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Recovery of precious metals from spent catalysts (solid waste) using

electrometallurgy method: A review

Conference Paper · February 2018

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 Recovery of precious metals from spent catalysts (solid waste) using
electrometallurgy method: A review

Vahab Ghaleh Khondabi1, Farzaneh Daneshpour1, Alireza Fazlali1*

1
Department of Chemical Engineering, Faculty of Engineering, Arak University, Arak, Iran
*
Corresponding author: [email protected]

ABSTRACT

This investigation presents an overview the use of electrometallurgy as a method for valuable metal recovery
from spent catalyst. Precious metals recovery is interesting due to their vast industrial applications, high market prices
and the limited resource of these metals. With the increase in environmental awareness, the disposal of any form of
hazardous waste has become a great concern for the industrial sector. Spent catalysts contribute to a significant amount
of the solid waste generated by the petrochemical and petroleum refining industry. The catalysts lose their effectiveness
over time, and when the activity of catalysts decline below the acceptable level, they are usually regenerated and reused
but regeneration is not possible every time. Recycling of some industrial waste containing base metals (such as Ni, V,
Co, Mo, Pt, Pd and etc) is estimated as an economic opportunity in the exploitation of these wastes. Several techniques
are possible to separate the different metals, among those selective precipitation and solvent extraction are the most
used. Pyrometallurgical treatment and bio-hydrometallurgical leaching were also proposed in the scientific literature but
up to now they did not have any industrial application. The state of art in recovery of metals from spent sources by
electrometallurgy (as an environmentally friendly technology and performance with high efficiency and purity)
highlighted and existing advantages and disadvantages of this technique are analyzed in this study.

Keywords: Electrometallurgy, Precious metals, Recovery, Spent catalyst

1. Introduction

The importance of catalysis to chemical processes is enormous. An estimated 90% of the chemical production
processes are based on catalytic technologies, encompassing four major market sectors: fuel refining, polymerization,
chemical production and environmental remediation [1, 2]. The catalysts deactivate with time and when the activity of
the catalyst declines below the acceptable level, it is usually regenerated and reused [3, 4], but regeneration is not
always possible [5], and after a few cycles of regeneration and reuse, the catalyst activity may decrease to very low
level and further regeneration may not be economically feasible. The spent catalysts are discarded as solid wastes [6, 7]
and their contribution to environmental contamination is increasing every day. The hazardous nature of the spent
catalysts is attracting the attention of environmental authorities in many countries and the environmental laws become
more severe in recent years. Spent catalysts have been classified as hazardous wastes by the United States
Environmental Protection Agency (USEPA) [8, 9]. At the same time, most of these catalysts contain platinum group
metals (PGMs), including: platinum (Pt), palladium (Pd), rhodium (Rh), ruthenium (Ru), iridium (Ir) and osmium (Os)
[10], and valuable metals such as: nickel (Ni), vanadium (V), molybdenum (Mo) and cobalt (Co) [11] in the form of
oxides or sulfides supported on carriers such as alumina, silica, etc. Recovery of these metals, many of which in turn
consumed in carbon and stainless steel- making as an alloying agent to produce ferro-alloys and other valuable
products, is an attractive option [12–14].

In the field of recovery of the mentioned metals, the focus is on the extraction of these metals from catalytic
converters of cars, catalysts of petroleum, petrochemical and pharmaceutical industries. Recovery methods are
classified in a variety of ways, such as extraction with organic solvents [15-17], ion exchange resins [18, 19], adsorption
onto activated carbon [20, 21] and membrane utilization [22]. Most of these processes have a large number of chemical
reactions that require more than one operating unit and also require advanced equipment to remove these metals, which
will cost a lot. But in most of these sources, these methods are classified into three groups of methods: pyrometallurgy,
hydrometallurgy and electrometallurgy [23, 24]. In addition to the above mentioned methods, metal-to-gas transfer and
bioleaching methods are also available as recovery methods for metals. The choice of method depends on the number
and type of metals in the catalyst, their concentration, the nature of the catalyst base and the total amount of the catalyst

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[25, 26]. Among the techniques used to separation of metals, the electrolysis process is considered in terms of variety
and simple equipment, easy operation and cost effective operating costs and the high recovery with high purity metals
[27, 28].

