Minerals Engineering 99 (2016) 89–95

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Minerals Engineering
journal homepage: www.elsevier.com/locate/mineng

Ultrasound treatment on tailings to enhance copper flotation recovery

A.R. Videla a,⇑, R. Morales a, T. Saint-Jean a, L. Gaete b, Y. Vargas b, J.D. Miller c
a
Mining Engineering Department, Faculty of Engineering, Pontificia Universidad Catolica de Chile, Chile
b
Physics Department, Faculty of Science, University of Santiago, Chile
c
Metallurgical Engineering Department, College of Mines and Earth Sciences, University of Utah, USA

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

Article history: As ore grades fall, the amount of tailings production for the same copper production is expected to rise.
Received 24 March 2016 Flotation recovery of copper sulfide from the El Teniente plant has deteriorated in recent years, in this
Revised 5 September 2016 regard ultrasound treatment of tailings for enhanced copper recovery was evaluated in laboratory exper-
Accepted 24 September 2016
iments. The impact of the ultrasound wave was examined under different conditions, with the conclusion
Available online 5 October 2016
that improved recovery occurs when ultrasound is applied during conditioning and flotation. The results
can be explained by the effect of acoustic cavitation that cleans particle surfaces and minimizes slime
Keywords:
coatings, facilitating the action of the reagents. In this way, improvement in copper recovery of up to
Ultrasonic treatment
Ultrasound
3.5% were obtained.
Flotation Ó 2016 Elsevier Ltd. All rights reserved.
Copper tailings
Copper recovery

1. Introduction the poorest tailings in order to recover bornite, chalcopyrite,

One of the biggest challenges facing the mining industry is the
deterioration of mineral grades. This problem makes it necessary
to improve the recovery of current operations to offset the steady
decline of Cu grades. Such a decline of average saturation grade has
meant a fall of 1.0% Cu to 0.86% of global average grade during the
last decade (Chile, Ministerio de Minería, Corporación Chilena del
Cobre, 2015). It is estimated that in Chile the amount of tailings
generated only as products of copper sulfide concentration reaches
481 M ton annually, a figure that will continue to rise as mineral
grades fall. That is why it is interesting to explore the use of new
technologies to improve overall recovery and reduce tailings.
Ultrasound treatment is used in various industries for surface
cleaning (Farmer et al., 2000; Gallego-Juarez, 1994; Zhao et al.,
2007). Ultrasound treatment has lead to interesting research in
the mineral processing industry to improve coal processing
(Ozkan and Kuyumcu, 2006, 2007; Ozkan, 2012; Ambedkar et al.,
2011), fluid-solid particle separation (Riera-Franco de Sarabia
et al., 2000) and flotation of oil shale cleaning (Altun et al.,
2009). Moreover, various studies to optimize the flotation process
by using ultrasound treatment have been conducted (Aldrich and
Feng, 1999; Ishak and Rowson, 2009; Kang et al., 2009; Ozkan
and Gungoren, 2012; Schlesinger and Muter, 1989; Vargas et al.,
2006), but none of the studies contemplated the re-treatment of
⇑ Corresponding author.
E-mail address: avidela@ing.puc.cl (A.R. Videla).
cuprite or molybdenite.
Following this line of research, Ozkan (2002) has shown that
pre-treatment of magnesite by ultrasound increases magnetite
recovery. In his analysis, he assumed a cleaning effect on the sur-
face of the mineral. Similarly, Kang et al. (2009) have shown that
the application of ultrasound radiation in coal flotation improves
the efficiency of the process, reducing ash recovery. Also, sulfides
were oxidized due to the ultrasound effect.
Aldrich and Feng (1999) observed an improvement in the
ultimate recovery of sulfur from Merensky Reef, Africa, using ultra-
sound treatment, despite the negative effects of the concentration
of solids, temperature, conditioning time and gas flow. Meanwhile,
Vargas et al. (2006) found that conditioning by means of ultrasonic
radiation could preserve the concentration of copper sulfides, but
decrease the recovery of iron sulfides, resulting in improved
selectivity in the flotation, reducing the recovery of pyrite and
increasing the concentrate grade.
Previous work (Stoev et al., 1992) have shown the significant
positive impact that may have the application of mechanical vibra-
tion and the acoustic wave excited by them in several mineral pro-
cessing units, particularly in flotation. Their results were promising
and show applications of vibroacoustic excitation at low frequen-
cies to promote attachment of mineral particles to air bubbles,
increment of recovery, increment of flotation rate, increment of
selectivity, control bubbles size, emulsification of reagents, desorp-
tion of reagents, and froth control among others. The principle that
justifies the use of ultrasound relates to the same phenomena

