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Constrained Multivariable Control of a Pilot Flotation Column at

AEM Laronde Concentrator
R. del Villar
Département de génie des mines, des matériaux et de la métallurgie
Université Laval. Québec City, QC, Canada G1V0A6
D.E.Calisaya, A.Riquelme, A.Desbiens, É.Poulin

Département de génie électrique et de génie informatique
Université Laval. Québec City, QC, Canada G1V0A6
ABSTRACT A 15 cm diameter by 732 cm height, fully automated pilot column was

installed in the Agnico-Eagle’s Laronde concentrator (Québec), for evaluating the
performance of newly developed sensors and advanced process control algorithms. For
eventual comparison purposes, the pilot column is continuously fed with the same slurry
feeding the copper-circuit third cleaner column. It is equipped with electrical conductivity-
based sensors for estimating the three variables used in the multi-variable control algorithm
under evaluation: froth depth, fraction of wash water underneath the interface and gas hold-
up. Froth depth is regulated using a PI controller while a predictive controller is formulated
as the minimization of the tracking errors of gas hold-up and bias rate, keeping several
operating constraints between their practical upper and lower limits. In particular, an
unreachable high set point of gas hold-up can be selected in order to maximize the bubble
surface area available for particle collection, while maintaining bias rate above a minimum
value required for froth cleaning. The proposed strategy may indirectly help optimizing
flotation column operation by using these secondary variables, without the implementation of
a real-time optimization layer.
1 INTRODUCTION concentrate cleaning, is simply not measured

at all, as there is no commercial sensor
Flotation columns have already been used available. Therefore, besides froth depth,
for more than 30 years, mainly in cleaning continuous monitoring of process variables
stages, as a result of their froth washing is limited to flow rates (gas, feed, tailings,
capabilities. Despite their widespread usage, wash water), i.e., to manipulated variables.
the measurement of some pertaining Some new available sensors have been
variables and their use for automatic control industrially tested, e.g., the Sonar-TracTM
is rather scarce. Among the most important for gas hold-up (O'Keefe et al., 2007) and
variables directly related to the process the McGill hold-up sensor (Tavera et al.,
metallurgy (concentrate grade and recovery), 2002). Others sensors, for bias rate and
froth depth (hf) is the only one normally frother concentration, have been successfully
monitored and controlled. Even though validated at laboratory scale by Laval’s
commercial sensors are available, the gas LOOP researchers (Maldonado et al., 2008b;
hold-up ( g), a variable directly related to Maldonado et al., 2010a). The McGill
concentrate recovery, is seldom measured bubble viewer (Gomez et al., 2007) and
and never controlled. Another important others similar devices have been extensively
variable, bias rate (Jb), responsible for used for off-line monitoring of bubble size
871
5GHO9LOODU'(&DOLVD\D$5LTXHOPH$'HVELHQV(3RXOLQ
and bubble space distribution, but not yet for hold-up in the collection zone and the
control purposes. fraction of wash water underneath the
On the other hand, advanced control and interface (related to bias rate) in an industrial
supervision techniques are available and environment, while froth depth is being
efficiently working in many industrial fields controlled independently through a classical
(Quin et al., 2003; Jelali, 2006). The bubble PID control loop.
size distribution, measured with the McGill
bubble viewer, has recently been measured 2 INSTRUMENTATION & CONTROL
and modeled (Maldonado et al., 2008c;
Matiolo et al., 2011), opening a door for the
control of bubble size (d32) in a laboratory 2.1 Variables and Sensors
two-phase system (Maldonado et al., 2010b).
For more than two decades, researchers from
At the laboratory level, our research group
McGill University and Université Laval
has demonstrated the usefulness of some
have been working on the development of
conductivity-based sensors (for froth depth,
devices or techniques for the measurement
gas hold-up and bias rate), as well as the
of flotation column operating variables such
good performance of several advanced
as froth depth hf , bias rate Jb, gas hold-up Hg,
control techniques (del Villar et al., 2010).
bubble diameter db , BSD, bubble size distri-
Usually developed in two-phase systems
bution, and bubble surface area flux, Sb .
(water-air), most of these tools have also
These variables are hereafter named as
been validated in a three-phase system (pulp-
“secondary controlled variables”, to make a
air). A thorough NSERC-CRD industry-
distinction from the ultimate metallurgical
university research project (Agnico-
controlled (primary) variables: concentrate
Eagle Mines Laronde concentrator, Xstrata
grade and recovery. A third level of
Nickel - Strathcona concentrator, COREM
variables are the so-called tertiary variables,
and Université Laval), concerning the
typically flow rates, being manipulated to
application of all above mentioned aspects to
maintain the secondary variables at their
the optimization of flotation column
optimal set points. These latter values would
operation, has recently been completed.
ultimately lead, through empirical models, to
Besides the industrial evaluation of
the desired values of primary variables,
conductivity-based sensors for froth depth,
ideally determined by an economical
gas hold-up and bias rate, it aimed at:
criterion (i.e. Net Smelter Return).
(a) producing an on-line version of the
McGill bubble viewer for process control
purposes, (b) improving the modeling of the 2.1.1 Froth depth
obtained bubble size distribution, This variable is successfully measured in
(c) studying the relationship between the industrial columns using a float combined to
floatable particle size distribution and the an ultrasound emitter and receiver. In the
bubble size distribution, with the objective case of the present work, this option was not
of controlling this latter at its optimum possible as a result of the small section of
value, and (d) using all these tools for the pilot column. Therefore, it is measured
control and real-time optimization purposes. through a semi-analytical technique
The present work is a critical step towards proposed by Pérez (Pérez et al., 1993) and
the final objectives of this CRD program, improved by Grégoire (del Villar et al.,
since the multivariable stabilizing control of 1999), based on the conductivity profile
secondary variables (such as hf, Jb, g, and across the interface position. This approach
Sb), is fundamental for the development and has recently been improved (Maldonado et
the implementation of an indirect (or al, 2008a) by using a non-linear interpolation
hierarchical) real-time optimization strategy. between the two probable values of froth-
This paper presents the results of the depth determined by the “maximum slope
simultaneous constrained control of gas method” (Uribe et al., 1991). A final
872
improvement concerns the measurement of water flow rate in the feed stream, originates
electrical conductivities through a Field- from a steady-state water balance in the
Programmable Gate Array (FPGA), which lower part of the column, underneath the
allows precise measurements over a very feed port. Consequently, the calculated value
large range of conductivities (article recently is very inaccurate (a small value, bias, being
submitted) calculated by subtraction of two large values
subjected to large measurement errors) and
2.1.2 Gas hold-up strongly relies on steady-state conditions,
which excludes its use for control purposes.
Collection zone gas hold-up can be A much better estimation approach was
measured in columns using the hydrostatic proposed by Maldonado et al. (2008b), who
pressure reading at two relatively close related the actual bias rate (Jb) to the
heights of the column. To relate the pressure volumetric fraction of wash water present
difference to the gas content, the value of the underneath the pulp-froth interface (Hw). This
specific gravity of the non-aerated pulp is latter was estimated by the authors through a
required, although seldom available. local ‘conductivity balance’, underneath the
Another device recently introduced is the interface and close to the feed port. For a
Sonar-Trac™ (O’Keefe et al. 2007). In the two-phase system, Hw can then be estimated
case of the present work this latter method using the following expression, where kf and
was excluded as a result of the small cross kw are the conductivity of the feed water and
sectional area of the pilot column, whereas wash water streams.
the first one was not considered because of
the problem of measuring the specific k f k* (2)
gravity of the non-aerated pulp. İw
k f kw
The measure of gas hold-up (volumetric
fraction of gas) in the collection zone is then The conductivity k* of the liquid (without
made using the method proposed by Tavera gas) contained in the ith conductivity-cell of
(Tavera et al., 2002) based on Maxwell's the froth depth sensor, immediately below
equation for electrolyte mixtures (Maxwell, the cell containing the interface, is given by
1892). This equation relates the relative equation 3, where ki is the conductivity of
proportions of a dispersed non-conducting the liquid-gas mixture contained in that cell:
phase (i.e. gas bubbles) and the continuous
k
liquid phase to their respective electrical k * ( P S/cm) ki l (3)
conductivities. The final relation for klg
measuring the gas hold-up is then: From experimental data, it was finally
ksl kslg found that a linear relation exists between J b
İg (1) and Hw. However, obtaining this relation in a
ksl 0.5kslg continuous industrial operation, such of the
where ksl is the conductivity of pulp only present work at the Laronde concentrator, is
(solid and liquid) measured by the siphon quite difficult, since the only independent
cell of the McGill gas hold-up sensor and kslg method of measuring bias (for curve fitting)
is the conductivity of pulp-gas mixture, is a steady-state water balance, an almost
measured by its open cell. Once more, impossible endeavor in plants. Therefore, it
conductivities are measured using the FPGA ZDV GHFLGHG WR VLPSO\ XVH İw as controlled
technique variable.
Esteban-Rojas (2011) adapted this method
to estimate Hw in a three-phase system.
2.1.3 Bias rate Considering that the air hold-up is measured
The original definition of bias (Finch and sufficiently close to the interface and
Dobby, 1990) as the difference between the assuming no solid conductivity, and using
water flow rate in the tailings stream and the the "additivity rule" (Uribe-Salas et al.,1991)
873
for a three-phase system, he proposed the The ultimate goal of this university-
following expression for İw : industry- project is a real-time optimization
(RTO) of the column, which as described
next has not been implemented yet. This
§ 0.5 İ g 1 ·
100 ¨ k f k'slg ¸ layer would calculate on-line the set points
¨ 1 İ g ¸¹
İw © (4) for froth depth, fraction of wash water
k f kw (1 ) s ) underneath the interface and gas hold-up,
leading to optimal grade and recovery values
where kf is the conductivity of feed pulp, A schematic diagram of the proposed
k’slg is that of the pulp-gas mixture advanced control is depicted in Figure 1 (a
underneath the interface, kw is that of the thicker line means a stronger effect from one
wash water and )s is the percentage of variable to another). A PI controller
solids in the pulp. regulates the froth depth by manipulating the
tails speed pump. The volumetric fraction of
2.2 Automatic Control wash water present underneath the pulp-
froth interface and gas hold-up are regulated
A hierarchic structure is usually employed to with a model predictive control (MPC) that
adequately control a process. This pyramidal manipulates the wash water flow rate set
structure is composed of up to four control point and the gas flow rate set point. Model
layers (from bottom to top): instrumentation, predictive control is, by far, the most widely
regulatory control, advanced process control accepted multivariable control algorithm
and real-time optimization. used in the process industry. Several
Instrumentation has been discussed in the commercial MPC technologies allowing
previous section. Regulatory control, the model identification and control with
basic control layer, consists of local mono- constraints can be purchased and successful
variable control loops (usually PIDs) applications are found in many process areas
providing a constant operation for the (Quin et al., 2003).
flotation column inputs: feed flow rate (here The main advantage of MPC is its ability
feasible as upstream fluctuations are damped to handle coupling in multivariable
by the existing feed box), gas flow rate and processes while taking into account various
wash water flow rate. It is also supposed that constraints. In the case of flotation columns,
the feed has been correctly conditioned an important coupling that must be taken
ensuring adequate pH and reagent into account is the significant effect of the
concentration (collectors, frothers, etc.). gas flow rate set point on both the gas hold-
The advanced control layer aims at up and the fraction of wash water underneath
maintaining process (secondary) variables the interface (Figure 1). The importance of
having a strong influence on metallurgical controlled variables for the column operation
results (grade and recovery), such as froth and the operational constraints will be
depth, bias rate, froth parameters, gas hold- detailed in the next paragraphs.
up or bubble surface area flux, etc., in a The position of the pulp-froth interface
bounded region, i.e., an acceptable operating sets the height of the collection zone and
zone where it is possible to handle the therefore is directly related to the time
process and reach production objectives. In available for collection of hydrophobic
our case, the selected controlled variables particles on the gas bubble surface, the other
are froth depth, volumetric fraction of wash factor being the tails flow rate. As a result, it
water present underneath the pulp-froth is partly responsible for the recovery of the
interface and gas hold-up. The manipulated valuable mineral. However, large froth depth
variables are tails pump speed, gas flow rate set point changes would be necessary to
set point and wash water flow rate set point. obtain a significant effect on recovery,
Results of this advanced control will be seriously limiting its use for optimization
presented in the next section. purposes.
874
PI controller
Froth Tails Froth
depth pump depth
set point speed
Flotation column
with its
instrumentation
Gas Gas flow and regulatory Gas
hold-up Constrained rate set controllers hold-up
set point multivariable point
MPC
Fraction of Wash Fraction of wash

