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Coal–oil assisted flotation for the gold recovery

S. Sen, A. Seyrankaya
*
, Y. Cilingir
Dokuz Eylul University, Mining Engineering Department, Division of Mineral Processing, 35100 Bornova, Izmir, Turkey
Received 29 September 2004; accepted 23 March 2005
Available online 26 May 2005
Abstract
Using coal–oil agglomeration method for free or native gold recovery has been a research subject for many researchers over the
years. In this study, a new approach ‘‘coal–oil assisted gold flotation’’ was used to recover gold particles. The coal–oil–gold
agglomeration process considers the preferential wetting of coal and gold particles. The method takes advantage of the greater
hydrophobicity and oleophilicity of coal and gold compared to that the most gangue materials. Unlike the previous studies about
coal–oil–gold agglomeration, this method uses a very small amount of coal and agglomerating agents. Some experiments were con-
ducted on synthetic gold ore samples to reveal the reaction of the coal–oil assisted gold flotation process against the size and the
number of gold particles in the feed. It was observed that there is no significant difference in process gold recoveries for feeds assay-
ing different Au. Although there was a slight decrease for coarse gold particles, the process seems to be effective for the recovery of
gold grains as coarse as 300 lm. The decrease in the finest size (<53 lm) is considered to be the decrease in the collision efficiency
between the agglomerates and the finest gold particles. The effect of changing coal quantity for constant ore and oil amounts was
also investigated. The experiments showed that the process gives very similar results for both artificial and natural ore samples; the
best results have been obtained by using 30/1 coal–oil ratio.
Ó 2005 Elsevier Ltd. All rights reserved.
Keywords: Coal; Oil; Agglomeration; Flotation; Gold ores
1. Introduction
The optimal processing method for recovering gold is
determined by many factors. These factors can be sum-
marized as follows (Petruk, 2000; Allan and Woodcock,
2001 and Klimpel, 1999):
(a) Mineralogical mode of occurrence of gold.
(b) Identities of gold bearing minerals.
(c) Identities of associated metallic and non-metallic
minerals.
(d) Proportion of gold occurring in different host
minerals.
(e) Gold grain size distribution.
(f) Host and gangue mineral grain size distribution.
(g) Mineral alterations.
(h) Variations of the above within a deposit or with
time.
(i) Textures of the gold ores.
The subject of designing an effective gold recovery
process for a specific ore sample has always been a
challenge for researchers. Conventional gold recovery
methods include gravity, flotation, amalgamation and
leaching processes (Torres et al., 1999) but in the last
decades, numerous research studies have been done to
improve the conventional gold recovery methods and
to find alternative processing techniques. This paper is
concerned with flotation and coal–oil–gold agglomera-
tion of native and free gold.
0892-6875/$ - see front matter Ó 2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.mineng.2005.03.007
*
Corresponding author. Tel.: +90 232 388 3139; fax: +90 232 373
8289.
E-mail address: a.seyrankaya@deu.edu.tr (A. Seyrankaya).
This article is also available online at:
www.elsevier.com/locate/mineng
Minerals Engineering 18 (2005) 1086–1092
Previous studies on the flotation of native and free
gold have focused on many different factors affecting
the gold recovery (Allan and Woodcock, 2001; Teague
et al., 1999a,b; Valderrama and Rubio, 1998; Klimpel,
1999; Monte et al., 1997 and Forrest et al., 2001).
It can be stated that most of the main process variables
affecting gold recovery by flotation has been investigated
widely. Although flotation is a very affective process for
free and native gold recovery, sometimes it is not possi-
ble to obtain satisfactory results. It is inherently a slow
kinetic process and additional steps are generally in-
volved to increase product purity (Klimpel, 1999). Only
relatively fine gold particles are susceptible to flotation.
Gold particles approximately 20–200 lm in size range
can be recovered by flotation effectively. Selectivity for
gold decreases for fine gold particles (À20 lm) because
of the co-flotation of gangue components (Glembotski
et al., 1974). Flotation of gold particles coarser than
200 lm is very difficult due to their high specific density,
floating slower than finer particles and also requires
more collector to recover by flotation (Glembotski
et al., 1974; Klimpel, 1999).