http://dx.doi.org/10.1016/j.mineng.2016.09.019
0892-6875/Ó 2016 Elsevier Ltd. All rights reserved.
90 A.R. Videla et al. / Minerals Engineering 99 (2016) 89–95
described in this seminal work, a process based on the wave
spreading in the aqueous medium. Additionally, as the wave fre-
quency increases reaching high intensities such in ultrasound,
the vibroacoustic waves can lead to acoustic cavitation, a phe-
nomenon that causes bubble generation due to progressive pres-
sure drop in each wave cycle. The bubbles begin to oscillate
along the sound field in the first stage; after a few cycles the bub-
bles reach a critical size at which they resonate in a nonlinear
regime. This regime makes it difficult for the bubbles to expand
to larger sizes, making the medium’s response increasingly impor-
tant, due to the inertial forces that cause shrinkage of the bubble in
the compression cycle (Gaete et al., 1997). Eventually the bubbles
collapse under considerable elevated pressure emanating from the
medium (Mitome, 2003). This implosion generates a supersonic
microjet of fluid in the area where the bubble collapses. It has been
shown that this microjet possesses great capacity to erode a sur-
face which would remove contaminants on the surfaces of the par-
ticles, thus improving the efficiency of the concentration process.
This study suggests that the cavitation phenomenon caused by
ultrasound could improve the flotation tailings of copper sulfides.
The tailings consist of fine and ultra-fine particles of gangue, and
a percentage of particles containing copper that were not floated
due to lack of release and surface contamination. Copper sulfides
inside the tailings might have been oxidized and ultrasound treat-
ment may have removed the oxidized layer from the particles sur-
faces as well as helping the desliming. This would mean an
improvement in the overall recovery of the system before sending
the tailings to their final deposition.
Subsequently, the methodology of the development and evalu-
ation of laboratory flotation tests for processing the tailings of cop-
per sulfide is presented. For this evaluation a ‘Denver’ flotation cell
has been changed to be able to control the ultrasound field applied
to the particles. The results are analyzed via obtaining the kinetic
curve flotation, its parameters and the resulting Cu grade.
2. Materials and methods
2.1. Materials
To develop this study, copper sulfide tailings, provided by Valle
Central Mine, were used. The tailings have an average copper grade
Table 1
Characterization of collected samples.
Characteristic Sample 1 Sample 2
Uniformity 7,48 3,32
Specific surface [m2/g] 0,86 1,15
Average particle size D[3,2] [lm] 7,00 5,20
Average particle size D[4,3] [lm] 158,02 40,76
10% Under diameter [lm] 2,76 2,12
50% Under diameter [lm] 20,12 10,82
90% Under diameter [lm] 402,70 118,53
Volume [%]
Volume [%]
Parcle Size (Diameter) [μm] Parcle Size (Diameter) [μm]
Fig. 1. Particle size distribution in three samples collected from Minera Valle Central feed. Sample 1, 2 and 3 are shown from left to right.
of 0.12%, with most in the form of chalcopyrite, and with a specific
gravity of 2.7 [g/cm3]. The tailings consist of fine and ultra-fine par-
ticles under 70 mesh, which have previously passed through a
stage of grinding and flotation in the mine of ‘El Teniente’, a branch
of the national copper company CODELCO Chile, a mill plant
located in central Chile.
Three tailings samples of 500 ml out of the 100 L sample were
analysed to characterize the particle size of the supplied
material. After tailings were homogenized, increments of 50 ml
were taken from different parts of the container to complete
one sample. The samples were extracted and analysed via laser
diffraction technology with a Mastersizer 2000. Table 1 and
