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Hydrometallurgy: Yunjiao Li, Vladimiros G. Papangelakis, Ilya Perederiy

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55 views9 pages

Hydrometallurgy: Yunjiao Li, Vladimiros G. Papangelakis, Ilya Perederiy

niclek slag

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Bayu Muhammad
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Hydrometallurgy 97 (2009) 185–193

Contents lists available at ScienceDirect

Hydrometallurgy
j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / h yd r o m e t

High pressure oxidative acid leaching of nickel smelter slag: Characterization of feed
and residue
Yunjiao Li, Vladimiros G. Papangelakis ⁎, Ilya Perederiy
Department of Chemical Engineering and Applied Chemistry, University of Toronto, 200 College Street, Toronto, Ontario, Canada M5S 3E5

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

Article history: Discarded slags have potential adverse environmental impact and valuable metal contents. High pressure
Received 2 October 2008 oxidative acid leaching (HPOXAL) was employed to clean a slow-cooled copper–nickel flash smelter slag
Received in revised form 9 March 2009 containing about 1% Cu and 1% Ni and selectively leach the contained base metal values. Characterization of
Accepted 10 March 2009
the slag and leach residues was carried out using powder X-ray diffraction (PXRD), scanning electron
Available online 26 March 2009
microscopy (SEM) and particle size analysis (PSA). It was found that the copper–nickel smelter slag was
Keywords:
composed of major crystalline fayalite and minor amorphous silica phases with trace amounts of magnetite
Smelter slag and entrapped matte, existing as uneven and finely dispersed particles, which are responsible for the loss of
Pressure acid leaching base metals. Most of the copper in the slag appeared as sulfide, while most of the nickel existed in the oxide
Base metal dissolution form with a minor portion as sulfide. Cobalt and zinc phases were rarely detected because of their low
Fayalite content. During high pressure oxidative acid leaching, temperature and acidity were the key variables
Hematite controlling the leaching of the base metals and iron. At 250 °C and 20% acid addition, N 99% Ni, Co and Cu
could be extracted into solution together with 94% Zn and b 2.2% Fe. Iron and silicon were transformed into
crystalline hematite and amorphous silica in the residue. By adjusting the acidity to control the rate of
fayalite dissolution and the growth of precipitates, flower-like hematite particles associated with amorphous
silica were produced. An excellent slurry filtration rate of 0.36 m3·m− 2·h− 1 was obtained.
© 2009 Elsevier B.V. All rights reserved.

1. Introduction blister copper (Gonzalez et al., 2005). Historic copper smelting at


Penn Mine (1865–1919) generated approximately 200,000 m3 of slag
Non-ferrous slags are waste by-products produced in the proces- that was piled in an area immediately adjacent to the Mokelummne
sing of ores or concentrates by smelting and converting. During these river channel, causing water contamination and fish poisoning
operations, iron sulfide is oxidized to iron oxide and chemically (Parsons et al., 2001). Canadian operations of Vale Inco dispose of
combines with silica to produce a fayalite (Fe2SiO4) slag. Copper and more than a million tons of slag annually, whereas the total inventory
nickel-enriched sulfide melt settles beneath the slag as matte. of Vale Inco's slag in the Sudbury area (Ontario, Canada) after
Generally, slags from non-ferrous smelting and converting operations ~90 years of operation should be more than 120 million tons.
contain 32%–52% iron that exists in the forms of fayalite (major) and Metallurgical slags produced from lead–zinc primary and secondary
magnetite (minor) (Curlook et al., 2004; Shen and Forssberg, 2003; sources have been defined by the European Community either as
Gbor et al., 2000a,b). Appreciable amounts of metal values, such as hazardous materials or as commercial substances (Ettler et al., 2002).
nickel, cobalt, copper and zinc, are present in the slag, thus Considering the environmental impact and the quantity of dumped
contributing to base metal losses and potential environmental slags, it has become essential to find a way to recover the valuable
pollution from waste slag disposal. metals and clean up the waste slags.
It was reported in 1994 that approximately 4 million tons of copper The base metal losses in slags are of two main types: dissolved
smelter slag were produced each year in the United States (Collins and oxides or entrained sulfides (matte). Base metals in slags can be
Ciesielski, 1994), while the annual production of nickel, lead and zinc recovered through slag-cleaning operations. A number of studies have
smelter slags was estimated to be in the range of 0.5 to 1.0 million focused on atmospheric leaching (Herreros et al., 1998; Banza et al.,
tons. More recently, in Chile, seven copper smelters produced 3.5– 2002; Altundogan et al., 2004; Anand et al., 1980) and high pressure
4 millions tons of slag each year along with about 1.5 million tons of oxidative acid leaching (Curlook et al., 2004; Baghalha et al., 2007; Li
et al., 2008; Klein and Stevens, 1972; Anand et al., 1983; Sobol, 1993). It
was found from our previous work (Curlook et al., 2004; Baghalha
⁎ Corresponding author. Tel.: +1 416 978 1093; fax: +1 416 978 8605. et al., 2007) that a slow-cooled smelter/converter slag with a
E-mail address: vladimiros.papangelakis@utoronto.ca (V.G. Papangelakis). crystalline structure could be leached more easily by an HPOXAL

