iodide, and HCl in the presence of oxidizing agent have shown the
possibilities of leaching precious metals, some of which have already
applied in industry. To replace the HNO3 and prevent the generation of
NOx, H2O2 has potential to be used for the leaching precious metals.
Other methods, such as supercritical fluids extraction and microwave-
assisted leaching, also have the potential to leach precious metals. The
leaching efficiency of precious metals is consistent with stability con-
stants of their complexes and oxidation potential. Increasing the sta-
bility of precious metals complexes and reducing their oxidation po-
tential are effective methods to enhance leaching rate. Precious metals
complex (except Ag) have higher stability constants in chloride solu-
tion. In order to reduce the acidity and formation of Cl2, chlorine salt is
suggested to be used to enhance the concentration of Cl−, decreasing
the oxidation potential of precious metals. In our recent work, more
than 98% of Pt was recovered from spent petroleum catalysts in the
conditions of 1.0 mol/L HCl, 5.0 mol/L NaCl, 0.10 vol.% H2O2, at 90 ℃
for 2 h.
Although technologies for precious metals recovery have gained
obvious improvements, there are still some challenges for future pro-
motion. In order to achieve the environment-friendly and sustainable
recycling for precious metals with high recovery rate, several con-
siderations have been proposed. First, further technologies should be
prepared with the aim of commercialization in term of investment and
cost. Second, recycling technologies should be varied and integrated
based on the physical and chemical properties of different materials.
Third, with the purpose of higher leaching efficiency and less pollution,
some assisted methods or pretreatments are essential. For example,
recovery of Pd, Pt, and Rh from an automotive catalyst by microwave-
assisted leaching has a remarkable increase with less time and reagent
consumption. With the guidance of above analysis, future technologies
Y. Ding et al. Resources, Conservation & Recycling 141 (2019) 284–298

for precious metals recycling can be more efficient and has less en-

Hazardous gases; waste emission;

Hazardous gases; waste emission;

Hazardous gases; waste emission
vironmental impact, lower cost, and higher recovery rate.

Chemical reagents; air quality;

Air quality; high temperature;

Air quality; high temperature;

Chemical reagents; waste

Chemical reagents; waste

Chemical reagents; waste

Chemical reagents; waste

Chemical reagents; waste

Acknowledgments
Occupational safety

Chemical reagents
solid waste; noise

solid waste; noise

waste emission
This work was sponsored by National Natural Science Foundation of
air quality
China (Grants U1360202, 51672024, 51472030 and 51502014).

air quality
emission

emission

emission

emission

emission
Appendix A. Supplementary data

Supplementary material related to this article can be found, in the

Environmental impacts and main pollutions

Emission of NOx, Cl2 or HCN; wastewater

online version, at doi:https://doi.org/10.1016/j.resconrec.2018.10.

Fine particles pollution; large amount of
Large amount of wastewater containing

Emission of HCN; wastewater pollution

Emission of Cl2; wastewater pollution

Emission of small amount of Cl2; low

041.
Emission of dioxin, PM 2.5 particles,

Emission Cl2; wastewater pollution

Waste oil and waste gas pollution

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