Fig. 1 display the results of the analyses and distributions of
the size for each sample, respectively. As can be seen, the results
show that the tailings is mostly composed of particles of about
10 lm, with 50% of the particles under 14 lm and 90% of the
particles under 220 lm. Sample one is coarser than sample two
and three. This difference may due to the fact that the upstream
classification process is not operating perfectly and few coarse
particles may have end in the final sample. In average though,
the product size is below the limit. No agglomeration was
observed in the sample. Samples were sonicated 20 min before
the particle size analysis.
2.2. Ultrasound treatment
In this study we evaluated the use of ultrasound to improve the
recovery of copper sulfides by applying three different conditions,
derived from experience gained from evaluating heavy minerals in
previous research (Celik, 1989; Cilek and Ozgen, 2009; Djendova
and Mehandjiski, 1992; Aldrich and Feng, 1999; Ozkan, 2002;
Vargas et al., 2006). The three ultrasound conditions applied are:
Ultrasound Conditioning (UC) where ultrasound is applied only
during conditioning; Ultrasound Flotation (UF) which applies
ultrasound only in flotation; Flotation and Conditioning with Ultra-
sound (FCU), in which ultrasound is applied throughout the pro-
cess of conditioning and during flotation. These tests were
compared with the results of a basic test called Standard Flotation
(SF) that considers the same operating conditions but without
applying ultrasound during any of the processess. All tests were
run in random order and in duplicate to control the variability of
Sample 3 Average Standard deviation
5,07 5,29 2,09
1,11 1,04 0,16
5,43 5,88 0,98
59,73 86,17 62,94
2,27 2,39 0,34
10,79 13,91 5,38
130,01 217,08 160,86
Volume [%]
Parcle Size (Diameter) [μm]
 A.R. Videla et al. / Minerals Engineering 99 (2016) 89–95
Table 2
Experimental design for flotation with ultrasound.
Identification Conditioning with ultrasound Flotation with ultrasound
[yes/no] [yes/no]
SF No No
UC Yes No
UF No Yes
FCU Yes Yes
results. Table 2 summarizes the conditions of application of ultra-
sound in the four types of tests.
The flotation tests were conducted in a ‘Denver’ cell with a
stainless steel reactor of 8 L effective capacity, fitted with 9 ultra-
sonic transducers (Clangsonic 2045-68LB P8), as shown in Fig. 2.
The transducers were connected to a Clangsonic SONOCLG XR
2000G generator of 2000 W. Each transducer emits 100 W of
power at a frequency of 20 kHz, obtaining an equivalent power
of 112.5 W/L. The ultrasonic frequency was kept fixed in one of
Eigen mode of the transducers during testing.
A calibrated probe, designed especially to measure cavitating
acoustic fields (Gaete et al., 1993), has been used to determine
the effective intensity of the acoustic field present in the flotation
cell. The probe’s design was based on stainless steel and brass,
which transforms external mechanical disturbances into electrical
signals that are sent to Arduino hardware, where the signals are
processed with a code written in Python. The probe measures
35 cm in length and 1.3 mm in diameter. With these dimensions
it is possible to make three-dimensional scans inside the Denver
cell without excessively modifying the internal acoustic field. The
experimental system was mounted within a steel structure that
allows three-dimensional scans controlled by a computer with an
accuracy of 0.1 mm in all three axes. Using that setup it was possi-
ble to measure the acoustic pressure at three different planes
inside the cell as shown in Fig. 3. The experimental set-up allow
to measured the acoustic pressure on the scanned planes gener-
(a) Denver Flotaon Machine
(b)
Cell
Transducers
Fig. 2. Schematic design of the Denver equipment and the flotation cell: (a) Outline