0304-386X/$ – see front matter © 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.hydromet.2009.03.007
186 Y. Li et al. / Hydrometallurgy 97 (2009) 185–193

Table 1
Chemical and mineralogical composition of slag.

Element Ni Co Cu Zn Al Si S Mn Mg Ca Fe(II) Fe(III)


% wt 1.018 0.244 1.070 0.141 1.65 17.7 1.54 0.05 0.80 0.79 34.7 5.10

Mineral Fe2SiO4 Fe3O4 SiO2 Al2O3 MgO CaO Othersa


wt.% 58.7 10.6 20.5 3.1 1.3 1.1 4.7
a
Including base metal oxides and sulfides.

process than a quenched slag with an amorphous structure. Extraction of the degree of crystallization were carried out by powder X-ray
of about 95% Ni and Co was obtained from slow-cooled converter diffraction analysis (XRD) with a Cu-Kα radiation source, using a
slags. Philips XRD system. The general morphology and approximate
In the HPOXAL process, the liberation of metals from fayalite particle size were observed using a JEOL JSM-840 scanning electron
matrix and the precipitation of hematite are two most important steps microscope (SEM) at 15 kV for scanning electron and at 20 kV for
in the selective recovery of valuable metals (Li et al., 2008). Iron backscattered electron (BSE) measurements. Powder particles were
precipitation, in particular, directly impacts the rate of solid–liquid dispersed on a conductive tape and gold coated for morphology
separation. However, few researchers focused on the characterization observation. A polished section was prepared from a slag block and
of slags and the acid-leached residues. Gbor et al. (2000a) reported on scanned across the interface to obtain phase images with back-
the characterization of smelter slags by optical microscopy, SEM/EDX scattered electrons. Energy dispersive spectrometry (EDX) micro-
and XRD, but did not give detailed information on the nature of base analysis was performed on various sample regions. Because of the
metals and/or matte droplets in the slags. Since knowledge about the very fine particle sizes and mixed structures of the materials, the X-ray
form and structure of fayalite slags and leach residues may help microanalysis was inevitably biased by the surrounding particles or
uncover the mechanism of the HPOXAL process, a detailed investiga- structures.
tion was undertaken using X-ray diffraction (XRD), scanning electron
microscopy (SEM) and particle size analysis (PSA). 3. Results and discussion

2. Experimental 3.1. Characterization of slag

2.1. Slag preparation and leaching The chemical composition of the slag determined by ICP-AES is
shown in Table 1. Iron and silicon are, of course, the main elements
The block slag as-received from Vale Inco's nickel smelter was that occur mainly in the form of fayalite and account for 57.5 wt.% of
crushed and then ground in a ball mill, and dry-sieved to less than the slag mass. Nickel and copper each constitute around 1% of slag
150 µm. It was then separated into small portions for each experiment mass together with some cobalt (0.24 wt.%) and zinc (0.14 wt.%).
through multiple splitting. Sulfur accounts for 1.54 wt.% as sulfide phases.
Slag leaching was conducted in a 2-L titanium batch autoclave Fayalite, the main component of slag, is the iron-rich end member
(Model 4524 Reactor, Parr Instrument Company) equipped with an of olivine solid-solution with an ideal formula of Fe2SiO4 or 2FeO·SiO2.
acid injector and a water-cooled titanium sampling line with an in- It crystallizes in the orthorhombic system with cell parameters a
situ graphite filter. Temperature was controlled with an accuracy of 4.82 Å, b 10.48 Å and c 6.09 Å. Fayalite can be dissolved in acid even at
±1 °C. Oxygen was introduced through a tantalum dip tube, with its pH 2 in fully oxygenated and anoxic solutions to release iron and silica
overpressure and flow rate controlled by two Brooks pressure and (Santell et al., 2001). This property makes it ideal for the liberation of
flow controllers, model 5866RT. Details of the experimental setup and valuable encapsulated metals by acid leaching.
procedure have been given previously (Li et al., 2008). Leaching was The diffractogram shown in Fig. 1 confirmed that the slag consists
run in the restricted flow rate mode until the completion of chemical of crystalline fayalite with magnetite and some unidentified minor
reactions in order to negate the effect of overpressure fluctuations. phases. The distinctly strong and narrow fayalite peaks demonstrate a
After that oxygen overpressure was allowed to climb to the set point, high degree of crystallinity obtained during slow cooling (Baghalha
regulated by a pressure controller. Vapour pressure fluctuations taken et al., 2007; Curlook et al., 2004). The weak peaks detected at 2θ values
into account by reading temperature. Autoclave cooling was per-
formed for approximately 30 min, until the temperature dropped to
70 to 80 °C.