Using the coal–oil agglomeration method for free or
native gold recovery has been a research subject for
many researchers since a patent was granted to BP Aus-
tralia Ltd in 1986. Though, it is possible to agglomerate
gold particles with oil due to its high natural oleophili-
city, gold ores do not contain enough gold particles to
form agglomerates. For this reason, a highly hydropho-
bic/oleophilic material is needed to produce agglomer-
ates with oil and gold (Calvez et al., 1998). The
coal–oil–gold agglomeration process considers the pref-
erential wetting of coal and gold particles. It takes
advantage of the greater hydrophobicity and oleophilic-
ity of coal and gold compared to that of most gangue
materials.
Coal–oil–gold agglomeration combines flotation with
a fine coal treatment process to yield a high grade con-
centrate and to minimize processing time while provid-
ing maximum efficiency. In coal–oil agglomeration the
suspension of finely ground coal particles in water is
strongly agitated with a small amount of oil. Intensive
agitation provides for the reduction of the immiscible li-
quid into fine spherical droplets (U
¨
nal and Aktas ß, 2001).
The oil droplets overspread the coal surfaces and the
collision of these oil wetted particles causes formation
of ‘‘liquid bridges’’ each upon them. As a result, the fine
particles in the beginning are converted to the masses
which were bounded together by liquid bridges (Keller
and Burry, 1987). Hydrocarbons or vegetable oils can
be used for oil agglomeration of coal. However, high
prices of hydrocarbons make their commercial use
uncertain. Vegetable oils, especially crude vegetable oils
are less expensive than hydrocarbons and unlike mineral
oils, they are renewable and nonpolluting resources
(Alonso et al., 1999).
Characterization of the oil utilized processes is shown
in Table 1. The quantity of the immiscible liquid used,
thermodynamic conditions of the process and the final
separation technique determine the name of the method
(Laskowski, 2001).
Different applications have been proposed by
researchers for the production of coal–oil–gold agglo-
merates (Gaidarjiev et al., 1996). Agglomerates may be
produced in a two-stage process. In the first stage, an
oleophilic material with (30–70%) is added under high
shear conditions to form the micro-agglomerates and
for the second step, the rest of the material is added
under low shear conditions to increase the size of the
agglomerates (Marciano et al., 1994). Moses and Peter-
senÕs study (2000) indicates that increasing the stirring
rate to a certain value results in obtaining higher gold
and mass recoveries for the flotation of agglomerates.
Wu et al. (2004a) investigated the adhesion behavior
of gold particles to coal–oil agglomerates and the study
revealed that in addition to gold particles, gold flocs and
even micro-nuggets can be detected on the agglomerates.
The authors say these flocs are probably formed by the
movement of initially penetrated gold particles over the
surface of the agglomerates.
Placers, tailings, and free milling ores can be evalu-
ated by coal–oil–gold agglomeration. It has been re-
ported that there is no significant difference in gold
recoveries with up to 5% sulfides in the feed (Calvez
et al., 1998). The coal–oil–gold agglomeration process
consists of two separate parts: production of coal–oil–
gold agglomerates and recovery of these agglomerates
from pulp. Flotation of the agglomerates or screening
can be employed for the recovery stage (House et al.,
1988).
The recovery of gold by CGA process depends
on many factors: Degree of inter-particle collisions;
Table 1
Oil utilized separation processes (Laskowski, 2001)
Method Presence of ionic collector Presence of oily collector Oil consumption Conditioning Separation method
Extender flotation Yes Yes 0.05–0.5 kg/t Regular Flotation
Agglomeration flotation Yes Yes A few kg/t Intense Flotation
Emulsion flotation No Yes Up to a few kg/t Regular Flotation
Oil agglomeration Yes Yes 5–10% Slow/intense shearing Sizing
Liquid–liquid extraction Yes Yes N/a Intense Phase separation
S. Sen et al. / Minerals Engineering 18 (2005) 1086–1092 1087
agglomerate strength and stability; mineralogy of gold
(Calvez et al., 1998); type, amount and size of carbona-
ceous material; type and amount of oil; type, degree and
time of agitation; contact time and number of recycling
of the agglomerates (Marciano et al., 1994; Moses and
Petersen, 2000; Wu et al., 2004a).