of the Denver flotation equipment and the cell, side view; (b) Outline of the
flotation cell, top view.
Fig. 3. Lateral views of plane under study inside the DENVER cell.
91
ated by the acoustic field: the displacement of the probe was dri-
ven for a 3D system computer-controlled with a device similar to
the CNC machines.
The acoustic pressures within the cell at the three levels indi-
cated are presented in Fig. 4. It can be observed how the acoustic
field concentrates in certain areas of the cell, raising the pressure
up to almost 75 kPa. The lowest pressure level measured was
around 15 kPa, therefore the ratio between maximum and mini-
mum acoustic pressure inside the Denver Cell is 5. In Fig. 4 the root
mean square (RMS) intensity of the acoustic field is shown on a
color scale, where dark red represents the greatest intensity of
the acoustic field and blue the lower intensity. In the areas of high
energy concentration a greater effect of acoustic cavitation should
occur. Fig. 4 reveals that exposure of the tailings slurry to the ultra-
sonic field is not uniform throughout the cell.
The transducers have a fundamental excitation frequency of
20.804 kHz amplitude for a sinusoidal signal of 36.36 kHz fre-
quency, which is maintained with small variations of approx.
1 kHz. This type of excitation results in widening the band of the
power signal, allowing compensation for small differences in the
resonance frequency of each transducer. Fig. 5 shows the excitation
wavelength used for the modulation of the transducers.
2.3. Flotation experiments
The operating conditions for the flotation experiment were kept
constant for all tests and are summarized in Table 3. Reagent Ore-
Prep X-133 was used as frother and Aero 343 as collector, both
supplied by CYTEC.
A similar procedure was follows for each flotation test. At the
start of each test, the percentage of solids of the material was mea-
sured through a Marcy pulp density scale, adjusting the concentra-
tion with water until the required value in the cell was reached.
Originally, time counting initiates the conditioning stage under
stirring only (without aeration) by adding the respective doses of
each reagent. Regarding reagent addition, pH is adjusted by adding
CaO until pH 10 is reached, then 30 g per ton of collector and
frother is added. Initiation of aeration ended the conditioning stage
and started the flotation stage. During the flotation process CaO
was added to maintain pH 10 throughout the test. The concentrate
froth was collected manually via over-flow and paddling a spatula
at regular time intervals of approximately 15 s, collecting samples
at 0.5, 1, 2, 4, 7 and 12 min.
To calculate the copper content, the products were dried and
analyzed by atomic absorption spectrophotometry on a Perkin
Elmer Analyst 100 instrument. The test was considered valid if
the difference between the measurements of each Cu content
between replicates was less than 2.5%. Regarding the calculation
of the recovery, the results were adjusted to an equation of first
order recovery (Wills and Napier-Munn, 2005) by adjusting the
data according to the model proposed by García-Zúñiga:
Rt ðtÞ ¼ R1 ð1  eðktÞ Þ ð1Þ
where Rt is recovery (%) of a valuable metal in an instant t (min);
with R1 representing the maximum estimated recovery and k the
kinetic constant of the flotation process, respectively.
3. Results
As Fig. 6 shows, the García-Zúñiga model (Eq. (1)) fits wells to
the data under analysis. Fig. 6(a) shows that the recovery in the
standard flotation (SF) test with no ultrasound applied. Fig. 6(b)
shows the results for ultrasound during conditioning only (UC).
Fig. 6(c) shows results for ultrasound during flotation only (UF)
and finally Fig. 6(d) shows when ultrasound is applied during
92 A.R. Videla et al. / Minerals Engineering 99 (2016) 89–95