2.2. Chemical analysis

The slag and residue samples were digested in aqua regia at 80 °C


for 3 h, filtered and then diluted with 5 vol.% HNO3 for elemental
analysis by inductively coupled plasma-atomic emission spectrometry
(ICP-AES, Perkin Elmer, Optima 3000).
The analysis of free acid in leach solutions, corresponding to total
sulfate minus that stoichiometrically bound to metals as electrolyte
salts, was performed by standard alkali titration in the presence of
CaCDTA with a TitroLine 96 titration unit. Iron(II) was determined by
potassium dichromate redox titration.

2.3. Characterization

Particle size analysis was carried out with a Malvern Mastersizer S


Particle Size Analyzer. Phase structure identification and confirmation Fig. 1. Powder XRD pattern of slag.
Y. Li et al. / Hydrometallurgy 97 (2009) 185–193 187

Fig. 2. BSE images and EDX spectra of a slag sample.

Fig. 3. BSE images and EDX spectra of a matte particle.


188 Y. Li et al. / Hydrometallurgy 97 (2009) 185–193

of 30.22°, 35.58°, 43.30°, 57.08° and 62.70° are consistent with the Fig. 2 shows the SEM/EDX results for a block-sectioned slag sample. A
existence of spinel magnetite which is formed under high oxygen backscattered electron (BSE) image shown in Fig. 2(a) is accompanied
overpressure at a high temperature during smelting (Gilchrist, 1989). by a higher-resolution, enlarged view–Fig. 2(b). Four distinct phases,
The rough baseline in the XRD pattern shows that there are some fayalite, silica, matte and magnetite, with different colors and brightness
amorphous constituents — most likely metal oxides combined with were identified. EDX measurements were carried out on different areas
silica, such as 2MgO·SiO2. Other ferrites (minor or trace) that could be and the typical EDX spectra are shown in Fig. 2(c) to (f). The bright
present include ZnO·Fe2O3 and CaO·Fe2O3. Assuming magnetite is the white-colored small dots (Area 1), with an average particle size of
only significant phase containing Fe(III), the slag is estimated to approximately 10 μm, contain major sulfur and iron as well as trace
contain 10.6% of magnetite and 58.7% of fayalite by weight based on amounts of nickel and are entrapped matte droplets. This was confirmed
the chemical analysis shown in Table 1. Based on the silicon content, by the EDX spectrum shown in Fig. 2(c). It can be seen that the matte
20.5 wt.% is SiO2 present as free amorphous silica or metal silicates, droplets are finely and unevenly embedded in the slag in different
except for fayalite. The rest of the slag (10.2%) includes metal oxides particle sizes ranging from 2 to 20 µm (Fig. 2(a)). The large dark grey-
such as MgO, CaO, Al2O3, etc. colored region (Area 2) is fayalite. As expected, large amounts of silicon

Fig. 4. X-ray elemental mapping of a slag sample.


Y. Li et al. / Hydrometallurgy 97 (2009) 185–193 189

(HPOXAL) is a very suitable process for the selective recovery of the


base metals from slags (Baghalha et al., 2007; Li et al., 2008).