Unlike the previous studies (Table 2) about coal–oil–
gold agglomeration, very small amounts of coal and
agglomerating agents were used in this study. Flotation
was used as primary recovery process; it was used to
both separate the coal–oil–gold agglomerates from the
pulp and to recover gold particles which had not pene-
trated into the agglomerates. Only small amounts of
coal and agglomerating agents were added to the pulp
to assist gold flotation. Therefore, the method can be
called ‘‘coal–oil assisted gold flotation’’.
2. Experimental
2.1. Materials used
(a) Lignite coal (À150 lm) produced by rod mill from
Canakkale/Can (7.3% ash content) was used as the
agglomerating material.
(b) Pure quartz (À120 lm) and irregularly shaped
gold particles (91.6 Au and alloying metals)
were mixed to produce artificial gold-bearing ore
samples.
(c) Natural gold ore samples averaging 12 g/t Au
grades (100% passing 120 lm) from Efem C¸ uk-
uru/Izmir ore deposit. It is a vein-type epithermal
gold deposit with related stockwork and replace-
ment mineralization. Non-metallic host rock min-
erals include quartz, rhodonite and rhodochrosite.
Associated sulphides include pyrite, pyrrhotite,
chalcopyrite, sphalerite and galena, and their oxi-
dized products (Oyman et al., 2003). Most of the
gold is very fine (2.5–50 lm), occurring as free
grains in quartz and carbonate, and as inclusions
in sulphide minerals.
(d) Flotation reagents and agglomeration agents, as
listed in Tables 3 and 4.
2.2. Methods
2.2.1. Preparation of oil emulsions
Different vegetable oils (crude olive oil and crude cot-
ton oil) by 20% and diesel oil by 60%, amyl alcohol by
10%, Dowfroth 1012 by 10% were emulsified in a four-
baffled emulsifying cell to produce oil emulsions. Amyl
alcohol and Dowfroth 1012 were used to assist oil
emulsification and to provide frothing agents for further
flotation steps.
2.2.2. Direct agglomerate formation (coal–oil–gold)
Coal particles and oil were added to the gold bearing
pulp directly and coal–oil–gold agglomerates were pro-
duced in the flotation cell. A Denver sub-A flotation
machine with speed control was used for the agglomer-
ate production and separation. One thousand grams of
synthetic gold-bearing ore (25% solids by weight) was
used in the experiments. Coal particles (20 g), flotation
reagents and oil emulsion were added to the gold bear-
ing pulp at the same time and agitated at 2000 rpm stir-
ring speed for 20 min. Stirring speed was decreased to
850 rpm and the pulp was conditioned for 10 min for
agglomerate formation. The produced coal–oil–gold
agglomerates were separated from pulp by flotation.
The tests were conducted at a natural pH level.
2.2.3. Pre-agglomerate formation (coal–oil) and coal–
oil–gold agglomerate flotation
Coal particles were agglomerated using oil prior
to mixing with the gold-bearing ore pulp. An IKA-
Table 2
Previous CGA studies and approximate coal–oil consumptions
Study Carbonaceous material/ore
agglomerate/ore ratio
Oil/carbonaceous material oily collector/carbonaceous
material ratio
Wu et al. (2004a) 0.625 (w/w) (Graphite/synthetic ore) 0.4 (w/w) (Tetradecane/graphite)
Calvez et al. (1998) 0.15–1 (w/w) (Agglomerate/synthetic ore) 0.27–0.403 (w/w) (Oil/bituminous coal)
Moses and Petersen (2000) 1 (w/w) (Industrial charcoal/synthetic ore) 0.24 (v/w) (Ethyl oleate/industrial charcoal)
Marciano et al. (1994) 0.25–1.1 (w/w) (Agglomerate/synthetic ore) 0.2–0.35 (w/w) (Oil/metallurgical coal)
Table 3
Flotation reagents used in the study
Collector Consumption (g/ton)
KAX 50
Aerofloat 242 50
Aerofloat 208 50
Na
2
SiO
3
1000
Table 4
Agglomeration reagents used for a typical experiment
Collector Consumption (g/ton)
Vegetable oils 400
Diesel oil 1200
Amyl alcohol 200
Dowfroth 1012 200
1088 S. Sen et al. / Minerals Engineering 18 (2005) 1086–1092
Eurostar (Power control-visc) stirrer was used for emul-
sification and a Denver sub-A flotation machine with
speed control was used for the agglomerate separation.