2. Description of electrometallurgy process

Electrometallurgy is the group of technologies used for extraction of metals from solutions, including molten salt
solutions (electrowinning), or for the purification of metals by electrochemical dissolution into/deposition out of such
solutions (electrorefining) [29]. Both operations are accomplished in an electrolytic cell, a device that permits electrical
energy to perform chemical work. This occurs by the transfer of electrical charge between two electrodes immersed in
an ionically conducting liquid (electrolyte) containing metal dissolved as positive ions. At the negatively charged
cathode the metal cations acquire electrons (are reduced), and deposit as neutral metal atoms. At the positively charged
anode there are two possible reactions, depending upon the type of cell. In an electrowinning cell, nonmetal anions
generally undergo oxidation at the anode to give gaseous products, whereas in an electrorefining cell the dissolution of
the anode metal itself occurs [30].

Three-dimensional electrode cells have been investigated extensively over the past two decades and have been
shown to be suited to applications in different areas such as electrowinning, effluent treatment and electroorganic
synthesis. The extremely high specific surface area of these new generation cells makes them attractive systems for
numerous electrochemical processes which can only be successfully carried out with low current densities. The early
research in three-dimensional electrodes was focused on the fixed and fluidized bed, especially on the latter. The main
purpose of these investigations was application of the cell for the winning of heavy metals from very dilute solutions
[31-32]. Despite early optimism the fluidized bed electrode (FBE) cell (Fig. 1) has manifested many limitations in later
investigations such as: poor conductivity of the dispersed phase at higher bed expansion, deposition of metal on the
feeder electrode and diaphragm, channeling through the bed in scaled up cells, bipolar characteristics with large
interelectrode distances, relatively short lifetime of the diaphragm etc [34, 35]. Some of these shortcomings have
seriously limited the viability of the FBE cell for metal reclamation. The disadvantages prompted the appearance of
some new types of cell, derived from the FBE cell, such as the inclined FBE cell [36], the moving bed cell [37], the
vortex bed cell [38], the spouted bed electrode (SBE) cell (Fig. 2) and rotating cylinder electrode (RCE) (Fig. 3).

Fig. 1. Schematic diagram core-annular flow structure of fluidized bed electrode (FBE) [33]

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 Fig. 2. Spouted electrochemical reactor (SER) [39]

Fig. 3. Rotating cylinder electrode (RCE) scheme [40]

3. Literature Review

Electrolysis in order to recover heavy metals from the wastes [41], Ni-Cd batteries [42], metals on the circuit
board [43] or wastewater [44, 45], the separation of arsenic as a toxic metal [46-48] and other heavy metals from solid
wastes [49] that cause many problems for the environment and soil treatment from heavy metals [50-54] has been used
up to now. Over the years a number of studies have been carried out on metal recovery by electrometallurgy. The
previous work relevant to the present study have been summarized in Table 1.

Stankovic, V.D. and Stankovic, S. [55] used the spouted bed electrode (SBE) cell with a three-dimensional
electrode to investigate the depletion process of copper ions from dilute solutions. The potentiostatic mode of operation

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gave better results for both electrowinning rate and energy consumption. Higher electrode potentials provide higher
current efficiencies. No agglomeration of the particles or deposition of metal on the feeder surface was observed.

Venkateswaran, et al. [56] studied the elctrowinning of nickel from nickel chloride electrolyte. They examined
influence of electrolyte-pH, current density, temperature and addition agent (boric acid) for better nickel deposition.
Lower energy consumption associated with the chloride route in relation with sulphate is mainly due to better
conductivity of the electrolyte and higher reversibility of electrode reactions.

Lupi, C. and Pasquali, M. [57] investigated an electrowinning and electrolysis process for Ni metal and powder
recovery from LiCoxNi1-xO2 at constant current density and constant potential, respectively. Nickel electrowinning
performed at 250 A/m2 current density, 50 ºC temperature, pH=3–3.2, with an electrolyte having about 50 g/l Ni and 20
g/l H3BO3 composition, produces a good aspect Ni deposit with acurrent efficiency and a specific energy consumption
of about 87% and 2.96 kWh/kg respectively. The electrolysis at constant potential of a solution containing 1.7–1.8 g/l of
Ni produces a very pure powder in 80 min, leaving less than 100 ppm of nickel in solution.

Kirshin, M.Yu. and Pokhitonov, Yu.A. [58] studied the deposition of palladium from nitrate solution at a
platinum electrode. In the range of potential E from +0.5 to +0.25 V, the rate of Pd deposition from 1 M HNO3 solution
was 0.7-0.9 mg.cm-2 at current efficiency of about 70%. The degree of Pd recovery by cathodic deposition is more than
99%.

