RESEARCH FRONT

CSIRO PUBLISHING Full Paper

www.publish.csiro.au/journals/ajc Aust. J. Chem. 2009, 62, 341–347

Processing of Electric Arc Furnace Dust using

Deep Eutectic Solvents

Andrew P. Abbott,A,C John Collins,B Ian Dalrymple,B Robert C. Harris,A

Reena Mistry,A Fulian Qiu,A James Scheirer,A and William R. WiseA
A Chemistry Department, University of Leicester, Leicester, LE1 7RH, UK.
B C-Tech Innovation Ltd, Capenhurst Technology Park, Chester, CE1 6EH, UK.
C Corresponding author. Email: [email protected]

The present paper describes the design and operation of the first large-scale extraction and separation of metals from a
complex matrix using an ionic liquid. The liquid was a deep eutectic solvent based on choline chloride. The hydrogen-
bond donors were mixed to optimize solubility and fluid viscosity. It was found that the incorporation of a fine particulate
dust actually decreased the viscosity of the fluid. The present paper shows that selective extraction of zinc and lead can
be achieved through judicious choice of the hydrogen-bond donor and it is also shown that metals in solution can be
separated using cementation with zinc powder. Electrowinning of pure zinc is demonstrated but scale-up tests suggest
that the process is relatively slow and has poor current efficiency. An alternative methodology was developed to rapidly
recover the zinc from solution using dilute ammonia solution. It is also shown for the first time that cementation can be
efficiently carried out in ionic liquids because the recovered metal is porous and allows thick layers to be deposited.

Manuscript received: 2 November 2008.

Final version: 7 February 2009.

Introduction that they can be used for the biphasic extraction of Cs+ and Sr2+ .
The processing of metal oxides is essential for metal extrac- Nockemann et al.[11] have used protonated betaine bistriflamide
tion, waste recycling, and catalyst preparation. One of the salts to dissolve metal oxides such as UO2 , ZnO, CdO, and HgO.
major difficulties with metal oxides is that they are insoluble The metal salts can be stripped from the ionic liquids by treatment
in most molecular solvents and generally require strong aque- with acidic aqueous solutions. The two phases were miscible
ous mineral acids for their dissolution. Separation has usually above 55◦ C but separated below this temperature.
been achieved using solvent extraction with specific chelating The area of imidazolium-based ionic liquids with discrete
agents for given metals. Over the past 10 years, there have been anions as extraction solvents has recently been reviewed by
significant developments in the use of ionic liquids. Ionic liq- Dietz.[12] The review covers the use of neutral and anionic
uids have been of considerable interest for a wide variety of complexing agents such as crown ethers and organophosphorus
applications including synthesis, electrochemistry, and sepa- acids. The use of task-specific ionic liquids has been reviewed
ration science.[1–3] An increasing number of groups are now separately by Davis.[13]
using ionic liquids for solvatometallurgical processing. These In a different approach, we have shown that ionic liquids
are primarily using imidazolium-based liquids and a significant can also be formed by taking quaternary ammonium salts and
number of studies have concentrated on uranium processing. Dai complexing them with simple hydrogen-bond donors (HBD)
et al.[4] studied the dissolution of UO3 in imidazolium chloro- such as amides[14] and carboxylic acids.[15] These mixtures form
aluminate melts. The solubility was found to be in the range eutectics where the depression of freezing point can be up to
1.5–2.5 × 10−2 M in Lewis basic melts and the main metallic 200◦ C. The mixtures have been shown to have similar solvent
species in solution was found to be [UO2 Cl4 ]2− . The solvation properties to ionic liquids with discrete anions but clearly have
of uranium and europium ions in these liquids has been modelled the advantage that they are easier to produce on a large scale,
by Chaumont and Wipff.[5] which has obvious implications for metal recovery processes.[16]
Issues associated with water sensitivity of chloroaluminate We have shown that these types of ionic liquids can dissolve a
melts can be overcome using discrete anions such as PF− 6 and range of metal oxides[17] and they can be used to separate met-
(F3 CSO2 )2 N− and this is where most studies have focussed als from a complex mixture using electrochemistry.[18] These
recently. Dai et al.[6,7] have used crown ethers and calixarenes liquids are, however, all totally miscible with water and can-
to extract a range of metals from aqueous solutions. Studies by not be used for biphasic extraction. The solubility of 17 metal
Rogers et al. used azonaphthols and crown ethers[8] in a similar oxides in the elemental mass series Ti through Zn was reported
manner. in three ionic liquids based on choline chloride.[19] This has
Recently Visser et al.[9,10] have also developed a new class of also been shown for the practical application of recovering
task-specific ionic liquids with monoaza-crown ether fragments Zn and Pb from a waste material produced by the electric arc
covalently attached to the imidazolium cations and have shown furnace (EAF).[18]