3.2. Behaviour of base metals and iron during leaching

During HPOXAL, base metals enter the aqueous solution in a


soluble sulfate form via the acid dissolution of oxides and oxidation of
sulfides (Li et al., 2008). Simultaneously, iron in the fayalite and
magnetite phases is easily dissolved into the solution at a high
temperature under acidic conditions and Fe(II) is then oxidized to Fe
(III) by oxygen. In terms of chemistry and process conditions, slag
HPOXAL combines the traits of High Pressure Acid Leaching (HPAL) of
laterite ores and total pressure oxidation of sulfide minerals
(Whittington and Muir, 2000; Wilmot et al., 2004)
It was reported that Fe(III) in the solution inhibited fayalite
dissolution because the Fe(III) absorbs and passivates the mineral
surface (Santell et al., 2001). However, Fe(III) precipitates almost
instantaneously as insoluble hematite at elevated temperatures which
Fig. 5. Effect of temperature on base metal extractions. Solid loading 20%; acid addition
33 wt.%; PO2 500 kPa; time 120 min (adapted from Li et al., 2008). reduces the passivation by Fe(III). The reactions can be described as
follows:

Fe2 SiO4 þ 2H2 SO4 ¼ 2FeSO4 þ 2H2 O þ SiO2 ð1Þ


and iron as well as a trace portion of magnesium appeared in this area, as
shown in Fig. 2(d). The EDX spectrum in Fig. 2(e) came from the small Fe3 O4 þ 4H2 SO4 ¼ FeSO4 þ Fe2 ðSO4 Þ3 þ 4H2 O ð2Þ
dark-colored region (Area 3). Obviously, the predominant counts of
silicon and small counts of potassium, calcium and aluminum in Fig. 2(e)
1
indicate that silica is in a mixture with some (K, Ca, Al)-containing 2FeSO4 þ =2 O2 þ H2 SO4 ¼ Fe2 ðSO4 Þ3 þ H2 O ð3Þ
silicates such as feldspar. No phase differences can be distinguished in
this black area due to the limited resolution at a low magnification. The Fe2 ðSO4 Þ3 þ 3H2 O ¼ Fe2 O3 þ 3H2 SO4 ð4Þ
light grey-colored regions (Area 4) are rarely present, and they are
irregularly distributed in the slag. It was confirmed by the EDX analysis in
There is also a possibility of basic iron sulfate formation as an
Fig. 2(f) and the XRD pattern in Fig. 1 to be spinel magnetite (Fe3O4 or
intermediate step in reaction (4); however, if it had formed, it would
FeFe2O4) crystals with a small portion of Cr being a substitution in a
not have been detected because it re-dissolves rapidly during cooling
possible form of FeCr2O4.
by reversing reaction (5).
Fig. 3 (a) shows a BSE image of another area. The distinctly bright
particle was confirmed by EDX to be another matte inclusion. The point
microanalysis results at positions 1, 2 and 3 are shown in Fig. 3(b), (c) Fe2 ðSO4 Þ3 þ H2 O ¼ 2FeOHSO4 þ H2 SO4 ð5Þ
and (d), respectively. An uneven distribution of base metals was found
in this particle. At position 1, the strong copper peaks and distinct iron Overall reactions:
and zinc peaks shown in Fig. 3 (b) indicate the existence of copper and
small amounts of iron and zinc, but no significant amount of sulfur was 1
Fe2 SiO4 þ =2 O2 ¼ Fe2 O3 þ SiO2 ð6Þ
detected. It is likely a small metallic copper droplet formed during
smelting at high oxygen potential (Davenport et al., 2001). The Zn and 1
Fe peaks are from the electron scattering in the surroundings of matte. 2Fe3 O4 þ =2 O2 ¼ 3Fe2 O3 ð7Þ
However, this particle contains a large amount of sulfur, a moderate
amount of iron and a small amount of copper at position 2 (Fig. 3(c)).
At position 3 (Fig. 3 (d)), besides sulfur, iron and copper, a small
portion of nickel was detected as well. It is evident that the base metals
are distributed unevenly in matte droplets.
The distribution of species within the slag can be further
monitored with the help of X-ray elemental mapping, as shown in
Fig. 4. An SEM image of the section where the elemental mapping was
performed is shown in Fig. 4 (a). This section was intentionally
selected because of the four distinct areas that could be easily used for
phase identification. Sulfur mapping (Fig. 4 (b)) indicates entrapped
matte droplets. The bright dots in Fig. 4(c), (d) and (e) represent the
distributions of copper, nickel and zinc, respectively. Very limited zinc
was detected due to its very small content and cobalt is finely
dispersed in the slag and cannot be detected.
Considering the microstructure characteristics of the base metals
in the slag, flotation will not be effective for the separation of base
metals and the cleanup of the hazardous slag. As a result, the base
metals need to be chemically liberated from the fayalite. While
sulfuric acid can dissolve fayalite and base metal oxides, oxygen is also
needed to leach out the non-oxide base metals and oxidize Fe(II) to Fig. 6. Extent of iron dissolution as a function of temperature. Solid loading 20%; acid
promote iron hydrolysis. High pressure oxidative acid leaching addition 33 wt.%; PO2 500 kPa; time 120 min (adapted from Li et al., 2008).
190 Y. Li et al. / Hydrometallurgy 97 (2009) 185–193