wash water water water underneath
underneath flow rate the interface
the interface set point
set point
Figure 1. Schematic diagram of advanced control of a flotation column
Nonetheless, pulp-froth interface position then selecting a gas hold-up set point as high
is an important is a control variable since its as possible would maximize the bubble
constancy is a guarantee of stable column surface area available for particle collection.
operation: a continuously moving interface Therefore, the constraints implemented in
is certainly undesirable since it implies the the MPC algorithm and their justifications
risk of feeding the column in the middle of (Maldonado et al., 2009), are the following:
the froth zone or deepening it so much that a
risk of froth collapse exists. x Gas flow rate set point Jg max
While some authors claim that a slight, - To prevent hydraulic entrainment
but positive, bias value (or fraction of wash - To prevent loss of the interface
water underneath the interface) ensures an - To prevent froth “burping”
adequate cleaning action, others have x Gas flow rate set point > Jg min
established that small values do not - To keep solid in suspension
contribute to reduce the gangue entrainment x Wash water flow rate set point Jw max
(Finch et al., 1990; Clingan et al., 1987). On - To avoid froth mixing
the other hand, high bias values (above 0.4 - To avoid wash water short-circuiting
cm/s) are detrimental since they might
generate increased froth mixing and thus, x Wash water flow rate set point Jw min
drop-back of collected particles (Yianatos et - To promote froth stability
al., 1987). - To easy transfer of collected particles to
Gas is at the heart of the flotation process. the concentrate
Therefore, controlling gas hold-up, bubble x Fract. wash water below interface Hw max
surface area flux or bubble size distribution - To avoid reduction of valuable mineral
appears to be the way to improve the column residence time in the collection zone
metallurgical performance. If, as in the
present case, only gas hold-up is measured, x Fract. wash water below interface Hw min
875
- To perform cleaning action thus reducing manipulated by varying its pump speed. To
entrainment measure froth depth, the pilot flotation
Since the MPC can handle operating column is instrumented with eleven
constraints, an alternative to the RTO stainless-steel conductivity electrodes,
(Maldonado et al., 2009) can be obtained by located in the uppermost section of the
an ingenious use of the advanced-control column. These electrodes are 14 cm external
layer, without implemented the RTO level diameter by 1.5 cm height rings, flush-
itself. The idea of this optimization approach mounted inside the column wall at 10 cm
consists in selecting an unreachable high set interval, for measuring the conductivity
point for the gas hold-up (i.e. equivalent to profile across the interface. Both the wash
maximizing the bubble surface area water and the column feed pipes, are
available for particle collection at a given provided with flow conductivity cells (a pair
collector dosage, thus maximizing recovery), of 3 cm external diameter and 1.5 cm height,
while respecting operating constraints (e.g. 5 cm apart), for measuring the conductivity
ensure a positive bias rate to prevent gangue of the corresponding stream.
entrainment, i.e. lower concentrate grade, as
well as some other constraints listed above).
Results of this original approach on a two-
phase system are presented in the next
section.
3 EXPERIMENTAL SET-UP & TESTS
3.1 Experimental Set-up

The pilot flotation column used in this work
is made of 14 cm internal diameter poly-
carbonate tubes for a total height of 720 cm,
provided with the necessary feed and tailing
ports, as well as a froth overflow launder. A
cylindrical porous stainless-steel sparger
(5 Pm porosity, 340 cm2 area) is located at
the bottom of the column for bubble
generation. A perforated copper ring is
placed over the froth overflow to provide a
gentle wash water spray for concentrate
cleaning.
Wash water (fresh water) is added using a
3.78 l/min gear pump, the flow rate being
measured using a 0.5 to 5 l/min McMillan
micro turbine flow meter. Tailings are
evacuated from the bottom of the column,
using a 0 to 37 l/min peristaltic pump. The
column is fed using a similar pump, from an
intermediate reservoir continuously filled Figure 2. Experimental set-up
with the same feed as the 3rd cleaner column
of the Laronde’s copper circuit, i.e. a slurry Gas hold-up is measured with a reduced
containing between 15% and 25% solids, version of the McGill air hold-up sensor.
99% of the particles being smaller than The tubes, for both open and syphon cells,
100 ȝP &ROXPQ IHHG IORZ UDWH LV measure 5.2 cm diameter by 30cm height
876
and contain two conductivity electrodes, prediction error minimization method

5.2 cm external diameter by 1.5 cm height provided by the Matlab® System
rings separated by 10 cm. The insert in Identification toolbox. Second-order models
bottom part of the syphon cell, can be easily were sufficient to adequately explain the
changed to avoid bubble entrance, according dynamic behaviors.
to the operating conditions The obtained dynamic models were used
As already mentioned, the bias rate was to design the considered controllers (PI and
replaced by its equivalent Hw, whose MPC), which were then tested for tracking
measurement, detailed in previous section, and regulation performance through
relies on available conductivity readings Matlab® simulations. The tuned controllers
from other variable sensors (also described were then implemented in the column
there). The only remaining necessary value, control system and their performances were
solid concentration, is measured with a again evaluated for both tracking and
Marcy balance and manually introduced into regulation.
the iFIX® Hw function. Then, a series of control tests was
Wash water flow rate is controlled using a completed, seeking the evaluation of the
local PI control loop (Moore Mycro 353). controlled column behavior under the
Gas flow rate is regulated by a built-in PI following conditions:
controller within the Aalborg GFC-1737 1) no active constraints: to evaluate the
mass flow controller. Graphical interfaces performance of the closed-loop system
and data acquisition are performed by a and the ability of MPC to handle
HMI/SCADA software iFIX®, working interactions in the column;
under a Windows XP® operating system. An 2) with an active constraint: to evaluate the
Opto 22 I/O system is used to centralize capability of MPC to deal with operation
sensor and actuator signals as shown in restrictions; and
Figure 2. Algorithms for the froth depth 3) long-term functioning: to illustrate the
control and multivariable predictive control robustness of the system facing varying
of İg DQG İw are implemented in Matlab®, operating conditions.
which exchanges information with the
iFIX® database. All signals are sampled at a After reaching a steady-state condition
two seconds interval. following a given set point change, samples
of the feed, concentrate and tailing streams
3.2 Experimental Work were collected for subsequent chemical
The experimental work implied the analysis, aiming at evaluating the
following steps: (a) hydraulic system concentrate recovery and grade achieved
evaluation and sensor calibration, (b) under those conditions. These results would
process dynamic identification and eventually allow determining the operating
controller tuning, (c) control testing and (d) conditions (controlled variables) leading to
sampling to assess the achieved the optimal column performance.
metallurgical performance. Due to the
prevailing space limitations, only step (c) 4 RESULTS AND ANALYSIS
will be detailed here. This section demonstrates the capacity of the
The process dynamic identification multivariable constrained MPC to achieve an
exercise, basically consisted in varying (in effective control of secondary variables of
open loop) over a 2 hour period, a given pilot flotation columns and illustrates its
manipulated variable (alternatively, tail, potential of being included into a RTO
water and gas flow rates) and recording all strategy. Results are first presented on a two-
targeted controllable variables (hf, İw DQGİg). phase system to emphasize the possibility of
The identification of the process transfer optimizing flotation column operation
functions was then made using an iterative without having to implement a complete
877
optimization layer. Then, results obtained in (cm2). The underlying objective of this test
an industrial environment at Agnico-Eagle was to progressively increase the gas hold-
Laronde concentrator are shown. up while maintaining the bias rate above a
minimum limit. From a metallurgical point
4.1 Tests on a Two-Phase System of view, this means maximizing the bubble
surface area for particle collection (i.e.,
These results were previously obtained increasing recovery) while ensuring froth
during preliminary testing of MPC on a two- cleaning (i.e., constant grade). For the first
phase column installed at COREM pilot set point change, applied at 20 minutes, the
plant in Quebec City (Maldonado et al., target gas hold-up is reached but the
2009). The experimental set-up is very specified bias rate could not be maintained
similar to that described in a previous as a result of the upper constraint imposed
section. The control strategy is also similar, on the wash water rate. When the gas hold-
except by the fact that bias rate is directly up set point is changed for a second time (at
controlled, instead of the fraction of wash 65 min), the minimum limit on the bias rate
water underneath the interface. is hit and the desired value for the gas hold-
Figure 3 shows the performance of the up could not be attained. Under these
control system for a series of set point conditions, the MPC strategy maximizes the
changes applied to the gas hold-up. Jw, Jg bubble surface area and ensures that other
and Jt are the superficial velocity of wash operational requirements are met.
water, gas and tails, i.e. the flow rate (cm3/s)
divided by the column cross-sectional area
Figure 3 – Control of a two-phase flotation column: set point (- -), controlled and
manipulated variables (-), constraint (- .)
878
4.2 On-site Tests at Laronde Concentrator can see that, for the first three set point
Test I, shown in Figure 4, presents the changes, the wash water rate reaches the
results of a MPC for tracking set point maximum constraint. These set point
changes on gas hold-up while keeping the changes have minor impact on the gas hold-
fraction of wash water underneath the up, which is reasonable from a physical
interface as constant as possible. In this case, point of view. The addition of wash water
no constraints are active, so that it is has a little effect on the gas hold-up in the
possible to directly appreciate the collection zone. The general performance of
performance of the closed-loop system. The the controller is quite satisfactory for this
time response of the gas hold-up is test
acceptable as well as the control action on The final test (Test III) confirms the
the gas rate. Interactions in the column are capacity of the multivariable constrained
adequately managed by the controller, as the control strategy to operate on a long-term
gas hold-up set point changes do not basis under different conditions. Figure 6
excessively impact the fraction of wash- shows the closed-loop system continuously
water underneath the interface. working for a ten hour period with good
Results for the second test (Test II) are performances in terms of both manipulated
presented in Figure 5. The fraction of wash and controlled variables behavior as well as
water underneath the interface is constraints handling
progressively increased then decreased. One
38
h (cm)
36
f
34
0 20 40 60 80 100 120 140
12
Hg (%)
9
6
0 20 40 60 80 100 120 140
15
Hw (%)
10
5
0 20 40 60 80 100 120 140
25
pump (%)
Tails
20
15
0 20 40 60 80 100 120 140
0.7
J (cm/s)
0.5
0.3
g
0 20 40 60 80 100 120 140

(cm/s)
0.15
0.1
w
J
0.05
0 20 40 60 80 100 120 140
time (min)
Figure 4 – Test I: set point (- -), controlled and manipulated variables (-)
879
38
h (cm)
36
f
34
0 20 40 60 80 100 120 140
9
Hg (%)
8
7
0 20 40 60 80 100 120 140
30
Hw (%)
20
10
0 20 40 60 80 100 120 140
pump (%)
25
Tails
20
0 20 40 60 80 100 120 140

J (cm/s)
0.55
0.5
0.45
g
0 20 40 60 80 100 120 140

J (cm/s)
0.19
0.16
0.13
w
0 20 40 60 80 100 120 140

time (min)
Figure 5 – Test II: set point (- -), controlled and manipulated variables (-), constraint (- .)
40
h (cm)
30
f
20
0 50 100 150 200 250 300 350 400 450 500 550 600
15
Hg (%)
10
5
0 50 100 150 200 250 300 350 400 450 500 550 600
30
Hw (%)
20
10
0 50 100 150 200 250 300 350 400 450 500 550 600
30
pump (%)
25
Tails
20
15
0 50 100 150 200 250 300 350 400 450 500 550 600
1.1
J (cm/s)
0.7
g
0.3
0 50 100 150 200 250 300 350 400 450 500 550 600
0.2
J (cm/s)
0.15
w
0.1
0 50 100 150 200 250 300 350 400 450 500 550 600
time (min)
Figure 6 – Test III: set point (- -), controlled and manipulated variables (-), constraint (- .)
880
Minerals and Metallurgical Processing, Vol. 3,