© CSIRO 2009 10.1071/CH08476 0004-9425/09/040341

RESEARCH FRONT

342 A. P. Abbott et al.

An EAF is one of the most commonly used methods for the 35 Zn

production of steel and is primarily used in the remelting of Pb
scrap steel. The EAF used in steel making and recycling has 30
become a very intensive and rapid process. It involves passing a

Extraction efficiency [%]

high-energy electric current (∼450–500 KWh tonne−1 ) through 25
ferrous scrap and alloying elements to produce molten steel.
Approximately 15–20 kg of dust is formed per tonne of steel 20
but the high content of metals such as Pb and Cd mean that the
waste is classified as toxic. The dust forms when volatile met- 15
als, such as zinc and lead, are vapourized at the high operating
temperature and several million tonnes of dust are produced per 10
annum. There are several different treatment processes that are
either commercial operations or at a developmental stage,[20,21] 5
and these include: high temperature metal recovery, hydromet-
allurgical processes and vitrification or chemical stabilization 0
2 urea 1.5 urea:0.5 EG 1 urea:1 EG 0.5 urea:1.5 EG 2 EG
treatments. In the current work, we demonstrate the optimiza-
tion of the extraction process and the selective cementation HBD composition
of lead.
Fig. 1. Extraction efficiency of Pb and Zn from the arc furnace dust at
50◦ C in deep eutectic solvent of various compositions after 72 h. HBD,
Results and Discussion hydrogen-bond donors.
Small-Scale Optimization
It has previously been shown that using urea-based deep eutec- 3.0  10
7
tic solvents (DES) (1 mol equiv. ChCl:2 urea) offers selective
dissolution of Zn and Pb oxides from EAF dust while showing 2.0  10
7
negligible solubility for iron oxides.[18,19] A process for treating 1.0  10
7
EAF dust will therefore involve three steps: extraction of lead
and zinc from matrix, isolation of lead, and recovery of zinc. The 0.0
I [A]

main issue with the use of the urea-based eutectic is the relatively

1.0  10
7
high viscosity (∼800 cP at 298 K), which makes it much more
difficult to pump the fluid and to filter the undissolved dust. To
2.0  10
7 Pb
reduce the viscosity of the solvent, different molar amounts of
ethylene glycol were used with urea to form hybrid DESs with
3.0  10
7
Zn
the molar ratio 1:2 (ChCl:HBD).
4.0  10
7
Fig. 1 shows the extraction efficiency for Pb and Zn from the