Fig. 7. Effect of acid addition on base metal extractions. Solid loading 25%; PO2 500 kPa; Fig. 9. XRD pattern of a typical residue.
temperature 250 °C; time 120 min (adapted from Li et al., 2008).

The properties of hematite, such as particle size and morphology, From Fig. 7, it was found that acid addition which levels up to 20 wt.%
directly affect the viscosity of the slurry, its filterability and to some of slag was sufficient to extract N97% Ni, Co, Cu, as well as 95% Zn in
extent the solubility of iron. Slurry viscosity affects the mass transfer 2 h. Excessive acid addition gave no benefit in terms of enhancing base
and consequently the extraction of base metals at temperature as well metal extractions and increased lime consumption needed for
as the subsequent solid–liquid separation under ambient conditions. neutralisation downstream. Fig. 8 shows the total iron concentration
Consistent with our previous work (Li et al., 2008; Baghalha et al., at 250 °C increased roughly 30-fold from 0.04 to 1.30 g/L due to the
2007), it was found that the acidity and temperature are the key exponential increase of hematite solubility with the acid addition
factors affecting the dissolution of valuable metals and iron in either increased from 15 to 30% (Liu et al., 2003; Reid and Papangelakis,
sulfide or oxide form in the presence of oxygen. 2006). However, percentage iron dissolution remained below 1.2% at
250 °C.
3.2.1. Effect of temperature It was also noticed that there was a noticeable difference in iron
The effect of temperature on base metal extractions and iron levels before and after autoclave cooling with an acid addition level of
dissolution is shown in Figs. 5 and 6, respectively. As expected, with an 30%. Iron concentration dramatically increases from 1.3 g/L before
increase in temperature from 175° to 250 °C, base metal extractions in cooling to 8.3 g/L after cooling down to 70–80 °C (Fig. 8(b)),
2 h increase from about 90% to about 99% whilst iron exhibits a reverse corresponding to 14.5% iron dissolution due to the re-dissolution of
trend due to the decrease in hematite solubility. From Fig. 6, the total precipitated hematite (or basic ferric sulphate) which impacts the
iron concentration reduces from 4.0 to 1.1 g/L corresponding to a subsequent iron removal step.
decrease in iron dissolution from 3.8 to 1.0%. Hence, a temperature of Therefore, an acid addition level of 20% or lower is recommended
250 °C or higher is preferable in terms of leaching selectivity. for maintaining a high recovery of base metals and low iron
dissolution. Flash discharging of the autoclave slurry is assumed to
3.2.2. Effect of acid addition be capable of minimizing hematite re-dissolution.
A series of similar tests with various acid additions was previously
performed (Li et al., 2008) with the results shown in Figs. 7 and 8. 3.3. Characterization of hematite residues

A series of analyses was conducted to measure the chemical


composition and to determine the mineralogy, morphology and
particle size of hematite residues obtained under different leaching
conditions. The efficiency of the solid–liquid separation process relies
on the density, size and shape of the individual particles in the slurry,
and is reflected by the filtration rate. Formation of large amounts of
fine hematite particles worsens the filterability of the leach slurry, and
promotes iron re-dissolution from hematite due to a high specific
surface area.

Table 2
Chemical composition of residues (wt.%) produced under: acid addition 20%; solid
loading 25%; 250 °C; 120 min.