Fig. 4. Distribution of the absolute critical pressure inside the Denver flotation cell. The first picture (upper) corresponds to plane 1 inFig. 3, the second one to plane 2 and the
last one to plane 3.

Fig. 5. Excitation signal for the transducer system. The top signal is for a period of the wave that modulates in amplitude below. It can be seen how this variation is repeated
over time.
 A.R. Videla et al. / Minerals Engineering 99 (2016) 89–95 93

Table 3 Table 4
Conditions of the flotation process. Average parameters adjusted to the flotation results using the García - Zúñiga model.
Maximum recovery (R1), kinetic constant (k) and Coefficient of Variation (COV) are
Parameters Ranges shown.
Conditioning time 6 min
Identification R1 [%] C.O.V [%] k [min1] C.O.V [%]
Frother (OrePrep X–133) 30 g/ton
Average R1 Average k
Collector (Aero 343) 30 g/ton
Air impeller speed 1200 rpm SF 27,89 4,07 0,55 4,11
Solids percentage 30% UC 28,94 0,93 0,43 2,33
Pulp pH (CaO added) 10 UF 29,23 2,63 0,37 4,66
FCU 31,40 2,95 0,43 6,98

conditioning and flotation time as well (FCU). From Figures can be

observed that after twelve minutes of flotation each condition SF,
UC, UF, and FCU reaches 27.89%, 28.94%, 29.23% and 31.40%
recovery respectively. Therefore, the application of ultrasound
equals or exceeds the results obtained by standard flotation
without ultrasound.
The first order flotation model also helps to evaluate the kinetic
response of the flotation process. In this regard, once the recovery
limit (R1) was determined, we proceeded to calculate the kinetic
flotation constant (k) according to Eq. (1). In Table 3 adjusted val-
ues and the variation coefficients are shown, obtained by the least
squares method. All adjustments conform to a very low variation
level as shown in Table 4. The FCU test shows recovery being 4 per-
centage points higher than standard flotation without ultrasound.
This improvement was significantly above measurement error. In
the best case, the FCU treatment presents a statistically significant
difference with the Cu recovery obtained by SF with a 95% confi-
dence. In the other two cases the statistically confidence is reduced
but still is over 80%. From the results we can assure there is an
experimental difference in the Cu recovery.
Fig. 7 shows a superposition of the mean values of the resulting
flotation tests. It is graphically observed that the FCU test with
ultrasound during conditioning and flotation improved the recov-
ery presenting a faster kinetic response than standard flotation.
Regarding the concentrate grade (% Cu), it was found that when
ultrasound was applied the concentrate grade improved in relation
to standard flotation. As shown in Fig. 8, the best result was
obtained by applying ultrasound during the flotation stage only,
improving from 0.6% Cu to a final grade of 0.77% Cu.
One explanation for these improvements is that fine and ultra-
fine particles are superficially cleaned by the microjets from the
collapse of cavitation bubbles. Cleaning the surface facilitates the
action of the collector on the cleaned surface, increasing the per-
centage of available surface for adhesion of the collector, and so
fomenting the action of the reagents. Another hypothesis is that
the detected beneficial effect is due to an agglomeration action of
ultrasound on the ultrafine particles (6–50 lm) in the areas of
highest sound pressure (Fig. 4), which would allow them to acquire
enough kinetic energy to emerge together with the bubbles

35% 35%
(a) (b)
30% 30%

25% 25%
Recovery (%)

Recovery (%)

20% 20%

15% 15%

10% 10% Test 1

Test 1
Test 2
5% Test 2 5%
Mean Mean
0% 0%
0 5 10 15 0 5 10 15
Time (min) Time (min)

35% 35%
(c) (d)
30% 30%

25% 25%
Recovery (%)

Recovery (%)

20% 20%

15% 15%

10% Test 1
10% Test 1

Test 2 Test 2
5% 5%
Mean Mean
0% 0%
0 5 10 15 0 5 10 15
Time (min) Time (min)

Fig. 6. García Zúñiga setting for the quadruples of (a) SF, (b), UC (c), UF and (d) FCU.
94 A.R. Videla et al. / Minerals Engineering 99 (2016) 89–95

35% (Vargas et al., 2006). Additionally, the effect of the ultrasound

could stem from the generation of sufficiently small bubbles lead-
30%
ing to a better particle bubble and particle size relation than the
25% standard flotation without ultrasound, improving the flotation of
Recovery (%)

fine particles.
20% An analysis of some particle tailings has been conducted to
determine if any surface cleaning ocurred. This analysis was under-
15%
taken via electronic scanning by SEM (Scanning Electron Micro-
10% SF scopy), obtaining images presented in Fig. 9. In most cases a
UC decrease of ultrafine particles is observed on the surface of the par-
5% UF
ticles subjected to ultrasound, which would corroborate the
FCU
0%
hypothesis of the cleaning effect of ultrasound and would improve
0 2 4 6 8 10 12 14 the efficiency of the reagents.
Time (min)