1.0
0.8
0.6
0.4
0.2 0.0 0.2 0.4 0.6
arc furnace dust with different molar ratios of DES. These exper-
E [V]
iments were carried out using 0.1 g of dust and 10 mL of DES. It
can be seen that the extraction efficiency is relatively unaffected
Fig. 2. Cyclic voltammogram at 0.5-mm Pt disc electrode in
by composition, even down to only 0.5 mol equiv. of urea. The ChCl/urea/ethylene glycol (1:0.5:1.5) after extraction of electric arc furnace
efficiency for Zn drops significantly, however, with only ethyl dust (scan rate = 20 mV s−1 ).
glycol (EG) as the HBD. The viscosity of the 0.5 mol equiv.
of urea liquid was only 56 cP compared with 800 cP in the
1 ChCl:2 urea. For all subsequent studies, the liquid used was the
1 ChCl:1.5 EG:0.5 urea. For all systems, the Fe content was less process, a sacrificial metal with a more negative redox poten-
than 1 ppm, showing that the extraction efficiency is effectively tial than the metal being recovered is immersed in the solution.
zero, ensuring the desired selectivity of the process. The metal ions in the liquid are reduced and deposited onto the
sacrificial metal, which in turn is oxidized and goes into solu-
tion. In aqueous solutions, this tends to be an inefficient process
Zinc–Lead Separation because the immersion deposit is dense and precludes dissolu-
It has previously been shown that electrolysis of EAF dust extract tion of the underlying metal. Although cementation to recover
yields a zinc-rich lead alloy with no traces of any other metals.[18] metals from solution has not been used before for ionic liquids,
What is needed is a selective method to separate zinc from lead in we have recently shown that immersion deposits of silver on cop-
solution in a quick and efficient way. When the EAF dust was dis- per and copper on aluminium can be obtained.[23] The deposits
solved in the hybrid solvent, the resulting voltammogram showed are porous and sustained deposition can be achieved. For the
a significant difference from that in 1 ChCl:2 urea previously current case, the process is Pb2+ + Zn(s)
Pb(s) + Zn2+ , which
reported.[18] Differences have also been observed for the depo- is ideal because zinc metal is an inexpensive substrate that will
sition of Zn–Sn alloys in urea- and ethylene glycol-based liquids be recovered in the final stage of the process.
and these have been ascribed to differences in speciation.[22] A sample of EAF dust was extracted using the 1 ChCl:1.5
Fig. 2 shows that separate signals for the two metals are observed EG:0.5 urea mixture at 50◦ C for 2 days. The resultant liquid was
and these are separated by ∼500 mV, which suggests that the filtered and a zinc sheet was immersed for 2 days at 25◦ C. At
metals could be separated potentiometrically; however, practi- the end of this time, a black deposit was produced and energy
cally this is difficult to scale up and leads to impure products. A dispersive X-ray spectroscopy (EDAX) analysis of the sample
common alternative in aqueous solutions is cementation. In this showed the only metal present on the surface was lead. This
 RESEARCH FRONT

Processing of Electric Arc Furnace Dust 343

100

2h
8.0  10
6 4
80
6
8
6.0  10
6

% Pb extracted
20
0 60
I [A]

4.0  10
6
40

2.0  10
6
20
0.0

1.0
0.5 0.0 0.5 1.0 0

0 2 4 6 8
E [V] Time [h]

Fig. 3. Anodic stripping voltammetry for 3.4 × 10−3 mol dm−3 PbCl2 in 1 ChCl:0.5 urea:1.5 EG at 50◦ C (scan rate = 20 mV s−1 ). A Zn sheet, area: 14 cm2 ,
was immersed in the liquid and voltammograms were run after different lengths of time (left) and graph of lead extracted as a function of time (right).

60 1.16
Neat
Neat
1 wt-%
50 1.14 1 wt-%
2 wt-%
5 wt-% 2 wt-%
1.12 5 wt-%
40 10 wt-%
10 wt-%
Density [g cm
3 ]
Viscosity [cP]

1.10
30
1.08
20
1.06
10
1.04

0 1.02
20 30 40 50 60 70 80 20 30 40 50 60 70 80
Temperature [C] Temperature [C]

Fig. 4. Viscosity (left) and density (right) as a function of temperature for a 1 ChCl:1.5 EG:0.5 urea deep eutectic solvent containing various amounts of
electric arc furnace dust.