Pre-agglomeration of coal particles and conditioning
of flotation pulp were started simultaneously. Thus, oil
emulsion was added to the emulsifying cell, agitated at
2000 rpm for 5 min. Coal particles (10% by weight) were
added to the oil-water emulsion and agitated at
2000 rpm for another 5 min. Flotation reagents were
added to the pulp that was agitated at 2000 rpm for
10 min. Pre-agglomerated coal particles–oil–water sus-
pension was added to the gold-bearing pulp and agitated
at 2000 rpm for 10 min. Stirring speed was decreased to
850 rpm and pulp was conditioned for 10 min for
agglomerate formation. The produced coal–oil–gold
agglomerates were separated from the pulp by flotation
at a natural pH level.
2.2.4. Conventional flotation
A Denver sub-A flotation machine with speed control
was used for the tests. A natural gold ore sample from
Efem C¸ ukuru/Izmir gold ore deposit (12 g/t Au) and a
synthetic gold ore sample containing À106 lm gold par-
ticles assaying 4.58 g/t Au have been subjected to the flo-
tation tests. Flotation reagents were added to the pulp
and pulp was conditioned at 2000 rpm for 30 min. A
25% solid/liquid ratio (by weight) was used and the tests
run at a natural pH level. The same flotation reagents
were used at the same dosages as with coal–oil–gold as-
sisted gold flotation experiments. And 5 min of flotation
time was applied for the experiments.
2.2.5. Analysis of the agglomerates
After being separated, agglomerates were burned in a
furnace at 900 °C for carbonaceous and volatile material
burning. The roasted material was a mixture of ash and
gold particles. The mixture was treated with aqua regia
to dissolve the gold. The gold assay was determined by
using a Perkin–Elmer Atomic Absorption Spectropho-
tometer (model 2280).
3. Results and discussion
3.1. Effect of gold assay on the process
The two different experimental paths followed are
given in Fig. 1. Artificial ore samples with different gold
assays and crude olive oil–diesel oil emulsion were used
as agglomerating reagents.
Production of coal–oil–gold agglomerates in ore
slurry was not successful without a pre-agglomeration
stage due to low oil concentrations in pulp and slime
coating on the coal particles. Hence, only a limited
number of agglomerates could be generated, about
25% of coal particles were converted to coal
agglomerates.
As previously stated by Calvez et al. (1998) and Wu
et al. (2004a,b), for CGA, the results suggest the same
relationship for the process between the number of
agglomerates generated and the number of recoverable
gold particles. The coal agglomerates surface area for
gold particles penetration and the number of coal
agglomerates for inter-particle collisions play the major
roles in the process. For this reason, increasing the num-
ber of gold particles in pulp for the same limited amount
of coal agglomerates caused recovery losses in the exper-
iment (see Fig. 1, path I).
The pre-agglomeration stage (see Fig. 1, path II) in-
creased the number of coal agglomerates in the slurry
and consequently, the agglomerates surface area for
gold penetration. Similar to the literature, increasing
the number of agglomerates in pulp and providing
enough surface area for gold particles penetration gave
rise to gold recoveries.