Fig. 7. Average recovery kinetics according to type of ultrasound treatment. 4. Conclusions

Based on the experimental results, ultrasound could be a com-

0.90%
plementary technology to process tailings in classical flotation
0.85%
processes given its potential to improve the recovery of the fine
Cumulave Grade (%)

0.80%
and ultrafine particles. For a standard copper concentrator overall
0.75%
recovery is around 90%, therefore 10% of the feed Cu is lost in the
0.70%
tailings and could be potentially recovered. As shown from the
0.65% current results, if a 30% recovery is achieved from this 10% copper
0.60% lost in the tailings, it could mean an increase of about 3.1 per-
0.55% centage points in the overall recovery, achieving a total of 93.1%
SF
0.50% UC Cu recovery. Therefore the use of ultrasound during conditioning
UF
0.45% FCU and flotation of fines and ultrafines deserves further consideration
0.40% although the economical incentive to apply this technology will
0 2 4 6 8 10 12 14
depend on the balance between the marginal benefit obtained
Time (min)
with the extra Copper production and the investment cost need
Fig. 8. Concentrate grade as a function of flotation time for different ultrasound to apply an equivalent ultrasound treatment to high volumes.
treatments. Given the current cost of the high frequency ultrasound

Fig. 9. Images of concentrate chalcopyrite particles resulting in the concentrate after flotation from SF and FCU experiments (magnification 6.000). Above: SF concentrated
particles. Below: FCU concentrated particles.
 A.R. Videla et al. / Minerals Engineering 99 (2016) 89–95
equipment there is still significant work to be done to make the
technology attractive.
It is believed that improvements are mainly explained by the
phenomenon of surface cleaning via fluid cavitation produced by
ultrasonic waves and bubble jets, resulting in cleaning the particle
surface and improving the functioning of the collector. However,
more research is required to understand and properly control the
applied pressure field and the effects on the flotation of ultrafine
particles. It would be particularly convenient to make further pro-
gress in understanding the potential action of agglomeration and
deagglomeration.
of the ultrafine particles via ultrasound. Other possible effects
to be considered is the ultrasound effect on the liquid. It was
observed that the energy density heats up the slurry in some
degrees, which potentially leads to changes in the chemical equi-
librium in solution, which may have an effect in pH, redox poten-
tial, z–potential and contact angle.
According to the results shown, ultrasound applied at any stage
of the process improves final recovery and kinetics of the flotation
process of fine and ultrafine copper sulfide particles under evalua-
tion. This improvement is above measurement errors of the tests
and represents significant increase in recovery compared to the
recovery obtained by standard flotation. Importantly, the latter
feature may allow reduction in the volume of reactors needed to
reach a given throughput level for the same Cu recovery, allowing
reduction of facilities lay-out and/or increasing production capac-
ity with the same equipment.
Fig. 4 demonstrates that exposure of the tailings slurry to the
ultrasonic field is not uniform inside the cell. Design should be
optimized and controlled with an optimal distribution of the trans-
ducers in the reactor’s geometry. Another alternative to improve
acoustic field uniformity would be the redesign of the cell so that
the ultrasound effects are maximized, searching resonance condi-
tions. In any case, transducer interference should be avoided as it
is destructive and lowers the efficiency of the process. This aspect
of the research and development program will be addressed in a
subsequent investigation.
The presented research work has been limited to evaluation of
ultrasound impact on the particle solid surface. However ultra-
sound irradiation impacts on solid-liquid interfaces and liquid-air
interfaces changing for instance the contact angle. Some of our pre-
liminary studies have shown that a significant change in contact
angle can be achieved by the solid surface vibration lead by an
ultrasound field. These impacts require further attention and
should be addressed in future research.
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