shows that cementation can be used as a method for achieving a series of scale-up experiments were performed using 75 kg of
effective separation of Pb from Zn in the EAF dust. liquid and 5 kg of dust.
To determine the kinetics of lead cementation, voltammetry
for 3.4 × 10−3 mol dm−3 PbCl2 in 1 ChCl:0.5 urea:1.5 ethy-
Scale-Up
lene glycol at 50◦ C was performed (note: no ZnCl2 present).
A Zn sheet (area = 14 cm2 ) was immersed in 10 mL of the liq- Dust Loading
uid and voltammograms were run after different lengths of time. The first issue to be addressed was one of dust loading in the
The results are shown in Fig. 3. This looks different from the DES for the large-scale experiments. In aqueous solutions, the
anodic response in Fig. 2 as no alloy is being formed. From addition of finely divided dust causes a significant increase in
the area under the peaks, the concentration of lead remaining in the solution viscosity. The effect of EAF dust loading on vis-
the liquid was determined and the rate of extraction was found cosity and density of the ChCl:urea:EG hybrid was determined
to be 3 × 10−7 mol cm−2 h−1 . The experiment in Fig. 3 was as a function of dust loading weight and temperature. Fig. 4
repeated with a considerably decreased amount of Zn powder shows that when 1 wt-% EAF dust is added to the ionic liquid,
(0.02 g = 1.5 equiv. of Zn) added to 3.4 × 10−3 M PbCl2 dis- the viscosity decreases by ∼50% at all temperatures. This is a
solved in a mixture of 1 ChCl:0.5 urea:1.5 EG. The high surface remarkable observation and has also been observed for other
area of zinc dust means that almost all the lead can be extracted small particle species in these DESs.[24]
in the above solution in ∼10 min, using significantly less Zn Ionic liquids in general are viscous and it has been shown
than in the sheet. This shows that cementation is an extremely that this is due to the large ions and the small void volume in the
effective method of extracting lead from the solution. liquid.[25] The decrease in viscosity on addition of solid can be
Electrolysis of the resulting liquid using a mild steel cathode explained by the dust particles breaking up the structure of the
at a current density of 2.5 A dm−2 resulted in the deposition of ionic liquid. Movement of the particles will cause microscopic
a thick, dark grey metallic film. EDAX confirmed that this was stirring and allow improved mass transport. This is potentially a
only zinc with no traces of lead. Based on the above protocol, very useful concept for improving mass flow in ionic liquids. The
RESEARCH FRONT

344 A. P. Abbott et al.

Zn dust

EAF dust
Electrolysis cell

Zn

Zn/Pb/Cd
Pb

Cementation tank

Leach tank

Fig. 5. Schematic diagram of the cell for extracting lead and zinc from electric arc furnace (EAF) dust together with a photograph of the pilot plant built
for 5 kg dust extraction batches.

addition of up to 5 wt-% causes no further change in viscosity. 80

The addition of 10 wt-% causes an increase in the viscosity but it
is still lower than that of the pure fluid. The addition of dust also 70
has a negligible effect on the density of the liquid, presumably 60
because the dust has a similar density to the ionic liquid, which
Extraction efficiency

can be seen in Fig. 4.The effect of the particulates on the structure 50

is difficult to quantify because the solubility of metals will have
Zn
an effect on viscosity. However, recent analogous studies with 40
Pb
alumina, which is insoluble, showed that the effect is real and it
was possible to show that there is an increase in free volume of 30
∼17% when 0.05-µm particles are added.[24] It was decided for
20
the large-scale experiments to use a dust loading of 7 wt-%.
Fig. 5 shows schematically the pilot plant that was built for 10
the extraction process. The main extraction tank has a capacity
of 125 L and there were 2 × 25 L tanks in which batches could be 0
treated to remove lead using cementation with Zn dust, followed 0 500 1000 1500 2000 2500 3000
by a 12-L electrolysis cell. Fig. 5 also shows a photograph of the t [min]
plant constructed for this purpose.
Fig. 6. Extraction efficiency of Pb and Zn from the arc furnace dust at
50◦ C in the hybrid deep eutectic solvent as a function of time.
Extraction Efficiency
Fig. 6 shows the extraction efficiency for the same batch of EAF that the zinc was present in several forms including franklin-
dust at a 5-kg scale as a function of time. Comparison of Figs 1 ite, ulvospinel, and small quantities of cuprospinel. Franklinite
and 6 shows that scale-up improves the extraction efficiency for was by far the major spinel structure found. It can exist in sev-
zinc although the extraction of lead is slightly decreased. This eral different forms, the main one of which has the formula
may be because the solution is close to its saturation concen- (Zn,Mn,Fe)2+ (Fe,Mn)3+ 2 O4 , and the spinel has an isometric
tration for total metal content. The increased extraction of zinc crystal system. Ulvospinel has the formula Fe2TiO4 and also
compared with the small scale is probably due to increased stir- has an isometric crystal system. These materials are notoriously
ring, which allows better mixing of the dust and DES. Although difficult to dissolve in aqueous media; however, as they typically
increased solubility was obtained, not all of the zinc could be constitute half of the dust, the DES is probably dissolving some
extracted even after 72 h. This could be due in part to the speci- of these phases in the large-scale experiment, albeit slowly.[26,27]
ation of the zinc. X-Ray powder diffraction analysis was carried It can be seen from Fig. 6 that a significant amount of the Zn
out on the undissolved dust after extraction and it was found has dissolved after 24 h, which is a viable time for an extraction
 RESEARCH FRONT