Wu et al. (2004b) proposed that gold recovery by
CGA is not affected by initial number of gold particles
in pulp. Likewise, Fig. 2 clearly shows that gold recov-
ery by coal–oil assisted gold flotation process is also
not affected, whereas the Au grade of the product
increases linearly with increasing feed grade.
A gold concentrate of about 4375.00 g/t Au was
obtained with a recovery of 76.36% from a gold ore
assaying at 18.33 g/t Au (see Fig. 2).
Fig. 1. Representation of coal–oil–gold agglomeration process.
S. Sen et al. / Minerals Engineering 18 (2005) 1086–1092 1089
3.2. Effect of gold particle size on the process
The effect of gold particle size on the process effi-
ciency has been studied using pre-agglomeration. Artifi-
cial ore samples containing gold particles in different size
fractions assaying at 6.417 g/t Au were used. Olive–
diesel oil emulsion was used as the agglomerating
reagent.
The process considers assisting flotation by coal–oil
agglomerates for the recovery of gold particles. There-
fore, the mechanism of the each process should be scru-
tiny before making any statements about the reasons
for interpretation of the results.
Firstly, particle size plays an important role in the
probability of particles for collision, and attachment
processes, as well as remaining attached in the pulp
phase in flotation. Fine particles typically have de-
creased particle–bubble collisions and this characteristic
can significantly influence and lowers the process recov-
eries. Coarse particles generally badly float mostly due
to the inevitability of the bubble–particle aggregates to
prevent the particle detachment from the bubble surface
caused by the particle weight and turbulence eddies dur-
ing flotation. In addition, coarse particles may need
longer induction times (Phana et al., 2003; Feng and
Aldrich, 1999; Nguyen, 2003; Nguyen et al., 1998; Dai
et al., 2000 and Bravo et al., 2005). In conclusion, the
flotation recovery of both fine and coarse particles is
usually remarkably low. Flotation method is the main
part of the proposed recovery system ‘‘coal–oil assisted
gold flotation’’ and so, low recovery values for both
coarse and fine gold particles would be expected unless
the assistance of coal–oil agglomerates does not improve
the recovery.
Wu et al. (2004b) proposed for CGA: once a tiny pre-
cursor ‘‘nucleus’’ forms, the fine gold particles would
easily attach on the coal agglomerates. It is therefore,
gold particles in the finest size (<53 lm) were success-
fully recovered and a superior concentrate containing
1096 g/t Au with a 75.2% recovery was obtained by
coal–oil assisted gold flotation. As it was predicted
relatively poor recovery values obtained for the coarsest
gold particles (À300 + 212 lm). These gold particles
detached from the air bubbles and/or they chipped-off
from the agglomerates during the agitation because of
their high density (Fig. 3).
As a result, coal–oil assisted gold flotation gave rela-
tively high recovery and superior grade values in com-
parison to the conventional flotation. The process is
still carrying some disadvantages of flotation but it can
be clearly seen that assistance of coal–oil agglomerates
improved the flotation performance for coarse and fine
gold particles.
3.3. Effect of coal quantity on the process
Experiments were conducted on both artificial ore
samples assaying at 4.58 g/t Au and natural ore samples
(12 g/t Au) from Efem C¸ ukuru/Izmir gold ore deposit.
Crude cotton oil–diesel oil emulsion was used as the
agglomerating reagent.
The amount of oil and degree of agitation control the
size of the agglomerates for CGA (Calvez et al., 1998).
In this experiment, different coal/oil ratios were used
without changing the agitation rate. Flotation parame-
ters were also kept constant to provide the system stabil-
ity and to achieve the effect of coal quantity on the
process.
The experiments showed that the process gives very
similar results for both artificial and natural ore sam-
ples. The best results were obtained by using a 30/1
coal–oil ratio (Figs. 4 and 5). Conventional flotation
produced a concentrate assaying at 101.20 g/t Au with
a 65.36% recovery for Efem C¸ ukuru gold ore samples.
A concentrate assaying at 108.20 g/t Au with a 47.19%
recovery was obtained by conventional flotation for
synthetic ore sample.