Test Po2 Ni Co Cu Zn Al SiO2 S Mg Ca Fe Fe


No. (kPa) (T) (II)
1 186 0.011 0.002 0.019 0.008 1.45 36.9 0.32 0.01 0.49 37.3 0.95
2 276 0.009 0.001 0.026 0.011 1.45 36.9 0.35 0.02 0.50 37.4 0.94
3 434 0.009 0.001 0.013 0.008 1.42 36.9 0.32 0.01 0.48 36.9 0.89
Fig. 8. Iron concentration variation before and after slurry cooling. Solid loading 25%;
4 703 0.009 0.002 0.017 0.011 1.46 37.3 0.32 0.02 0.52 37.9 0.94
PO2 500 kPa; temperature 250 °C; time 120 min.
Y. Li et al. / Hydrometallurgy 97 (2009) 185–193 191

Fig. 10. SEM images and EDX spectrum of a residue obtained at 47 wt.% acid addition. Solid loading 15 wt.%; PO2 500 kPa; temperature 250 °C; time 120 min.

Fig. 11. SEM images and EDX spectrum of a residue obtained at 25 wt.% acid addition. Solid loading 25 wt.%; PO2 500 kPa; temperature 250 °C; time 120 min.
192 Y. Li et al. / Hydrometallurgy 97 (2009) 185–193

The chemical composition of the dried residues obtained at an acid


addition of 20 wt.%, with increasing oxygen overpressures is given in
Table 2. It can be seen that only about 0.01–0.03% base metals remain
in the residue. Iron, accounts for 37–38% mainly as hematite (about
53 wt.% Fe2O3) and silica also accounts for around 37%. The balance of
about 10% could be other metal silicates or water in silica gel.
A diffractogram of the representative residue obtained from Test 1
in Table 2 is shown in Fig. 9. All the narrow and sharp peaks occurring
in the XRD pattern are a perfect match for the crystalline hematite
structure. No other crystalline structures were detected by XRD. The
rough baseline indicates that silicon exists in the residue in the
amorphous form, and other metals, such as aluminum, calcium and
magnesium, could be present either as small amounts of crystalline or
amorphous silicates and sulfates.
It was observed that acid addition not only has a significant effect
on iron dissolution, but also affects the physical properties of the
hematite: i.e. morphology and particle size. Low acid concentration
favours the formation of regularly flower-shaped coarse and homo-
geneous hematite particles, which bring the benefits of lowering the
viscosity of the slurry and accelerating filtration. The filterability Fig. 13. Particle size distributions of residues obtained at different acid addition levels.
PO2 430–500 kPa; temperature 250 °C; time 120 min.
worsens under highly acidic conditions due to the formation of large
amounts of fine hematite particles as a result of fast fayalite
dissolution. microanalysis focusing on a large particle is shown in Fig. 10 (d). As
Figs. 10–12 show SEM images and EDX spectra of hematite residues expected, the strong silicon and oxygen peaks on the EDX spectrum
obtained at different acid addition levels ranging from 20 to 47 wt.%. confirmed the existence of amorphous silica in the particle together
The particle size distributions for these residues are shown in Fig. 13. with iron and trace amounts of aluminum, sodium and calcium.
From Fig. 10, it can be seen that the residue particles produced at Clearly, in a highly acidic solution, the fast decomposition of fayalite
a high acidity (47 wt.%) vary in size and have irregular shapes. A resulted in the generation of a large quantity of amorphous silica,
wide particle size distribution curve was measured for this sample which glued together with hematite particles to form the big particles.
(Fig. 14 (a)). Most of the particles vary in size from 0.1 up to 70 µm Some particles are built of irregularly scale-piled matrices, as shown in
(Fig. 10(a)). The large particles are layered-accumulations with many Fig. 10 (c). This kind of residue with particles of various shapes and
small hematite particles sticking on the amorphous silica matrices sizes exhibited poor filterability with a slurry filtration rate of only
(Fig. 10 (b)). The elemental composition determined by X-ray about 0.036 m3·m− 2·h− 1.

Fig. 12. SEM images and EDX spectrum of a residue obtained at 20 wt.% acid addition. Solid loading 25 wt.%; PO2 430 kPa; temperature 250 °C; time 120 min.
Y. Li et al. / Hydrometallurgy 97 (2009) 185–193 193

Compared with the residue particles in Fig. 10, the ones obtained (NSERC-I2I Program) and the kind support and supply of the slag
at a low acid addition level of 25% are more even in terms of sample from Vale Inco.
size distribution. Most of these particles are scale-like aggregates,
0.5–10 µm in size, as shown in Fig. 11 (a) and (b). But there are still References
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The authors would like to acknowledge the financial support from
the Natural Science and Engineering Research Council of Canada

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