5 CONCLUSION No. 3, pp. 121-125.
del Villar, R., Grégoire, M., and Pomerleau, A.
This paper presents the multivariable (1999). Automatic control of a laboratory
constrained control of a pilot column flotation column. Minerals Engineering, Vol. 12
installed in the Agnico-Eagle’s Laronde No. 3, pp. 291-308.
concentrator. The controlled variables are del Villar, R., Desbiens, A., Maldonado, M., and
froth depth, fraction of wash water Bouchard, J. (2010). Automatic Control of
underneath the interface and gas hold-up, all Flotation Columns. In D. Sbárbaro and R. del
estimated from electrical conductivity Villar (Eds.), Advanced Control and Supervision
measurements. A PI controller regulates the of Mineral Processing Plants (pp. 249-286).
froth depth, whereas a multivariable London: Springer-Verlag.
predictive controller maintains the fraction Esteban-Rojas, R.M. (2011). Validation industrielle
of wash water underneath the interface and de la mesure du différentiel d’eau dans une
the gas hold-up to their respective set points, colonne de flottation (Mémoire de maîtrise).
as long as operational constraints are Département de Génie des mines, des matériaux
respected. et de la métallurgie, Université Laval, Quebec.
This control scheme allows an indirect Finch, J.A. and Dobby, G.S. (1990). Column
optimization by setting an unreachable high Flotation, Pergamon Press, Oxford, UK.
set point of air hold-up, thus maximizing the Gomez, C.O., and Finch, J.A., 2007. Gas dispersion
bubble surface area available for particle in flotation cells. International Journal of
collection, while maintaining bias rate above Mineral Processing, Vol. 84, pp. 51-58.
a minimum value required for froth cleaning. Jelali, M. (2006). An overview of control
Also, several steady-state tests were performance assessment technology and
performed, during which the three controlled industrial applications. Control Engineering
variables were kept constant and feed, tails Practice, Vol. 14, pp. 441-466.
and concentrate samples were drawn at Maldonado, M., Desbiens, A., and del Villar , R.
steady-state conditions. Analysis of the (2008a). An update on the estimation of the froth
samples allowed establishing relationships depth using conductivity measurements. Minerals
between primary and secondary variables, Engineering, Vol. 21, pp. 935-939.
which will be later used in the design of a Maldonado, M., Desbiens, A., del Villar, R. and
new real-time optimization. Chirinos, J. (2008b). On-line bias estimation
using conductivity measurements. Minerals
6 ACKNOWLEDGEMENTS Engineering, Vol. 21, pp. 851-855.
Maldonado, M., Desbiens, A., del Villar, R., Girgin,
The authors would like to thank NSERC, H. and Gomez, C.O. (2008c). On-line estimation
AEM - Laronde concentrator, XStrata Nickel of bubble size distributions using Gaussian
- Strathcona concentrator and COREM for mixture models, Kuyvenhoven, R., Gomez, C.,
their financial support, Marlène Lanouette, Casali, A., (Eds.), 5th Int. Mineral Processing
Claude Bolduc and Alexandre Morasse Seminar – Procemin, pp. 389-398.
(Laronde metallurgists) for their precious Maldonado, M., Desbiens, A. & del Villar, R.
technical help during the plant tests, and (2009). Potential use of model predictive control
Ricardo Esteban-Rojas, Ghislain Sindjui- for optimizing the column flotation process.
Towo and Tomas Glaria (then students at International J. of Mineral Processing, Vol. 3,
Université Laval) for their contributions to pp. 26-33.
the equipment installation and start-up Maldonado, M., Desbiens, A., del Villar, R. and
and/or during the control tests. Aguilera, R. (2010a). On-line estimation of
frother concentration for flotation processes.
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(Eds.), Vol. 2, CIM, Sudbury, ON, pp. 391-407.
Yianatos, J.B., Finch, J.A., and Laplante, A.R.
(1987). The cleaning action in column flotation
froths. Trans. of the IMM, Section C96, C199-
C205.
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Recovery of Lithium Rich Mica from Mineral Waste
Z. Iqbal, N. A. Rowson, S. Blackburn

School of Chemical Engineering, University of Birmingham, Birmingham, UK
ABSTRACT Lithium is a strategically important metal for the UK and Europe due to the
limited availability of primary deposits of sufficient grade for economical processing in close
geographical proximity. Recent increases in lithium’s application in electrical technology
driven devices, such as: lithium ion batteries, has seen a great interest in developing
secondary sources of lithium for secure reserves. As lithium is a finite resource, if methods
are not investigated to recover the metal from secondary sources problems with its
availability and price may soon limit the development of the next generation of battery
technology.
This paper investigates mineral processing techniques for the extraction of lithium rich
mineral concentrates, in order to recycle lithium hence making it a sustainable source for
future generations. Various separation methods were investigated to develop a mineral
processing flow sheet for lithium concentrates from existing waste streams. Using this
technique sufficient lithium concentration levels were obtained with a recovery rate of up to
96%, thus making the process of potential interest.
1 INTRODUCTION Previous reports (J. R. Hawkes, 1987)

show that, lithium mica has been identified
1.1 Background as a waste product in the early stages of the
Over recent years, the demand for lithium process; it is produced as hydrocyclone
has increased, primary due to the increased underflow from the kaolin production
process. At present, the waste material has
use of lithium batteries in electrical devices; no use thus it is discarded. In order to
it is now classified as a strategically recover the metal lithium, initially we must
important metal (McKnee, 2011). Other separate the lithium bearing mineral,
applications for lithium include: glass, lepidolite, K(Li,Al)3(Si,Al)4O10(F,OH)2. This
ceramics and primary aluminium production can be achieved using various physical
(USGS, 2010). separation techniques, in this study the most
In one of Europe’s largest industrial significant lithium recoveries were obtained
mineral processing producers operations, using froth flotation. Lepidolite a lithium
significant amounts of waste product from rich mica, K(Li,Al)3(Si,Al)4O10(F,OH)2, that
kaolin production contains a lithium bearing has a high aspect ratio, flaky structure and a
mineral, Lepidolite, has been detected as a distinct lilac colour. Lepdiolite is a member
by-product. By attempting to recycle the of the mica group; these are silicate minerals
waste product to recover lithium, we are not that have silicon and oxygen as their two
only reducing the rate at which lithium ores major components. Other members of the
are utilized but also maintaining the mica group include: biotite,
environment balance by reducing waste K(Mg,Fe)3AlSiO10(F,OH)2, and muscovite,
produced by industries. KAl2(AlSi3O10)(F,OH)2, which act as
impurities in this study.
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The fundamental principle of froth studies indicated that optimal recovery was
flotation separation utilizes the differences achieved with a of particle sizes between 53-
in the surface chemistry of the minerals 250ђm. The hydrocyclone underflow was
species present in the kaolin waste. Minerals
can be classified into two groups: polar and initially screened to remove particles less
non-polar. Polar minerals are minerals that than 53ђm, as these compromise froth
have strong covalent or ionic surface flotation efficiency. The feed samples were
bonding with high free energies. Non-polar analysed using a particle size distributor,
mineral surfaces have weak molecular bonds QICPIC (HELOS/BF Sympatec), which
and are difficult to hydrate; as a result they performed a high speed analysis determining
are hydrophobic. These minerals form a the particle size and density distribution of
froth layer when air is passed through the
flotation cell and thus are collected as the the samples to show the efficiency of the
flotation concentrates (Rowson, 2010). In separation.
order to enhance the flotation concentrate we
can add reagents such as depressors,
collectors and frothing agents.
In order to determine the lithium
concentration in the flotation concentrate,
inductively coupled plasma (ICP) was
utilised. ICP uses emission spectroscopy to
quantify the elements. Atomic emission
spectroscopy detects and measures elements,
intensity of light emitted at specific Figure 1: Particle Size distribution of 53-250ђm
wavelengths. The samples are initially
heated at very high temperatures in order to
excite electrons. Atoms absorb energy by
collision thus are heated up which results in
excitation. The electron which is furthest
away from the nucleus moves into a higher
energy orbit which is unstable, thus the
electron drops back to its original position.
The energy difference this creates is omitted Figure 2: Particle Size distribution of 250-500ђm
in light energy which is detected and the
wavelength measured. The intensity of the
light omitted is due to the atoms excited as
shown by Manning T.J., Grow W.R., (1997). 1.2.2 Analytical procedures
ICP indicates the quantitative analysis of
lithium present. The samples were analysed using various
techniques to find the mineral and chemical
composition and lithium concentration of
1.2 Experimental the feed and separation products formed.
The quantitative chemical analysis was
1.2.1 Material carried out using a combination of: X-ray
fluorescence (XRF) and inductively coupled
The feed material was obtained from an plasma (ICP) by the following
industrial mineral processing company in manufactures: Bruker S8 Tiger X-Ray
Europe. It was taken from the early stages of Fluorescence Spectrometer and
the process, hydrocyclone underflow; which Thermoscientific iCAP 6000 series ICP
currently has no use and is discarded. The spectrometer, respectively.
hydrocyclone underflow is rich in various
mica species; previous reports (J. R. 1.2.2.1 Froth flotation separation
Hawkes, 1987) have found it may contain
lithium mica. This waste material has been The lithium concentration and recovery
used as the starting point for the experiments were carried in a Denver cell
development of a lithium concentrate with a 3 litre cell. The impeller speed was
recovery process flowsheet. Experimental set at 1500 reeves per minute. The feed
888
sample used for each experiment was 500g The highest, 0.071%, was found in the
which was then mixed with tap water to fill particle size range of 53-250µm. Similar
the cell. The mixture was then conditioned results were obtained with the particle size
at pH 1.5 for five minutes by the addition of range 250-500µm, here we obtained Li2O
sulphuric acid. The depressor was then (%) between 0.062-0.065% lithium feed
added, it reduces the impurities collected in concentrate. Hence further separation
the final concentrate, Cyquest 40E techniques were used in this particle size
Antiprecipitant (supplied by Cytec range. The lowest Li concentration levels
Industries, UK). The cationic collector used were found below 53µm.
was AEROMINE 3030C Promoter
(supplied by Cytec Industries, UK). The
amount of depressor and collected added
was varied in order to optimise the lithium
concentrate recovered.
1.2.2.2 X-ray fluorescence
The samples were prepared into pressed
pellets by mixing 0.5g of the sample with
0.1g of wax (supplied by Specac Ltd, UK).
The samples were analysed by full analysis Figure 3: Relationship between lithium oxide
which ran for eight minutes, this then gave content and particle size in ore deposit
us the elements/oxides present in the
pressed pellet. The results show that 2.1 Particle size range 53-250ђm
rubidium oxide (for the mineralogy of this
specific deposit) is a good indicator for Flotation experiments were conducted using
lithium recovery hence we can use it to samples from the particle size range 53-
estimate the initial recovery rate as it is 250µm. The optimal pH for the experiments
much easier and accessible form of analysis. was found to be 1.5, under these conditions
both the greatest lithium concentration and
1.2.2.3 Inductively coupled plasma recovery rate, 0.47% and 99% respectively
were obtained. Other experimental
Prior to lithium analysis the powder samples parameters (such as collector and depressor
were prepared into solutions. The samples dosage levels) were investigated at pH 1.5.
were weighed and 0.1g was mixed with Figure 5 and 6 compare the depressor and
0.95g of sodium tetraborate (BORAX), collector dosage, respectively.
followed by heating at 1000oC for 10
minutes. The samples were allowed to cool
down before adding 50 ml of a 3% solution
of nitric acid and then placing them in a
water bath for 30 minutes. The solutions
were then filtered using 12.5cm Whatman
No.40 filter paper into 100ml volumetric
flasks, the flasks where then diluted with
distilled water. The samples were then
analysed for the amount of lithium metal
they contained.
2 RESULTS AND DISCUSSION

Figure 4: Flotation recovery of Li2O, constant
Various particle size ranges of the feed
sample were analysed for lithium content.
889
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pr
variables were: depressor ge
and collector dosage to economically recover lithium from this
(6m
6ml/
6m l/kg
l/kg).
kg).
(6ml/kg). specific ore deposit – others are now being
investigated for processing potential.
Figure 5: Flotation recovery of Li2O, constant

variables were: pH (1.5) and collector dosage
(6ml/kg). Figure 7: Flotation recovery of Li2O, constant
variables were: pH (1.5) and depressor and collector
dosage (6ml/kg).
3. CONCLUSION
Using froth flotation a 0.47% lithium

concentrate was produced from a 0.071%
very low grade feed material, with a
recovery rate of 99%.
Further work will involve optimising the
process flowsheet for the lithium
concentrate to make it more suitable for
downstream processing.
ACKNOWLEDGEMENTS
Figure 6: Flotation recovery of Li2O, constant This study was sponsored by Engineering
variables were: pH (1.5) and depressor dosage and Physical Sciences Research Council.
(6ml/kg).
REFERENCES
2.2 Particle size range 250-500ђm McKnee, G, 5, 2011. House of Commons,
Strategically important metals. Science and
Further investigations were carried out on Technology Committee, 1, pp.1-146.
the optimal conditions, which were: pH 1.5, Brian W. Jaskula, 2010. USGS, Mineral yearbook,
collector dosage 6ml/kg and depressor
6ml/kg. Lithium, pp.1-12.
Figure 7, shows that the experiments J,R, Hawkes, 1987. British geological survey, The
processing the smaller particle size range 53- lithium potential of the St Austell granite, 19.
250ђm, gave a greater lithium concentrate Siame, E, Pascoe, RD, 24, 2011.. Minerals
grade compared to the coarser size fraction Engineering, Extraction of lithium from
of 250-500ђm. This is thought to be due to micaceous waste from china clay production,
inefficient liberation of the lithium from the pp.1595–1602.
granite/kaolin matrix. Although the final
concentrate values are still too low in order Rowson, NA, 2010.. Mineral purification
890
techniques, pp.1-36.
Manning, TJ, 1997.. The chemical educator,
Inductively Coupled Plasma-Atomic Emission
Spectrometry 2, pp.1430-4171.
Amarante, MM, 1999.. Processing a spodumene ore
to obtain lithium concentrates for addition to
glass and ceramic bodies volume, page interval,
12, pp.433-436.
891
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916
Fractional Method of Sulfide Copper Ore Processing