According to Wu et al. (2004b) producing smaller
agglomerates provides increased collision rates, so
(0-53) (53-75) (75-106) (106-150) (150-212) (212-300)
0
200
400
600
800
1000
1200
1400
0
20
40
60
80
100
Grade, Au (g/t)
Recovery, Au (%)
Gold Particle Size Range, (micron)
R
e
c
o
v
e
r
y
,

(
%
)
G
r
a
d
e
,

(
g
/
t
)
Fig. 3. Gold concentrate grade and recoveries vs. gold particle size
fractions in the feed.
Head Grade, (g/t)
0 5 10 15 20
G
r
a
d
e
,

(
g
/
t
)
0
500
1000
1500
2000
2500
3000
3500
4000
4500
R
e
c
o
v
e
r
y
,

(
%
)
0
20
40
60
80
100
Conc. Grade (Pre-agglomerated), Au (g/t)
Conc. Grade, Au (g/t)
Conc. Recovery (Pre-agglomerated), Au (%)
Conc. Recovery, Au (g/t)
Fig. 2. Gold concentrate grade and recoveries vs. feed grade.
1090 S. Sen et al. / Minerals Engineering 18 (2005) 1086–1092
higher K (rate constant) values and faster adhesion,
whereas larger agglomerates bestows slightly larger
attachment probability. Calvez et al. (1998) obtained
higher gold recovery values by using lower oil/coal
(higher coal/oil) ratios. Increasing the available surface
area of the agglomerates for gold penetration increases
the gold recovery. Similarly, coal–oil assisted gold flota-
tion produced concentrates with higher recovery values
for higher coal/oil ratios. Larger agglomerate surface
area also provides the fine gangue particles to sneak into
the agglomerates. Therefore, increasing the coal/oil ratio
decreases the grade of the concentrates for both
synthetic (Fig. 4) and natural gold ore samples (Fig. 5).
4. Conclusions
Unlike the previous studies about coal–oil–gold
agglomeration, this method uses very small amounts
of coal and agglomerating agents. Therefore, the
method can be called ‘‘coal–oil assisted gold flotation’’
and it seems to be effective for gold ore processing.
The experiments showed that use of oil and coal parti-
cles to assist gold flotation successfully increases the flo-
tation performance. In fact, there is a reciprocal
interaction between the flotation and coal–oil agglomer-
ation in this process. Researchers have found that
presence of flotation collectors such as xanthate in the
pulp help coal–oil–gold agglomeration (Sen, 2000;
Wu et al., 2004a,b) and increased agglomeration
performance assists the flotation and so the overall
recovery.
The pre-agglomeration stage provides to use higher
number of coal–oil agglomerates in the slurry, agglom-
erates surface area is larger for gold penetration and
similar to the literature about CGA, it gives the oppor-
tunity to achieve higher gold recoveries.
Experiments showed that the recovery values of coal–
oil assisted gold flotation are not affected by the initial
number of gold particles.
The process is still carrying some disadvantages of
flotation but it can be clearly seen that assistance
of coal–oil agglomerates improves the flotation
performance for coarse and fine gold particles. Rela-
tively high recovery and superior grade values in com-
parison to the conventional flotation can be obtained
by coal–oil assisted gold flotation for these problematic
particles.
The process gave very similar results for both artifi-
cial and natural ore samples. Higher gold recovery val-
ues have been obtained by using lower oil/coal (higher
coal/oil) ratios, but larger agglomerate surface area also
increases the fine gangue entrainment into the agglomer-
ates. Therefore, increasing the coal/oil ratio gave rise to
the recovery, whereas the grade of the concentrates de-
creased for both synthetic and natural gold ore samples.
High recovery values can be obtained by coal–oil as-
sisted gold flotation without any recycling stages of
coal–oil–gold agglomerates.
The process needs small amount of oil and coal par-
ticles addition into the flotation slurry to enhance the
gold recovery and it makes the method economically
applicable. The results of this investigation seem to be
very encouraging for the development of coal–oil as-
sisted flotation technology as an alternative process for
the recovery of gold.
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