Processing of Electric Arc Furnace Dust 345

2A
35000 2.5
80
3
30000 3.5
70 4
Concentration [ppm]

25000 5

Current efficiency [%]

6
20000 60

15000 50
10000
40
5000
30
0

0 20 40 60 80 100 120 20
2 3 4 5 6 7
Time [h]
Time [h]
Fig. 7. Concentration of zinc as a function of time during the depletion test
carried out at 3.5 A. Fig. 8. Current efficiency for the electrowinning of zinc from the hybrid
deep eutectic solvent at 50◦ C as a function of applied current.

time. Clearly, by increasing the temperature, extraction rates, and

possibly efficiency can be improved, but this is a parameter that
still has to be optimized. Filtration on a small sale was carried to determine the current efficiency of the process. These data
out using a 0.45-µm mesh filter and syringe. This resulted in a are shown in Fig. 8. It can be seen as in most electrowinning
clear solution. On a large scale, the DES was filtered through processes that the current efficiency decreases as the applied
a double bag filter (both 1-µm mesh size) and this removed voltage increases such that the efficiency is relatively poor (75
the majority of the suspended particulate matter (which was to 32%) with voltages that yield reasonable deposition rates. The
in the range 0.5–3 µm). There was still a significant turbidity extraction efficiency also decreases as the zinc concentration in
to the solution and the filtration is still an issue that needs to be solution decreases. Exhaustive electrolysis was carried out over
addressed, although it is not significantly different to filtration a 72-h period, at the end of which the cathodes were analyzed
of any other fine particulate suspension. using EDAX. It was found that there were no traces of lead in
the deposit. The zinc morphology is shown through an scanning
Pb Cementation electron microscopy image of the surface in Fig. 9, together with
a photograph of the electrode.
A 20-L aliquot was taken from the extraction tank and 100 g of The results in Figs 7 and 8 show that the electrowinning of
zinc dust was added. After 2 h, a sample of DES was taken and zinc from solution is slow and current-inefficient and probably
the Zn and Pb concentrations were determined using inductively economically unfavourable on a large-scale owing to the low
coupled plasma–atomic emission spectrometry (ICP-AES). value of zinc metal. An alternative approach would be to pre-
The Pb concentration was reduced by 75% and a concomitant cipitate the metal from solution with a complexing agent that
increase in the Zn concentration was observed, showing quan- forms an insoluble species. This has the potential advantage that
titative exchange of the two metals in solution. The experiment a higher-value product could be obtained.
was repeated four times and the residual lead concentration was It has previously been shown that iron, chromium, and nickel
found to be 12 ppm on average, which was close to the back- could be precipitated from a DES that had been used for elec-
ground level. The amount of lead removed depended strongly tropolishing by the addition of an equal volume of water.[28] The
on the concentration of zinc in solution. When the zinc concen- DES was filtered and regenerated by evaporating off the water.
tration was 4000 ppm, 97% of the lead was removed but when the This was attempted with the leachate from tank 2 but found to be
Zn concentration was 12000 ppm, only 63% was removed. This ineffective at precipitating zinc. It is well known that ammonia
would be expected because the difference between the Zn2+/0 solution is an extremely effective precipitating agent for zinc in
and Pb2+/0 couples will be governed by the Nernst equation, aqueous solutions.[29] Various concentrations of ammonia solu-
which will accordingly affect the equilibrium constant. Inter- tion were added to aliquots of the leachate and the results in
estingly, on cementation, the lead aggregated to form large Fig. 10 show that dilute solutions are extremely effective at pre-
‘shot’-sized clusters that settled rapidly to the base of the cell, cipitating Zn from solution. This is most likely due to partial
simplifying separation. ammination of Zn that is not as soluble in the ionic liquid/water
as the fully amminated Zn species.[29] The rate of precipitation
Zn Recovery was greatest in the 1.75 mol-% and 3.5 mol-% solutions, with
Following the cementation step, a 10-L aliquot was run into the an almost immediate precipitation being observed. In the higher
electrolysis tank. This was fitted with a steel cathode (surface concentrations, the precipitation took longer and in the 26 and
area = 456 cm2 ) sandwiched between two iridium oxide-coated 35% tests, the precipitation occurred after being left overnight at
titanium plate anodes, each of similar surface area. The solutions 3◦ C. Small-scale tests showed that this liquid could be regener-
were electrolyzed at constant voltage and samples were taken at ated by filtration and then evaporation of the ammonia solution
regular intervals to determine the residual Zn levels in solution. from the liquid. The resulting liquid was slightly depleted of urea
Fig. 7 shows the concentration of zinc in solution as a func- owing to decomposition at higher temperatures but this could be
tion of time and applied voltage. The cathode was also weighed easily added to bring the liquid back to its original composition.
RESEARCH FRONT