A. Boteva, M. Parashkevova
Mining and Geology University St. "Ivan Rilski" Sofia-1700 , Sofia-2095

ABSTRACT Global experience shows that the use of fractional technologies provides
opportunities for economically viable complex ore processing. This study addresses the
possible use of fractional technologies for processing of complex gold-containing raw
materials. The ore has high pyrite content and part of this pyrite is gold-carrier, and another
part is not. Copper mineralization is represented by a set of primary and secondary sulfides. If
all the pyrite is removed, a large portion of the gold is lost, too. If the pyrite is left in the
copper concentrate, the latter is of poor quality. One solution of this problem is the fractional
technology. The study focused on the different influence of collectors on flotation kinetics of
ore components. The purpose of the study was to monitor copper and gold recovery kinetics
in the common concentrate and the cooper/gold ratio in individual fractional concentrates
employing xantogenate and mercaptobenzothiazole as collectors, jointly and separately. The
collectors were selected on the basis of the difference in the nature of bonds ensuring
adsorption of the respective sulfhydrile collector on sulfide mineral surfaces. Study results
showed that separation was possible for copper concentrate fraction with gold-containing
pyrite. The remaining pyrite had low gold content. In this low-gold-content fraction, the pyrite
was depressed and disposed with the residue. High-quality copper concentrate was obtained
and then blended with the remaining gold-containing pyrite to produce standard copper
concentrate with high gold content.
Key Words: fractional, flow sheet, sulfide copper ore, gold, pyrite
1 INTRODUCTION We looked for solution of this problem in

Sulfide copper ores with high pyrite and the differences of flotation rates with the use
gold content are one of the best studied of different collectors, which, for copper
minerals in technical aspect [Boteva, 2002]. sulfides are a large number [Boteva, 1992].
Nevertheless, the issue of separation of Correlation of such collectors to the other
gold-containing from non-gold-containing important sulfide mineral present in ore -
pyrite remains unresolved. If all the pyrite is pyrite – is especially important. Therefore,
removed, a large portion of the gold is lost, our research focused on isobutyl
too. If the pyrite is left in the copper xanthogenate and mercaptobenzothiazole.
concentrate, the latter is of poor quality.
This problem is particularly significant
where copper sulfides are not copper-rich
minerals such as chalcocite, covellite, and
bornite. In such cases, high quality of copper
concentrates is quite difficult to be achieved.
917
$%RWHYD03DUDVKNHYRYD
2 MINERALOGICAL DESCRIPTION machine with variable flotation cell volume

OF THE ORE SAMPLE AND was used for flotation. Collectors included
CHARACTERISTICS OF SELECTED isobutyl xanthogenate, double purified via
REAGENTS crystallization from alcohol solution, and
pure mercaptobenzothiazole dissolved in
The ore sample subjected to mineralogical ethyl alcohol.
analysis belongs to compact sulfide copper-
pyrite-polymetal ores with high gold content 3 RESEARCH METHOD AND
in copper minerals, quartz sulfide veins and RESULTS
pyrite. The enargite, with Cu content of
48,78 %, is the main mineral. Tetraedite, Research methods included open and closed
tennantite, chalcopyrite, bornite are also cycle flotation trials with different
present. Iron sulfides are represented mainly collectors. The other reagents were kept the
by pyrite /sometimes up to 80 % of the ore same and were noted on the relevant
minerals/ and by marcasite. Galenite and schemes. The results are presented in tables
sphalerite are also found. Gold is found both and on comparative graph. Figures 1, 2, 3
as virgin and as ore inclusion. In view of the show the schemes employed for flotation
significant pyrite quantities, gold is froth removal in portions for the purpose of
distributed quantitatively equally in copper flotation kinetics analysis of copper minerals
sulfides and pyrite. Ore sample composition and gold under different regimes. Results
is represented by copper of– 1,86 %; iron- are presented in tables 1, 2, 3, and the
14,30 % ; sulfur-18,81 % ; silver- 12,9 g/t comparison – on figure 4. Closed cycle trial
and gold- of 3,93 g/t. After crushing to 0-3 schemes are shown on figures 5 and 6, and
mm, the sample was processed in ball mill the results thereof - in tables 4 and 5.
to 0,08 mm 70 % by weight. Denver
Table 1. Flotation results by flow sheet on Figure 1

Products Assay Recovery,E ECu/EAu
Cu,% Au,g/t Cu,% Au,%
I concentrate 4,41 9,32 77,20 83,66 0,92
II concentrate 3,17 4,81 12,45 9,69 1,28
III concentrate 1,17 1,94 3,13 2,66 1,17
IV concentrate 1,44 1,54 2,00 1,10 1,82
V concentrate 1,47 0,63 0,83 0,18 4,61

I concentrate 10,20 12,50 40,85 22,93 1,78
II concentrate 4,95 6,15 9,34 5,31 1,76
III concentrate 3,79 5,55 9,37 6,29 1,49
IV concentrate 2,63 6,61 6,92 7,97 0,87
V concentrate 2,30 6,28 5,99 7,47 0,80
918

I concentrate 8,04 9,29 37,54 19,59 1,92
II concentrate 3,73 6,31 38,01 29,04 1,31
III concentrate 1,96 12,37 14,56 41,60 0,35
IV concentrate 1,79 4,40 2,97 3,30 0,90
V concentrate 1,57 5,04 1,15 1,67 0,67

Product Yield Assay Recovery
Copper concentrate 10,03 17,17 36,45 93,67 89,17
Tail 89,97 0,13 0,49 6,33 10,83
Ore feed 100,00 1,86 4,10 100,00 100,00

Products Yeild Assay Recovery
I copper concentrate 3,66 20,13 28,01 40,30 25,30
II copper concentrate 6,25 16,12 46,12 55,02 70,98
copper concentrate 9,91 17,60 39,07 95,32 96,60
tail 90,09 0,10 0,18 4,68 3,72
Feed ore 100,00 1,83 4,05 100,00 100,00
4 TRIAL RESULT ANALYSIS of copper minerals is extracted, though very

poorly, most probably in the form of
Trials with fractional froth removal in fig. 1- accretions with pyrite and adjoining rock
3 and change of collectors showed the minerals. If MBT is fed in the beginning
following: Fig. 1, copper minerals and the gold
The well-known fact was confirmed that contained therein are extracted. Then
mineral flotation rate expressed as ȿ IW is xantogenate is introduced leading to sharp
strongly dependent on the collector used. change of copper/gold ratio extraction in
Xanthogenate extracts sulfide minerals Table 3 thus ensuring good gold extraction,
without differences between copper sulfides the gold being mainly the pyrite – bonded
and pyrite in table 1. With variety.
mercaptobenzothiazole ɆȼɌ, the results
are different. Lack of collecting properties The results /graph on fig. 4/ allowed us to
with regard to pyrite in table 2 is evident. develop a closed cycle trial scheme as
We used as indicator for this purpose the compared to the classical scheme used in
gold contained in the pyrite. Gold bonded to practice in fig. 5 and fig. 6. Consecutive
copper minerals is extracted in the first four feeding of MBT and isobutyl xanthogenate
minutes and thereafter the remaining portion in the process ensured, by employing
919
ore
factional scheme, substantial increase of
isobutyl kst 60g/t line pH 10
copper and gold extraction. Obtaining two
griding 70%-0,08mm
concentrates in fig. 3 and subsequent minfroth 40g/t
blending thereof /table 5/ allowed for f lotation 2min
increased extraction of both gold and 10g/t kst
copper. These are most probably copper- I concent f lotation 2 min
pyrite accretions. 20g/t kst
II concent f lotation 2 min
5 CONCLUSIONS 5g/t kst
f lotation 2 min
Trial results led to the following III concent
5g/t kst
conclusions: IV concent f lotation 2 min
1.Fractional schemes using more than one

tail
collector fed consecutively allowed V concent
obtaining of copper concentrates with the Figure 1 Flowsheet with izobutyl ksantogenate
required copper content and good extraction
MBT 60g/t ore
of the gold contained in pyrite. lime Ph10
2. Given the current state of technology, grinding 70%-
0,08mm
gold losses in some of the pyrite are minfroth 40g/t
inevitable. Such losses are reduced where f lotation 2 min
copper sulfides are rich in copper MBT 20g/t
/chalcocide, covelline, bornite/ since more I concent f lotation 2 min
pyrite can be absorbed without affecting MBT 20g/t
profitable metallurgical processing of copper f lotation 2 min

II concent
concentrates.
MBt 20g/t
3. Except for MBT in combination with f lotation 2 min
xenthogenate , such experiments should be III concent
MBT 20g/t
carried out with other known collectors f lotation 2 min
which are selective in respect of copper IV concent
sulfides else [Bhambhani , 2012].

V concent tail
4. Technological opportunities for
separation of gold-containing from non- Figure 2 Flowsheet with merkaptobenzoltiazol /MBT/
gold-containing pyrite, through different in

terms of flotation susceptibility [Bogdanov,
1990], remain unutilized. Fractional
schemes are one way for such utilization.
920
ore flotation feed

MBT 40g/t lime pH 10
grinding 70% - grainding 70% -

0,08mm 0,08mm
minfroth 40g/t
f lotation 2 mins kst 20g/t I rougher f lotation
f lotation 2 mins
I concent
kst 20g/t
cleaner f lotation II rouger f lotation
f lotation 2 mins
II concent
kst 20g/t
tail
regrind
III concent f lotation 2 mins I copper concentrate R
kst 20g/t
f lotation 2 min I cleaner

Ivconcent
II cleaner
V concent tail
Figure3 Flowsheet with ksantogenate and merkaptobenzoltiazol

III cleaner
Relationship betw een ECu/EAu ratio and

flotation tim e
II copper concentrate
5
Figure5 Fractional flowsheet
4
ECu/EAu
Series1
3 flotation feed
Series2
2
Series3 grinding 70%-
1 0,08mm
0
rougher f lotation
1 2 3 4 5 6
flotation tim e,m in tail
I cleaner
Figure 4. Relationship between ECu/EAu

ratio and flotation time II cleaner scavenger
Series 1-by flow sheet in fig.1

III cleaner
copper concentrate
Figure 6 C-S flow sheet
921
REFERENCES
Boteva A, Thenika, 2002, Flotation technologies,

Sofia, 226p.
Boteva A, Thenika, 1992, Flotation reagents, Sofia,
250 p.
Bhambhani, T, 2012, Flotation Matrix 100 ,
XXVIMPC, NewDelhi, India, volume 2, p 381,
Bogdanov, O, Nedra, 1990, Teoria and technologia
flotation ore, Moskva 361 p.
922
Recovery of Copper from Sulfide-Oxide Ore by Flotation-

Leaching Technique
D. Moradkhani
University of Zanjan, Zanjan, Iran
H. Hamidinezhad
Imam Khomeini International University, Qazvin, Iran
M. Rajaie Najafabadi
Amirkabir University of Technology, Tehran, Iran
B.Sedaghat
R&D Center, Research & Engineering Co. for Non-ferrous Metals (RECo), Zanjan, Iran
ABSTRACT The aim of this study is to obtain the maximum copper recovery from the
copper sulfide-oxide ore by optimization of effective parameters of copper sulfides using
orthogonal array L18 (22 × 36) of Taguchi method and acid leaching of the optimum flotation
tailing (copper oxides) under optimum working conditions. The flotation test was optimized
with Design Expert 7 software. The optimum conditions were found to be: pH: 11, collector
dose rate: 300 gr/t, activator addition rate: 100 gr/t, time: 7 min, aeration rate on: 3 lit/min,
VROLG SHUFHQW SDUWLFOH VL]H ȝP DQG PL[LQJ VSHHG USP 8QGHU WKHVH
conditions, copper sulfides were floated and recovery and grade of copper obtained 68.36%
and 14.92% respectively at rougher stage. Tailing of the optimum flotation test was leached
and 441.2 ppm of copper obtained from leaching test with 98.69% of copper oxides recovery.
Finally, total copper recovery at 72.86% was obtained by using flotation-leaching process and
a process flowchart was presented.
Key Words: Copper sulfide-oxide ore, Optimization, Taguchi, Flotation- Leaching process.
1 INTRODUCTION molecular level are still not well known
(Montes and Montes Atenas, 2005). The
Froth flotation is a separation method used improvements in flotation efficiency usually
for the beneficiation of a considerable tend to the increase metal recovery and
portion of the world's mineral ores (Deglon, concentrate grade. However, at many
2005). It is a complex combination of concentrator plants the chances of improving
various physical principles, such as flotation efficiency, using only physical
surface chemistry, colloid chemistry, methods, are currently limited
crystallography, and physics. Various factors (Luszczkiewicz and Chmielewski, 2008).
influence the performance of a flotation unit, Copper ore is mainly copper sulfide or
among these are the bubble size (Gorain et copper oxide ore. Many copper sulfide
al., 1995), the stator and rotor configuration mines around the world have significant
(Forrester et al., 1998), the type and quantity copper oxide ore reserves associated with
of chemicals added (Evans et al., 1995; the larger primary copper sulfide deposit
Ralston et al., 2001) and residence time (Lee et al., 2009). An important problem
(Rubio et al., 2002). Collector specificity facing the copper industry in the world is the
and its role on the separation process at a recovery of oxide copper minerals because
923
'0RUDGNKDQL++DPLGLQH]KDG15DMDLH1DMDIDEDGL%6HGDJKDW
they float poorly. It is expected that the 2 EXPERIMENTAL