Garcia-Gabaldon, M. et al. [59] evaluated the Pd (II) effect on Sn (IV) electrochemical deposition. They
analysed fractional conversion, current efficiency, space-time yield and specific energy consumption for the
electrochemical reactor. At -0.6V, relatively low values of total energy consumed and a global current efficiency value
of 74% were reached. On the other hand, at this potential value and for t100, really good values for palladium (72%) and
tin (73%) fractional conversion were obtained.

Dorikar, D.K. et al. [60] studied the electrodeposition of nickel from nickel sulphate bath in ammonia medium.
The current efficiency was found to increase with increase in acetone concentration up to 15% V/V in bath solution.
The stability of the electrowon deposited nickel powder was found to be in the range of 85 to 89 %. The average
particle size of the deposited powder in the range of 13-16 μm was found to be decreasing as the concentration of the
acetone increases.

Lai, Y-C et al. [61] studied valuable metals recovery from spent hydrodesulfurization (HDS) catalysts using
acid-leaching and fluidized-bed electrolysis process. Acid B with a volume ratio of concentrated HNO3/H2SO4/HCl =
2:1:1, was found to be better than acid A (HNO3/H2SO4 = 1:1) at leaching metals. At 70 ºC, the best S/L ratio and
leaching time were 40 g/L and 1 h, respectively, for acid B. At this condition, the first stage leaching yields reached 90,
99, and 99% for the target metals of Mo, Ni, and V, respectively. Using acid B at S/L = 40 g/L, one stage leaching, and
2-h electrolysis at a constant current density=35.7 mA/cm2, with a stable cell voltage of 5 V, the electrolytic recoveries
of Mo, Ni, and V at 2 h were 15, 61, and 66%, respectively.

Jayakumar, M. et al. [62] studied the Electrolysis of palladium (II) in nitric acid medium at platinum and
stainless steel electrodes by cyclic voltammetry. The recovery and Faradaic efficiency were significantly lowered (to
40%) in the case of electrolysis from simulated high-level liquid waste due to other interfering competitive reactions.

Nathan, W. and Michael, L.F. [63] investigated the recovery of the remaining palladium from spent electroless
bond pad plating solution by means of electrochemical deposition onto a high surface area cathode. They suggested
their recycling method as an economic and environmental friendly system.

Prajapati, R.P. et al. [64] used electro-deposition for nickel recovery from spent catalyst of nitrogenous fertilizer
industry. Their results showed that the amount of Nickel recovered increase by increasing the initial nickel
concentration, temperature and time to deposition.

Terrazas-Rodriguez, J.E. et al. [65] carried out separation of palladium from mixture of metal ions (Pd2+, Rh3+
and Nd3+) by a rotating cylinder electrode reactor (RCER) and a parallel plate reactor (FM01-LC) with the same
cathode area (64 cm2) and electrolyte volume (300 cm3). The current efficiency in the FM01-LC reactor varies between
24% and 35% while in the RCER is 40–84%. The FM01-LC reactor requires more energy per volume (1.08–2.86
kW.h.m−3) than the rotating cylinder electrode (0.56–0.88 kW.h.m−3) for the electrochemical recovery of 96–99 wt% of

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 palladium ions. In the FM01-LC laboratory reactor, 99% of palladium ions were recovered after 30 min of electrolysis
while in the RCER, 120 min were necessary. More uniform high purity palladium deposits were obtained on the surface
of the RCER.

Sivasakthi, P. and Sathaiyan, N. et al. [66] developed a electrowinning process for cobalt recovery from a
petroleum refining waste catalyst. They optimized operation condition in this way: H2SO4 concentration: 5 g/L (2.13
pH), Duration: 120 minutes, Cobalt concentration: 30 g/L, Current density: 200 A/m2, Temperature: 30°C, Stirring: Nil.
At the optimized conditions, cobalt metal foil is electrolytically recovered about 70% from the waste catalyst roasted
leached solution.

Simescu-Lazar, F. et al. [67] investigated the in situ regeneration of a Pd/C/foam catalyst by electrochemical
method using a modified Mahoney–Robinson reactor (RM). Their results demonstrated that the acid solution (0.1 M
H2SO4) was the best electrolyte in that the catalytic activity of Pd catalyst could be recovered, at ambient temperature
with low catalyst loss.

Xue, Y. et al. [68] proposed an electrochemical detoxification and recovery process for reuse the components of
the spent SCR catalysts (V2O5-WO3/TiO2) under alkaline condition. They used the electrochemical advanced oxidation
processes (EAOPs) at surface-modified carbon felt cathode, where the HO2 and highly oxidative OH are in-situ
generated from two-electron ORR and electro-Fenton-like reaction, respectively. After electro-oxidative dissolution, the
crystal structure and original composition of the catalyst support (TiO2 and WO3) are well maintained for recycle or
subsequently re-fabrication process. After dipping active component on the detoxified catalyst, the regenerated catalyst
shows a comparable SCR catalytic activity with the fresh sample.