346 A. P. Abbott et al.

Acc.V Spot Det WD 20 µm

20.0 kV 5.0 SE 9.7

Fig. 9. Scanning electron microscopy (left) and photograph (right) of cathode after 7 h electrowinning at 50◦ C, 2.5 A, and at 40 rpm pump speed.

30000 Table 1. Average composition of electric arc furnace dust

25000 Element analyzed Average wt-% composition

Zn 33.2
20000 Pb 2.7
Zn [ppm]

Fe 33.3
Mn 3.7
15000 Ca 5.7
Mg 1.8
10000

5000
Experimental

5 0 5 10 15 20 25 30 35 40
Ammonia concentration in solution [%] Choline chloride [HOC2 H4 N(CH3 )+ −
3 Cl ] (Aldrich, 99%) was
recrystallized from absolute ethanol, filtered, and dried under
Fig. 10. Plot of Zn concentration remaining in ionic liquid after washes vacuum. Urea and ethylene glycol (both Aldrich, >99%) were
with various concentrations of ammonia solution. used as received. The mixtures were formed by stirring the com-
ponents together at 100◦ C until a homogeneous, colourless liquid
formed. The viscosity was determined using a Brookfield DV-E
viscometer fitted with a thermostatted jacket. Metal solubility
was determined by placing 0.1 g of the metal oxide (various
Conclusions
sources, all >98%) in 10 mL of the ionic liquid for 3 days at
The present work shows that metals can be extracted from solid 50◦ C. The solution was filtered at 50◦ C, diluted with 0.1 M HCl
matrices using DESs. Effective separation can be achieved by and analyzed using a JY Ultima 2 ICP-AES. The EAF dust is
selective dissolution through appropriate choice of the HBD, highly variable in composition depending on the batches of scrap
cementation of the metal in solution, electrowinning of the used. For the current research, one sample was used and the aver-
metal in solution or precipitation of the metal by addition of an age content of metals is shown in Table 1. The pilot plant was
aqueous-based complexing agent. This is a generic technology custom-built by C-Tech Innovation Ltd (Chester, UK).
that could be applied to a wide variety of matrices. The simplic-
ity in terms of synthesis and constituents means that this can be
applied to large-scale extraction. The inclusion of powders does References
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