reverse flotation technique may be
appropriate to recover such oxide copper 2.1 Materials
minerals from the accompanying mineral
oxides/sulfides (Saleh et al., 2008). The copper sulfide-oxide ore used in this
Generally copper oxide minerals do not research was obtained from the Chodarchaie
respond well to traditional sulfide copper mine, northeast of Zanjan, Iran. After drying,
collectors and require alternative flotation crushing and homogenizing, the sample was
techniques to concentrate the copper oxides. JURXQGHGWRDQGȝPXVLQJDEDOO
For example, Lee et al. (2009) found out mill in order to obtain various particle sizes.
those N-octyl hydroxamate collectors such Figure 1 shows the XRD analysis of the
as AM28 can be used successfully to recover sample. It indicated that the main copper
the oxide mineral component in mixed minerals in the ore were chalcopyrite and
copper sulfide-oxide blends. malachite.
In order to change the ore structure and The chemical analysis of the sample was
surface properties, process of sulfurization carried out by a Perkin-Elmer AA300 model
should be considered before the flotation atomic absorption spectrophotometer. Table
(Aydin et al., 2005; Ziyadanogullari and 1 summarizes the chemical composition of
Aydin, 2005; Akgün et al., 2006). Usually the copper ore used in the experiments. The
sodium sulfide is the sulfidizing agent which amount of copper in the sample was 1.28%
yields the best performance in most flotation which consisted of 1.09% copper sulfide
systems (Rey and Raffinot, 1953; Rey et al., (Chalcopyrite) and 0.19% of copper oxide
1954; Rey, 1979). (Malachite).
A leaching process can often be selected
for dissolving valuable metals from an ore or Table1. Chemical composition of sample
a secondary resource; while leaving most of used in the experiment (Wt.%)
the gangue largely unaffected. A large
Component Wt. (%)
number of studies have been carried out to
optimize these processes (Arslan and Arslan, Cu 1.28
2002; Wang and Zhou, 2002). Copper oxide Fe 2.28
minerals such as azurite, malachite, tenorite Zn 1.28
and chrysocolla are completely soluble Pb 0.23
either in acidic or alkaline medium at room Ca 0.19
temperature (Barlett, 1992 ; Ata et al., 2001; Ni 0.007
Oudenne and Olson, 1983). It has been very Mn 0.31
well known that sulfuric acid is the most
usual leaching agent for oxidized copper ore.
The aim of the present study is to obtain 2.2 Procedure and Equipment
the maximum copper recovery from the According to the various values of the solid
copper sulfide-oxide ore by optimization of percent and particle size parameters, the
effective parameters of copper sulfides sample was mixed with water to produce a
flotation (pH, collector dose rate, activator flotation feed. The experiments were
addition rate, time, aeration rate, solid implemented in a laboratory Denver flotation
percent, particle size and mixing speed) cell and pH was controlled by Inolab pH
using Taguchi method and Design Expert7 meter during the tests. The pH of the pulp
software and then acid leaching of the was adjusted with milk of lime.
flotation tailing (copper oxides) under The chemicals added in the process were
optimum working conditions (pH, as: activator (Na2S), collector (Potassium
solid/liquid ratio, temperature and leaching Amyl Xanthate) and frother (Pine oil). Each
time). stage of chemical addition having 2 minutes
conditioning period during the experiments.
924
The aeration rate was controlled with a Matar, 1990; Syrcos, 2003; Kamaruddin et
designed flow meter and the concentrate was al., 2010).
then collected for different time of flotation S/N ratio is formulized with the following
by bubbling air through the pulp. equation (Taguchi, 1987):
After optimization of flotation process,
the tailing of optimum flotation test was (1)
dried and homogenized. Then copper oxides
recovered from the tailing by leaching in
suitable conditions. Where n is the
number of repetition for an experimental
combination and yi is a performance value of
the ith experiment.
In this research to optimize copper
Intensity
flotation, Taguchi technique was used.

Primitive rough tests indicate that eight
parameters including: mixing speed, solid
percent, pH of pulp, collector dose rate,
2ș
aeration rate, time, particle size and activator
addition rate are effective. Thus, to
Figure 1. X-ray diffraction analysis of the investigate the effects of above mentioned
ore parameters in copper flotation, different
levels of them were selected. Copper grade
and recovery were selected as the responses.
2.3 Taguchi Method Orthogonal array L18 (22×36), which clarifies
The Taguchi method, introduced by Dr. 6 parameters at 3 levels and 2 parameters at
Genichi Taguchi, contains system design, 2 levels, was chosen to carry out the tests.
parameter design and tolerance design Table 2 shows the experimental procedure.
procedure to gain a robust process and result
3 RESULTS AND DISCUSSION
for best product quality.
Taguchi designs experiments using 3.1 Flotation
specially constructed tables known as
orthogonal array (OA). The use of these As the sulfide part of the ore can be
tables makes the design of experiments very extracted using flotation technique, the feed
easy and consistent, and it requires relatively firstly go to the flotation stage. After
lesser number of experimental trials to study extracting copper sulfide as the flotation
the entire parameter space. As a result, time, concentrate; the flotation tailing (copper
cost, and labour saving can be achieved. The oxide) can be extracted by acid leaching.
experimental results are then transformed
into a signal-to-noise (S/N) ratio (Roy,
1990).
These S/N ratios are meant to be used as
measures of the effect of noise factors on
performance characteristics. S/N ratios take
into account both amount of variability in
the response data and closeness of the
average response to target. There are several
S/N ratios available depending on type of
characteristics: smaller is better, nominal is
best (NB) and larger is better (Lochner and
925
Table 2. Experimental procedure

Mixing Solid Collector Aeration Time Particle Activator
No. speed Percent pH dose rate rate (min) size: d80 addition
(rpm) (%) (g/t) (l/min) (µm) rate (g/t)
1 1000 15 10 200 4 5 80 200
2 1000 10 10 100 3 6 120 200
3 1000 15 11 300 3 6 100 100
4 900 15 9 300 5 6 80 200
5 1000 10 9 300 4 5 100 150
6 900 15 11 100 5 5 100 200
7 900 10 11 300 4 7 120 200
8 1000 10 11 200 5 7 80 100
9 900 15 10 100 4 7 100 100
10 900 15 11 200 3 5 120 150
11 900 10 10 200 5 6 100 150
12 1000 15 9 200 3 7 100 200
13 1000 15 9 100 5 7 120 150
14 900 15 10 300 3 7 80 150
15 900 15 9 200 4 6 120 100
16 1000 15 10 300 5 5 120 100
17 1000 15 11 100 4 6 80 150
18 900 10 9 100 3 5 80 100
3.1.1 Effect of parameters on the copper indicates that higher collector dose rate has
sulfides recovery higher effect on the recovery of copper.
Figure 2 illustrates the effect of mixing
speed, solid percent, pH and collector dose
rate on the copper recovery.
As seen in figure 2(A), increasing the
mixing speed up to 1000 rpm increased the
Cu recovery. Due to more contact between
solid particles and collector molecules, the
connection of these particles increases and
so the recovery of copper also enhances.
According to experimental results
presented in figure 2(B), the recovery of Cu
decreased as the solid percent increased.
Decreasing the solid percent causes to create
more chances for solid particles to be
connected with collector molecules and thus
the copper recovery will be increased.
In this research 3 levels of pH of 9, 10,
and 11 were investigated. As seen in figure
2(C) increasing of the pH, increased the Figure 2. The effect of mixing speed, solid
copper recovery. It seems that pH of 11 is percent, pH, and collector dose rate on the
suitable for copper flotation. copper recovery
As the collector dose rate increases, the
probability of contact between solid Based on what figure 3(E) indicates, higher
particles and collector molecules also aeration rate between levels 1 and 2 has
increases and thus the probability of copper lower effect on the recovery of copper and
particles to be floated rises. Figure 2(D) the effect of this parameter on copper
recovery was insensitive between levels 2
4
926
and 3. High aeration rate causes disturbance percent increased. As the solid percent
in the pulp and this turbulence makes the increases, the probability of connection
mineral particles to be separated from air between solid particles and air bubbles
bubbles, so less copper would enter the decreases and thus both the grade and
concentrate. recovery reduce.
The time parameter was examined in 3 As can be seen from figure 4(C), higher
levels of 5, 6 and 7 minutes. Effect of time pH has higher effect on the grade of copper.
on the copper recovery is shown on the This is probably because that the pH of 11 is
figure 3(F). The more time spends, the more more effective for recovering the free
copper minerals enter the concentrate; but in particles of copper.
return, the grade of the concentrate would According to experimental results
decrease with time spending. presented in figure 4(D), the grade of copper
Figure 3(H) shows that increasing the increased as the collector dose rate increased
activator addition rate up to 200 g/t, between levels 1 and 2, but it some
decreased the copper recovery. It seems that decreased as the parameter increased
by increasing the Na2S concentration, this between levels 2 and 3. More than a certain
material acts as a depressant. collector concentration causes CMC (critical
In this study, the effect of particle size on micelle concentration) which results in
the copper recovery because of its reducing grade.
insensitive effect was pooled.
Figure 4. The effect of mixing speed, solid

Figure 3. The effect of aeration rate, time percent, pH, and collector dose rate on the
and activator addition rate on the copper copper grade
recovery
Figure 5 illustrates the effect of aeration
rate, time, particle size, and activator
3.1.2 Effect of parameters on the copper addition rate parameters on the copper
sulfides grade
grade.
Figure 4 illustrates the effect of mixing In this research 3 levels of aeration rate of
speed, solid percent, pH, and collector dose 3, 4, and 5 l/min were investigated. As can
rate on the copper grade. be seen in figure 5(E), increasing the
Figure 4(A) shows that increasing the
aeration rate from 3 to 4 l/min decreased the
mixing speed has not sensitive effect on the
copper grade. Also figure 4(B) shows that copper grade and increasing this parameter
grade of the copper decreased as the solid from level 2 to 3 was insensitive.
927
Based on what figure 5(F) indicates; time Where:

has negligible effect on the grade of copper. εȈ
p 2
j=1(yj-ym) (3)
This is due to entrance of some locked
particles (valuable and gangue minerals And
together) into the concentrate, thus the grade SST: Total sum of squared deviations
of copper decreases. about the mean
Figure 5(G) shows that the grade of Ȗj: Mean response for jth experiment
copper increased while increasing the Ȗm: Grand mean of the response
particle size. It is probably because of fine p: Number of experiments in the
particles which reduce the grade. orthogonal array
Figure 5(H) indicates that increasing the SSF: Sum of squared deviations due to
activator addition rate up to 200 g/t each factor
SSe: Sum of squares deviations due to
error
In addition, the F test was used to determine
which parameters have a significant effect
on the performance characteristic. Usually,
the change of the parameter has a significant
effect on the performance characteristic
when the F value is large (Esme et al.,
2009).
3.1.3.1 ANOVA for copper sulfides recovery

According to table 3, F-value for pH factor
is greater than extracted F-value from the
table (5.79) at 95% confidence level and for
df=2. Therefore variation of this parameter
has significant role on the copper recovery.
decreased the copper grade.
In other words, variations of pH could
change the recovery of copper in a
Figure 5. The effect of aeration rate, time, meaningful manner in this set of
particle size, and activator addition rate on experiments. In this table the term of particle
the copper grade size is pooled.
Also other parameters such as time,
3.1.3 Analysis of variance activator addition rate, and solid percent
have important role on the copper recovery.
The purpose of the analysis of variance
(ANOVA) is to investigate which
parameters significantly affect the 3.1.3.2 ANOVA for copper sulfides grade
performance characteristic. This is Table 4 shows the analysis of variance for
accomplished by separating the total copper grade. Normally, the larger F-value
variability of the grey relational grades, means that this factor has greater influence
which is measured by the sum of the squared on the recovery. Besides, the P-value is
deviations from the total mean of the grey another indicator. Values of less than 0.0500
relational grade, into contributions by each shows the model terms are significant.
welding parameters and the error. Thus; According to Table 4, F-value for solid
ε ή (2) percent factor is greater than extracted
F-value from the table at 95% confidence
928
level for df=1 (F=10.1) and also F-value for parameters have significant role on the
pH factor is greater than extracted F-value performance of the process. Besides, P-
from the table at 95% confidence level for Value confirms this finding.
df=2 (F=9.55). Therefore, variation of these
Table 3. Analysis of variance for copper recovery
Source Sum of DF Mean F p-value