Liwen Zhang, A. et al. [69] utilized the molten salt electrolysis for the separation of cobalt and tungsten from the
cemented carbide scrap in a NaCl-KCl melt at 750 ºC. Following 10 hours of electrolysis, under 100 mA, 0.3 and 0.6 V,
the cobalt powders of 100 nm in diameter, the tungsten powders of below 200 nm in diameter and a porous structure
carbon were obtained.

Deniz, A.B.d.C. et al. [70] evaluated the performance of electrokinetic remediation for vanadium removal from
deactivated catalysts in a fixed-bed reactor. They found that 0.5 mol.L−1 sulfuric acid concentration and electric
potential of 5 V provide the best operating conditions. Their results showed that 22.99% of catalyst vanadium content
was removed within 48 h and 81.62 kWh/kg energy consumption.

Table 1. Showing details of various experimental data and their performance

Metal Electrolyte Cathode Anode T (K) t (hr) i (A.m-2) SEC (Kwh.kg-1) C.E (%) Ref
Cu H2SO4 - - 298 <2.5 1000-3000 1-2 95 [55]
Ni HCl S.S Graphite 303-353 4 100-400 2.95 78 [56]
Ni H2SO4-H2O2 AISI 316L Pb-8Sb 298-323 2 125-250 2.91-3.18 87 [57]
Pd HNO3 Pt Pt <373 - 100-700 - 70 [58]
Sn, Pd HCl Graphite Graphite - <2.5 - 2.7 >70 [59]
Ni NH4OH S.S Graphite - 2 - - 95 [60]
Ni, V, Mo HNO3-H2SO4 S.S Iridium 343 2-4 357 - - [61]
Pd HNO3 Pt S.S 298 4-8 65 [62]
Pd - Cu Inert 298 2-24 - - - [63]
Ni H2SO4 S.S - 343 - - - - [64]
Pd, Rh, Nd HNO3 AISI 304L Pt 298 1.5-2 - 0.56-2.86 35, 62 [65]
Co H2SO4 S.S Pb-Ag 303-333 0.5-3 150-400 61.5-85.1 [66]
Pd H2SO4 S.S Pt 313 - - - - [67]
As, Ti, V, W Na2SO4 CF Graphite 298 - - - - [68]
Co, W NaCl-KCl WC-Co Graphite 1023 5 - - - [69]
V H2SO4 Pb Ti/Ru-Ir - 48 - 81.62 - [70]
i: Current density, SEC: Specific energy consumption, C.E: Current efficiency

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4. Conclusions

The use of catalysts, and hence, catalyst wastes have rapidly been increasing worldwide. Recovery of valuable
elements from spent catalysts becomes an unavoidable task not only for reducing the inventory cost of catalysts but also
for reducing the catalyst waste to prevent environmental pollution. This article provides an overview of past
achievements and present scenario of recovery studies carried out on the use of electrometallurgy method which could
serve as an economical environmentally friendly and large-scale means for recovering metals from secondary spent
sources (catalysts). Electrometallurgy is an expensive technology due to the consumption of electricity, in addition, the
electrochemical process required for this method occurs in an intermediate metal-electrolyte medium, so the efficiency
of this method is directly proportional to the interface medium level and through this limited factor gets, but on the
other hand, in the method of extraction of metals by electrolysis, the percentage recovery of high-purity metals is higher
than other methods. It seems that high performance and compatibility of this method with the environment can justify
the cost of investment and operation electrometallogy method, especially electrolysis, are more suitable than other
methods for separating metals.

This paper has reviewed the efforts made to recover metals from the spent catalyst by electrometallurgy. Based
on the study following conclusions are understood from previous works:

 The most electrochemical tests carried out in three-dimensional electrode cells equipped with HCl,
HNO3 and H2SO4 solution (electrolyte cell), stainless steel and graphite plate as were cathode (working
electrode) and anode (counter electrode), respectively at both potentiostatic approach.

 Optimum conditions for operation parameters: Temperature: 25-80 ºC, Electrolysis time: 2-4 hours,
Liquid/Solid ratio: 5-25 ml/gr and Current density: 100-400 A/m2.

 Specific energy consumption and Current efficiency in optimum conditions were 3 Kw.h/kg and >75%,
respectively.

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