Squares Square Value
Mixing speed 70.34 1 70.34 1.86 0.2311
Solid percent 116.05 1 116.05 3.06 0.1404
pH 2165.5 2 1082.76 28.59 0.0018
Collector dose rate 137.69 2 68.84 1.82 0.2551
Aeration rate 56.77 2 28.39 0.75 0.5191
Time 403.20 2 201.60 5.32 0.0577
Particle size - - pooled - -
Activator rate 258.32 2 129.16 3.41 0.1164
Residual 189.35 5 37.87 - -
Total 3397.2 17 - - -
3
Table 4. Analysis of variance for copper grade
Source Sum of DF Mean F p-value

Squares Square Value
Mixing speed 0.05 1 0.05 0.05 0.8368
Solid percent 19.80 1 19.80 22.18 0.0181
pH 83.08 2 41.54 46.53 0.0055
Collector dose rate 9.13 2 4.56 5.11 0.1081
Aeration rate 1.09 2 0.55 0.61 0.5987
Time 2.96 2 1.48 1.66 0.3272
Particle size 14.47 2 7.23 8.10 0.0617
Activator rate 4.40 2 2.20 2.46 0.2329
Residual 2.68 3 0.89 - -
Total 137.65 17 - - -
3.1.4 Optimum conditions of copper versus the experimental values for grade and
sulfides flotation recovery of copper respectively.
Finally, using these findings about
influential parameters on the process,
optimum working conditions could be
predicted. The proposed optimum conditions
were as: pH of 11, collector dose rate: 300
gr/t, activator addition rate: 100 gr/t, time: 7
min, aeration rate: 3 l/min, solid percent:
SDUWLFOH VL]H ȝP DQG PL[LQJ
a b
speed 1000 rpm. The predicted recovery and
grade for copper were 69.11% and 15.42%
respectively using DX7 software. Figures
6(a) and 6(b) show the predicted values Figure 6. Linear correlation between actual
and predicted values of copper grade (a) and
recovery (b)
929
As can be seen, the correlation between copper ore enters the conditioning stage.
actual values and predicted ones is After preparation, the feed go to the
satisfactory. flotation stage; and at the end of cleaner and
To investigate the accessibility of this recleaner stages, copper sulfides would be
result, a test with optimum conditions was extracted as concentrate of flotation process.
done. The experimental recovery and grade By acid leaching of the flotation tailing,
were 68.36% and 14.92% respectively at copper oxides would be achieved including
rougher stage. 441.2 ppm of Cu in filtrate and recovery of
98.69%. So total copper recovery will be
72.86%.
3.2 Copper Oxides Recovery Using Acid
The iron scrap would be added to the
Leaching of the Flotation Tailing
filtrate of leaching stage and finally during
A maximum recovery of copper during the the circle, the copper is being cemented. The
leaching tests of chodarchaie copper oxide copper content of the product will be more
ore was obtained in following condition: pH than 90%.
of 1, solid/liquid ratio: 1/8, temperature:
25°C and leaching time: 30 min 4 CONCLUSIONS
(Moradkhani et al., 2011). Tailing of the
optimum flotation test was dried, In this study, the effect of operating
homogenized, and leached under optimum conditions of flotation process was studied
leaching condition. 441.2 ppm of Cu with the Taguchi method using an L18 (22 ×
obtained from leaching test and copper 36) orthogonal array. As a result, the
oxides recovery was 98.69% during the ultimate optimum conditions were found to
leaching test. be: pH: 11, collector dose rate: 300 gr/t,
Thus total recovery of Cu could calculate activator addition rate: 100 gr/t, time: 7 min,
as equation (4). aeration rate on: 3 l/min, solid percent: 10%,
SDUWLFOH VL]H ȝP DQG PL[LQJ VSHHG
εȋͷή͸Ȍ (4) 1000 rpm. Under these conditions, copper
Where: sulfides were floated and recovery and grade
RT : Total recovery of copper after the of Cu were 68.36% and 14.92% respectively
flotation and leaching process at rougher stage. The most effective
a : Percent of copper sulfides (85.16%) parameter of flotation for maximum
b : Percent of copper oxides (14.84%) recovery of copper sulfides was found to be
R1 : Recovery of the copper sulfides as: pH and the most effective parameters for
during the flotation test maximum grade of copper sulfides were
R2 : Recovery of the copper oxides during found to be as: pH and solid percent. Tailing
the leaching test of the optimum flotation test was leached
under optimum leaching condition (pH: 1,
Finally, total copper recovery at 72.86% solid/liquid ratio: 1/8, temperature: 25°C
was obtained by using flotation-leaching and leaching time: 30 min). 441.2 ppm of
process. Cu obtained from leaching test and copper
oxides recovery was 98.69% during the
3.3 Working Diagram leaching test. The total copper recovery at
72.86% was obtained by using flotation-
The proposed process flowchart is shown in leaching process under optimum conditions.
figure 7. According to the diagram, the
crushed and homogenized sulfide oxide
930
Copper Sulfide Oxide

Ore
Conditioning
Flotation
(Raugher)
T Flotation
C (Cleaner & Recleaner) C
T
Sulfuric Acid
Copper Sulfide
Concentration Acid Leaching
Iron Scrap
Liquid
Cementation Solid
Dispose
Copper
Solid
(G=90%) Liquid
Figure 7. Flowchart of flotation-leaching cementation process
for leaching of malachite ore in H2SO4 solutions,

Chemical Engineering & Technology 24 (4), 409-
ACKNOWLEDGEMENTS 413.
The authors are grateful to the Research and Aydin, I., Aydin, F., Ziyadanogullari, R., 2005.
Enrichment of U, Mo, V, Ni and Ti from
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10.
Barlett, R.W., 1992. Solution mining, leaching and
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Arslan, C. and Arslan, F.,2002. Recovery of copper, tig welding process using grey relation analysis
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characteristics. Chem. Eng. Sci. 53 (4), 603- 615. 2008. Beneficiation of Egyptian Abu-Swayel
Gorain, B.K., Franzidis, J.P., Manlaig, E.V., 1995. copper ore by flotation. Physicochemical
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574-580. 234.
Lee, K., Archibald, D., McLean, J. and Reuter, Ziyadanogullari, R., Aydin, F., 2005. A New
M.A., 2009. Flotation of mixed copper oxide and Application For Flotation Of Oxidized Copper
sulphide minerals with xanthate and hydroxamate Ore. Journal of Minerals & Materials
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932
Quantum Chemical Representation of Antimonite Minerals and

Innovate Technology of Processing Complex Antimony Ores
P. M. Solozhenkin
Federal State Budget Establishment Research Institute of Comprehensive Exploitation of
Mineral Resources Russia Academy of Sciences ( IPCON RASc.) Kryukovsky Tupik, 4,
Moscow, 111020, Russia;
V. P. Nebera
Russian State Geological Prospecting University. Micluho-Maklaya. 23, Moscow 117997,
Russia.
Abstract The electronic level for individual atoms of prototype minerals were studied as well
as their reaction ability at interaction with reagent collectors in liquid phase. The ChemBio 3D
program of specialized complex ChemOfice Cambridge Soft Corp, MOPAC 2012. The most
wide spread prototypes of antimony sulfide minerals and its oxide minerals were studied.
Using certain equations of their rigidities, electronegativenes and charge transitions the
selectivity indices were calculated. The charges of separate atoms of minerals, as well as
sulfhydrilic collectors were estimated. The molecular models were shown and general steric
energy of mineral for attachment of butyl xanthate to individual atoms of antimonite,
gudmuntite and activated antimonite by the cations of lead and copper. The mechanism of
fastening of row sulfhydrilic collectors to minerals was analyzed. There were calculated
molecular orbitals and their levels.
The indices for selection of collectors at flotation of antimonite and gold-antimonite ores are
suggested.
Keywords: reagents for flotation, antimony minerals, molecular models, computer modelling
1 INTRODUCTION collectors reagents (before reagents were

synthesing and their properties estimated).
The flotation research is demanding That is important at flotation of
stereochemical representation of reagents antimonite ores because no computer
molecules at mineral surfaces attachments modeling for them were provided.
as well as effect of chemical activity of the
compounds. The importance of computer 2 MATERIALS AND METHODS
technologies and chemical programming
are productive at the research. For computer modeling of minerals
The quantum-mechanical research is prototypes the program ChemBio 3D from
reliable at the geometrycal presentation of ChemOffice of Cambridge Soft corp., as
molecules, as well as structural presentation well as program ɆɈɊȺɋ 2012 was
of compounds. The importance of applied. As a result, the basic computer
Quantitative Structure-Property parameters, and levels of moleculars
Relationship (QSPR) in calculation of the orbitals were estimated (higher occupied
reactivities indices of metals cations with molecular orbital HOMO and lower
unoccupied molecular orbital LUMO.
933
306ROR]KHQNLQ931HEHUD
Also, the particular charges of sulfhydryl a)

collectors and mineral prototypes were
estimated. For minerals and collectors were
also estimated the absolute rigidity and an
absolute electronegativity of internal
molecules and extend of charges transfer,
using principle rigidity-softness acids-
bases. Computers data were minimized by
MM2 program.
2.1 Quantum-Chemical Representation
of Antimonium Minerals.
The models of different minerals were
constructed, called as prototype minerals, b)
that reflect chemical formula, and the
distances between separate atoms correlate
with table data. The first data on prototype
antimonite and gudmuntite minerals and
their interaction with collectors and water
were published (Solozhenkin, 2012).
The molecular models of prototype
sulfide minerals kermesite Sb2S2O,
bertyerite FeSb2S4, Jemsonite Pb4FeSb6S14,
semseite PbSb8S21, bulanjerite Pb5Sb4S11,
gudmuntite FeSbS, as well as oxide
minerals valentinite Sb2O3, and
senarmontite Sb2O3, were studied.
Molecular models and molecular orbitals
were constructed, the energy levels were c)
calculated.
The structures of gudmuntite and
arsenopyrite were similar. In gudmuntite
the atoms of antimony could be substituted
by arsenic atom with forming arsenopyrite.
MO levels the same.
The different models of kermesite shown
on Figure 1
a)
Figure 1. The models of kermesite:

a- sferic roads model.
b – transparent – balls - rods
model in form of net with
border of interaction with water;
c- transparent model with border of
Van-der-Walls radius
934
The different models of bertyerite are electrophilic centers of sorption are cations
shown in Fig.2. of minerals.
a) Minerals have a negative magnitude of
HOMO and LOMO.
2.2 Quantum-Chemical Representation

of Antimonium Minerals Activation by
the Cations of Minerals.
The molecular models of prototypes of
antimony minerals with substitution of
atoms of antimony and sulfur by cations of
b) lead (copper) from known minerals,
containing antimony, were constructed.
The structure of antimonite Sb2S3 relate to
chain constructions as quaternary SbS-
groups in form of radicals Sb4S6 oriented
toward axis C. Therefore with the salts of
Pb, Cu and Ag could be formed combines
with Cu(I), Ag(I) , Pb(II) , Cu(II), Fe(II),
Ni(II), Co(II)(Solozhenkin,2007).
At Fig.3 are the molecular models with
different degree substitution of the atoms of
antimony and sulfur by the cations of Pb
(Cu) in combines of PbSb2S2, CuPbSbS3,
PbSb2S4, Pb2Sb2S5, and Pb3Sb2S6.
Figure 2. The bertyerite models: a)
chemical formula; b) balls - rods bond
model
Computer parameters of bertyerite:

Iteration 42; Stretch valency connections
0,7430; The bend of valency angle;
49,8625; Stretch-
bend corrections -1,5639; intrinsic torsion
0.0000; non 1,4 VDW interaction 3,1751;
1,4 VDW -03557; total energy 51,8611
kcal/mol.
The iron atom addition in bertyerite

structure resulted in increasing Total
Energy to 51.8611 cal/mole as compare to
kermesite 0.3670 kcal/mol.
Calculated computer parameters of
minerals were estimated: absolute rigidity
Ș eV, chemical potential up to Pirson and
Paru Ȥ, and the degry of charge WUDQVIHUǻ1.
Minerals have general characteristics of
absolute rigidity Ș =0,489÷6,391 eV.
Guantum-chemical representation state that
935
c)
a) b)
d)
e)
Figure 3. The molecular models with different degrees of replacement of the atoms of
antimony and sulfur by the cations of Pb (Cu) in combines; a- of PbSb2S2 ; b-CuPbSbS3; c-
PbSb2S4; d-Pb2Sb2S5; e-Pb3Sb2S6.
The cations of lead and copper could with forming combines of PbSb2S2 or
substitude the sulfur atom from antimonite (table1).
CuSb2S2. The lead (copper) cations miargilite, AgSbS2 aramayonite, Ag3SbS3
substituted two atoms of the antimony and pyrostilpnite and AgPbSbS3 freieslebenite.
sulfur with forming combines zincenite At activation of antimonite by silver cations
PbSb2S4 or CuSb2S4 could be substitutions in antimony radical
At activation of radicals Sb4S6 of Sb4S6 and forming combines andorite type
antimonite by cations of lead and copper it AgPbSb3S6
is possible substitutions and forming The iron cations displace from radicals
combines Pb2Sb2S5 and Cu2Sb2S5, or Sb4S6 two atoms of antimony and two
Pb3Sb2S6 ɢ Cu3Sb2S6 The cations of lead atoms of sulfur forming FeSb2S4 bertyerite
and copper could substituted the sulfur or Fe2Sb2S2 chain-like gudmuntite. The iron
atom from antimonite with forming cations displace antimony and sulfur atoms
PbSb2S2 or CuSb2S2 which not found in the from Sb2S3 forming FeSbS plain
nature. Silver cations (different quantity) gudmuntite. The charges of separate atoms
displace atoms of antimony and sulfur in in these compounds with MOPAC 2012
antimonite forming combines AgSbS2 program (table1).
936
Table 1. The charges of separate atoms combines
CuPbSbS3 PbSb2S4
Pb2Sb2S5 Cu2Sb2S5 Pb3Sb2S6 Cu3Sb2S6
(burnotite) (zinkenite)
S -0,7145 S -0,1995 S -0,2497 S -0,4486 Cu 0,5691 Pb0,9614
Sb 0,7145 Sb 0,5496 Sb 0,2132 Sb 0,3035 S -0,7089 S -0,6579
S -0,5595 S -0,2292 Pb 0,4231 Cu 0,5495 Sb 0,6117 Sb 0,5883
Sb 0,7142 Sb 0,5069 S -0,5958 S -0,3146 S -0,4849 S -0,4111
S -0,7148 S -0,5848 Pb 0,5156 Cu 0,4315 Pb 0,7016 S - 0,6581
S -0,7262 S -0,6236 S -0,5907 S -0,4304 S -0,6886 S -0,4112
Pb 1,0054 Cu 0,5688 Pb 0,7208 Cu 0,4652
Pb 1,0057 Cu 0,5794 S -0,2858 S -0,3620
S- 0,3731 S- 0,2989
Sb 0,6770 Sb 0,7264
S -0,4546 S -0,6216
Heat Heat Heat Heat Heat
Heat forming
forming forming forming forming forming
481,58243
-66,29983 -0,48387 666,48117 21ɛ 120,56877
Energy
Energy Energy Energy Energy
Energy
- - - -
-3333,91485ɷ -
1316,91550ɷ 2485,22537ɷ 1578,55667ɷ ɷ
1045,79531
Dipole Dipole Dipole Dipole Dipole Dipole
3,53245 4,25038 12,04004 11,98605 15,69869 13,08659
HOMO HOMO HOMO Į6202/802 HOMO HOMO
-8,480 -8,178 -6,692 -6,870;1,723 -8,157 -8,906
LUMO LUMO LUMO 6202/802 LUMO LUMO
-1,995 -2,593 -2,523 -7,618;1,331 -1,497 -2,500
Using these data possible to say, that from The charges at lead atoms are higher,
all constructed combines the most probable that on copper atoms. This explains using
forming on the surface of the prototype the salts of lead as activators of antimony
antimonite PbSb2S4 (zinkenite) and minerals than copper salts.
CuPbSbS3 (burnotite). These combines will The heat of forming for Pb3Sb2S6 and
be used at analyses of flotation process. Cu3Sb2S6 are high and their forming on the
surface have low probability.
There was estimated, that for zinkenite The computer parameters for antimonite,
general energy PbSb2S4 is -0.5996 activated by lead, Sb2Pb3S6: iteration 161,
kcal/mole and for burnotite. CuPbSbS3 - Stretch 0.0006; Bend 0.0547; Stretch-Bend
0.3856 kcal/mol. General energy for -0.0015; torsion 0.0000; Non-1,4 VDW
Pb2Sb2S5 is 21.9174 kcal/mol and total interaction -0.3284; 1,4 VDW -0.9291;
energy for Cu2Sb2S5 is 17.2149 kcal/mol. Total energy -1.2037 kcal/mol.
937
The computer parameters for lead by lead Pb3Sb2S6 were created, and their
activated antimonite Sb2Cu3S6: iteration parameters calculated.
161; Stretch 0.0006; Bend 0.0547; Stretch- The sketch of combines butyl xantogen
Bend --0.0015; torsion 0.0000; Non-1,4 acid with antimonite (spheric-rod model)
VDW interaction --0.3157; 1,4 VDW k- preactivated by copper Cu3Sb2S6 was
0.4984; Total energy -0.4979 kcal/mol. created and their parameters calculated
The general energy for copper activated The general energy for combine of
antimonite higher -0.4979 kcal/mol than for activated by lead antimonite and attached
lead activated antimonite -1.2037. butyl xantogenate acid lower (1.3314
Antimonite will react with lead cations. kcal/mol) than for the combine with
activated by copper antimonite and butyl
2.3 The Creation Combines of Collectors xantogenate (2.2566 kcal/mol) e.i. the
with Sulfide Minerals of Antimony. optimal structure of the combine was
reached at lower energy.
The authors consider that interaction of There was suggested
collectors with mineral surface could be diethylaminxantogenate
presented as complex combine of the (C2H5)2NCH2CH2OCSSNa–ȾEȺminɄɯ) as
mineral prototype and mineral bonding to a selective reagent for separation of
atom of metal (Solozhenkin, Solozhenkin, antimonite from arsenopyrite at activation
Krausz, 2012). Only for such created of antimony sulfide by high doses of the
combine could be reserved the basic lead nitrate (750-1000 g/t) with following
computer parameters and estimate flotation in low acid medium ( pH 5.5-6)
properties of the structure.The general At antimonite flotation from arsenate ores
energy for combine of activated by lead elective is sodium dibythylamin
antimonite and attached butyl xantogenate dithiophosphate (C4H9NH)2PS2Na. The
(1.3314 kcal/mol) lower than for combine collectors were attached to PbSb2S4
could be received the computer parameters zinkenite and chalkostibnite CuSbS2. At
and estimate properties of combine Fig. 4 is combine of ethylaminxantogen
structure. acid with PbSb2S4 zinkenite (its ball-rod
The combines of butyl xantogen acid and model) and their parameters (table 2).
antimonite (its ball-rod model) preactivated
b)
a)
Figure 4. The scheme of combine ethylamine xantogene acid with PbSb2S4 zinkenite: a)
initial chemical formulae; b) ball-rod model
938
At Fig 5 is the combine of The parameters of complex combines of

dibuthylamindithiophosphate acid with antimony minerals and collectors at Table
PbSb2S4 zinkenite (its ball-rod model) and 2.
their parameters (table 2).
a)
b)
Figure 5. The scheme of the combine of dibuthylamindithiophosphate acid with PbSb2S4

zinkenite (its ball-rod model): a) initial chemical formulae and their parameters b) ball-rod
model).
939
Table 2. The parameters of complex combines of antimony minerals and collectors

Complex combines of antimony minerals and collectors
0.8378
Stretch 0.8459 0.4303 1.0792
Bend 2.6443 2.4189 2.2128 52.2695

Stretch-Bend 0.2345 0.2504 0.1394 -0.6135
Torsion 0.1802 0.1750 -0.0512 -0.2544
-4.4945
Non-1, 4 VDW -8.4533 -8.1305 -7.3389
Parameters
1, 4 VDW 5.6953 6.5153 4.2134 8.8309
Dipole/dipole 2.4621 2.5067 -0.3242 -0.8548
Total Energy ,
3.6089 8.2097 -1.5100 53.1181
kcal/mol
Sb2PbS4
SbCuS2 Sb2PbS4 SbCuS2
+
+ DȾEȺmineɄɯ + +
DEȺmineɄɯ
DButyilȺmine '%XWLOȺPLQH
Iteration 301 Phosphate Phosphate
Iteration 424
Iteration 286 Iteration 826
General steric energy for combines with 2.4.1 Processing of gold-antimony ores of
activation by lead cation lower (3.6089; - Sarylah and Sentachan on the Sarylah
1.5100 kcal/ mol ) than with combines with plant.
copper activated prototypes minerals of
antimony. The practice of the processing and
Conclusion: Lead activators are preferable. innovation are presented in detail
(Solozhenkin,2006; Baltuhaev and
2.4 Innovate technologies for processing Solozhenkin 2009 a, 2009 b). High
antimony minerals flotation gold- recovery of both metals reached
antimony ores (Salomatova 2007; Matveev, Salomatova,
2008; Solozhenkin at. al.
The basic resourses for production of 2008;Solozhenkin,2008).
antimony in Russia is naw in republic Saha Some of processing data are below:
(Amusinsky at.al. ,2001, Komin,
Klyucharev, Volkova ,2006) that
comparable with production of Bolivian,
Un. S. Afr., Thailand, Mexico, Malaysia,
Italy, USA. Could be mentioned, that
medium contents of antimony in above
countries is 2-5% in Saha ores it is 20-25%.
Almost all prospected Saha ores (95%) are
counted by two deposits – Sarylah and
Sentachan. Antimonite is a main ore
mineral of both deposites.
940
(Solozhenkin, Bondarenko, Chertogova,

Sarylahskoye Sentachanskoye 2008). There was found:
deposit deposit The higher contents of antimony in ore
the better concentrate received;
Ore contents Sb, Sb, % 28,7 The higher the limit of the separation
the better concentrate received;
% 16,73; 13,2 Au, g/t 42,2
From the ore with the content of Sb
Au, Sb, % 58, 9 1% there was received concentrate 4,1 %
g/t 7,4; 4,7 Au, g/t 68,6 Sb. The recovery was high - 95-98%.
Concentrate Sb, % Sb, % 92, 1 Radiometric sorting is recommended
63, 01; 60 Au, 71,5% The authors have shown selectivity of
cjntent Au, new reagents "Oxafor-43" and "Pemisol.
g/t 12, 8; 13,4 The simple technological circuit without
Conc.Recovery. Sb, special depressors of arsenic minerals
% 91, 6 ;90 (Abdusalyamova at. el., 2012).
Au,
85,7-86% 2.5 The hydrometallurgy
2.5.1 Processing of lead- antimony
The results are highest in the world on Au- concentrates by the pulp electrolyses.
Sb ores.
There were recommended a number of This is a new process of hydrometallurgy
selective reagents. As an activating reagent developed in last 20 years. It unites three
is investigated hydrazine N2H2 1/2 H2SO4. parts of known processes of leaching,
The insignificant addition of hydrazine (8 solution cleaning and electrical settling
g/t) positively affects flotation, reducing (Solozhenkin, 2010: Solozhenkin, 2012).
losses of antimony by 0.4%, of gold by 6.6 New industry use only sulfide-alkali
%; the charge of the collector reduced by leaching of antimony concentrates
30 %. The sodium dimethyldithiocarbamate (Solozhenkin, 2006).
was studied as a collector for But acid processes have many
antimonite.The synergism of mixture of advantages for complex gold-antimony
dimethyldithiocarbamate with xantogenate. ores.
(Solozhenkin at.al. 1993). Hydrometallurgical processing could
The most perspective area of mineral produce the antimony three oxide and
base of Russia is East Transbaikalia antimony directly from concentrates
(Transbaikalian territory). In territory of without pyrometallurgical treatment and
East Transbaikalia is known more than 200 emanation of the sulfur dioxide in
exposes of antimony and mercury- atmosphere.
antimonies mineralization. Gold antimonial
deposits, including Solonechenskoye and 2.5.2 Innovate technologies for processing
Zhipkoshinskoye, with the average contents gold-antimony concentrates
of antimony from 4.5 up to 18%, and
industrially important by the contents of The authors applied as an antimonite
gold. solvent solutions Feɋ13, SbCl5,
tetrafluorineboron acid HBF4 to realization
2.4.2 Processing of antimony ores of of reaction under the circuit:
Zhipkoshinskoye deposit (Transbaikalia 2Sb2S3 +6MeA3 =2SbA3 +6MeA2 +3S,
territory). (1)
Where A- Cl, F, Br, I, HBF4; Me-Fe.
For low grade ore there was applied
roentgen radiometric separation
941
The method of ferrochloride leaching of The above listed process is innovating in

gold - antimony concentrates includes comparison to classical antimonite leaching
leaching by a acidic solution of iron process by sulfide-alkaline solutions.
chloride, separation from pulp sulfur and
cake, containing noble metals, an CONCLUSIONS
electrolytic sedimentation of antimony from 1. The modeling of the prototypes antimony
solution. An electrolyte is going back on minerals Studied. Computer parameters of
repeated leaching. minerals and charges of the separate
Use of antimony pentachloride solution minerals, the distances between atoms.
more effective, than FeCl3, as it excluded 2. The method of attachment for the
pollution of antimony trioxide by ions of different sulfhydryl collectors to the
iron because of hydrolyses reaction. separate atoms of prototype minerals was
Sb2S3 +3SbCl5 = 5SbCl3 + 3S; (2) elaborated.
3. There was shown that lead salts are
Sb2S3 +3HSbCl6 = 5SbCl3 + 3S+HCl (3) preferable as activators for antimony
sulfides several new reagents were
suggested as collectors for flotation of
The inventors -Olper, Marco - offered antimony ores.
derivative tetra fluorine boron acid HBF4 4 The prospect was shown for the acid
for extraction of antimony from sulfide ores leaching concentrates with use as the
after alkaline leaching, extraction of solvents antimony sulfide SbCl5 and Fe
elementary sulfur and electrowinning of (BF4)3, receiving high-quality antimony
antimony from fluorine borate solutions. trioxide and metallic antimony.
Extraction of element sulfur and electro
sedimentation of antimony from
tetrafluorineboron solutions are offered REFERENCES
derivative fluorineboron acid HBF4 for Amuzinsky V.A., Anisimova G.S., Zhdanov Yu.
extraction of antimony from sulfides ores Ya. at al. 2001, Sarilakhskoye and
after sulfide - alkaline leaching. Sentachnskoye gold-antimony deposites:
Geology, mineralogy and geochemistry.
Sb2S3 + 2 NaOH = NaSbS2 + NaSbSO + Moscow, MAIK Science/interperiodical., 218
H2O (4) p.p.
NaSbS2 + NaSbSO + H2SO4 = Sb2S3 + Abdusalyamova M.N, Dreisinger David,
Na2SO4 + H2O (5) Zinchenko Z.A, Solozhenkin P.M.,. Gadoev
S.A, Tyumin T.A and M.S. Ismailova. 2012.
The leaching of antimony from Processing of Mercury-Stibium Gold Bearing
Sb2S3 by iron (III) fluorineborate is carried Ores of Djijikrut Deposit. Books of Abstracts.
out on reaction: XXVI International Mineral Processing
Sb2S3 + 6 Fe (BF4)3 = 2 Sb (BF4)3 + Congress-
6Fe(BF4)2 + 3S. (6) IMPC-2012. New Delhi, India, September 24-
28, 2012 , volume 2, p.528.
Boltukhaev G.I., Solozhenkin P.M. 2009a .The
Electrolyses of the filtered solutions in processing of large size samples of antimony
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949
950
Investigation of the Beneficiation of Low Grade Manganese Ores

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ABSTRACT In this study, beneficiation of low grade manganese ores was investigated by
applying high intensity dry magnetic separation, MGS (Multi Gravity Separator) and flotation
methods. Manganese grades of the ores were 25.65% Mn and 13.96% Mn taken from Antalya
and Kayseri regions, respectively. Flotation and magnetic separation recoveries of both tested
samples were low and the grades of the concentrates were less than 45% Mn. Similar results
were also observed using a lab-type MGS but a concentrate could be obtained with 41.24%
Mn and 78.71% recovery for manganese ores taken from Antalya region.
Keywords: Manganese, Flotation, Magnetic Separation, MGS
ÖZET %X oDOÕúPDGD GúN WHQ|UO PDQJDQH] Fevherlerinin \NVHN DODQ úLGGHWOL NXUX
PDQ\HWLND\ÕUPDMGS ve flotasyon \|QWHPOHULX\JXODQDUDN]HQJLQOHúWLUilPHVLDUDúWÕUÕOPÕúWÕU
AntaO\D E|OJHVLQGHQ DOÕQDQ QXPXQH %25,65 Mn .D\VHUL E|OJHVLQGHQ DOÕQDQ QXPXQH ise
%13,96 Mn içermektedir. Flotasyon ve manyHWLN D\ÕUPD WHVWOHULQGH KHU LNL E|OJHGHQ DOÕQDQ
numunenin YHULPOHUL ROGXNoD GúN ROPXú YH HOGH HGLOHQ NRQVDQWUHOHULQ WHQ|UOHUL %45 Mn
GH÷HULQGHQGDKDD]GÕU $\QÕúHNLOGHODERUDWXYDUWLSL0*6NXOODQÕOGÕ÷ÕQGDGDEHQ]HUVRQXoODU
HOGH HGLOPLú DQFDN $QWDO\D E|OJHVLQGHQ DOÕQDQ PDQJDQH] FHYKHUOHULQGHQ YHULP YH
0QLoHUHQELUNRQVDQWUHHOGHHGLOHELOPLúWLU
Anahtar kelimeler: 0DQJDQH])ORWDV\RQ0DQ\HWLN$\ÕUPD0*6
1 INTRODUCTION
The world rapidly growing demand for applications of manganese include battery
manganese has made it increasingly cathodes (manganese dioxide), soft ferrites
important to develop processes for economic (manganese-]LQFIHUULWHVXVHGLQHOHFWURQLFV
recovery of manganese from low grade PLFURQXWULHQWVIRXQGLQIHUWLOL]HUVDQGDQimal
manganese ores and other secondary sources feed (manganese sulphate and manganous
(Zhang and Cheng, 2007). In the oxide), a water treatment chemical
metallurgical industry, manganese is used as (potassium permanganate), a colorant for
DGHR[LGL]LQJDQGGHVXOIXUL]LQJDJHQWDQGDV bricks and ceramics, and others (Corathers
an alloying element in certain steel, copper and Machamer, 2006).
and aluminum alloys. Non-metallurgical
951
2%D\DW0$OWÕQHU67RS
Manganese mineralization in Turkey is MGS (Multi Gravity Separator) consists of

divided into four main groups according to a slightly tapered open ended drum that
their age spans, hostjocks, processes of rotates in a clockwise direction and shakes
formation and mineralogical-chemical- sinusoidal in an axial direction. Inside the
textural features. The first is hydrothermal drum is a scraper assembly which rotates in
and rare hydrogenetic type manganese the same direction as the drum but at a
mineralization which is associated with slightly faster speed (Figure 1).
chiefly radiolarian chart series. The second is Feed slurry is introduced continuously
black shale hosted manganese mineralization midway onto the internal surface of the drum
that takes place in the black shale horizon via an accelerator ring cleaner. Wash water is
within the carbonates of Lower Cretaceous added via a similar launder positioned near
age in Western Taurides. These deposits are the open end of the drum. As a result of the
represented by relatively large reserves and high centrifugal forces and the added
are composed of rhodochrosite and its shearing effect of the sinusoidal shaking, the
oxidizing products. The third is volcanic arc dense particles migrate through the slurry
hosted ores along the Black Sea coast occur film to form a semisolid layer against the
in different types of metasomatic, wall of the drum. This dense layer is
hydrothermal and stratabaund settings. The conveyed by the scrapers towards the open
fourth is the post-tectonic sedimentary end of the drum where it discharges into the
hosted ores in the Thrace Basin (Öztürk, concentrate cleaner. The less dense minerals
1997). are carried by the flow of wash water
Generally, manganese deposits positioned downstream to the rear of the drum to
in Turkey have low grades and small discharge via slots into the tailings cleaner.
reserves. These reserves are approximately Wash water flow rate, vibrational
4.5 million tons. The largest manganese amplitude, vibrational frequency, tilt angle
reserves of Turkey are located in Denizli- and drum rotational speed are critical
Tavas-Ulukent ore beds with 4 million tons. variables which affect concentrate grade and
In Turkey, demands for manganese ores recovery (ÖzbayR÷OXDQG$WDOD\
result from iron and steel plants such as
Kardemir, Isdemir and Erdemir corporations.
Shake
Feed slurry
Scraper Bars (4)
Washwater
Scrapers (34)
Figure 1. Pilot Scale MGS (Wills and Napier-0XQQ
952
When manganese ores have been floated, Table 1. Chemical Composition of Kayseri
fatty acids have been used as collector Manganese Ores
(McCarroll, 1954; Kurova, 1970; Goldberg Element % Element %
et al., 1986a; Kharlamov et al., 1966;
Fahrenwald, 1957). Al 0.660 O 43.936
Manganese flotation with anionic
collectors decreases in the order: manganite, As 0.006 P 0.323
pyrolusite, and psilomelane. Ba 0.295 S 0.068
This order was observed for both oleic
acid and tridecylic acid and was explained by Ca 1.306 Si 24.193
Goldberg et al. (1968) to be established by
Cr 0.009 Sr 0.053
the corresponding order of increase in
surface hydration energies (Goldberg et al., Fe 14.460 Ti 0.029
1968a, 1968b, 1969; Kharlamov et al., 1966;
K 0.274 Y 0.003
Kharlamov and Kirnosov, 1966; Fuerstenau
et al., 1986). Mg 0.409 Zn 0.004
Some manganese flotation studies were
performed by using sodium oleate as Mn 13.960 Zr 0.013
collector (Yamaguchi, 1932; Acevedo, 1977;
Song, 1994; Andrade, 2010; Andrade et al.,
2012). Table 2. Chemical Composition of Antalya
In this study, dry magnetic separation, Manganese Ores
MGS and flotation methods were applied in
order to recovery manganese from low-grade Element % Element %
ores. Al 0.495 Mo 0.016
2 MATERIAL AND METHOD Ba 0.329 Ni 0.014
2.1 Materials Ca 0.064 O 45.925
The feed samples for this study were taken Cl 0.027 P 0.092
from Antalya and Kayseri regions. A Philips
model PW2404 WDXRF spectrometer was Co 0.006 Pb 0.008
used for the determination of the chemical
composition of both samples as seen in Cr 0.065 S 0.067
Tables 1-2.
Mineralogy of the samples was Cu 0.027 Si 26.141
determined using a Shimadzu XRD-6000 Fe 0.667 Sr 0.017
analyzer applying Cu x-UD\ WXEH Ȝ
Angstrom). K 0.253 Ti 0.010
As seen from Figures 2-3, the manganese
ore taken from Kayseri region consists of Mg 0.083 V 0.023
quartz, hematite, goethite, todorokite, Mn 25.651 Zn 0.010
manganese (II) oxide (MnO) and tricalcium
aluminate while the sample taken from
Antalya region mainly consists of quartz,
manganite and pyrolusite.
953
2%D\DW0$OWÕQHU67RS
G = Goethite
M = Manganite
H = Hematite
Q = Quartz
Figure 2. XRD Pattern of Kayseri Manganese Ores
P = Pyrolusite
Q = Quartz
M = Manganite
Figure 3. XRD Pattern of Antalya Manganes Ores
954
2.2 Methods In the tests, three different sized samples

(-2.8+1 mm), (-1+0.5 mm) and (-0.5+0.150
Magnetic separation experiments were mm) were prepared and used from Kayseri
conducted using a high intensity dry samples. Also, magnetic field strength was
magnetic separator (PERMROLL) at the chosen as 1.7 Tesla.
Department of Mining Engineering of Each test was carried out by using
Istanbul Technical University. approximately 1.5 kg sample. Other working
conditions are given in Figure 4.
Feeding Feeding Feeding

(-2.8+1 mm) (-1+0.5 mm) (-0.5+0.150 mm)
Permroll Magnetic Permroll Magnetic Permroll Magnetic

Separator Separator Separator
Non
Front knife 100o Front knife 120o Front knife 120o 1st
Magnetics
Rear knife 70o Rear knife 120o Rear knife 120o Magnetics
Feeding Speed 120 rpm Feeding Speed 120 rpm Feeding Speed 120rpm
Moderate Magnetics
Permroll Magnetic Permroll Magnetic Permroll Magnetic

Separator Separator Separator 2nd
Front knife 100o Front knife 100o Front knife 120o Magnetics
Rear knife 85o Rear knife 110o Rear knife 120o
Feeding Speed 120 rpm Feeding Speed 120 rpm Feeding Speed 120 rpm
Moderate Magnetics
Figure 4. Flow Sheet of the Dry Magnetic Separation Tests

After the magnetic separation tests, tests, pulp density was set at %15 solids and
samples were sized below 0.106 mm by the pulp was fed into the MGS device
using a raw crusher and ceramic ball mill for through feeding pump as 2.6 L/min. After
both MGS and flotation tests. In spite of pulp was fed; in order to form separation
being detected degree of liberalization as layers in the walls of the drum, one minute
0.106 mm, removal of slimes was not was waited during all tests before sampling
was carried out. Afterwards, concentrated
applied to both of the methods in advance. If
and residual portions were taken from
removing slimes had been applied, the large concentrate and tailings section of MGS at
part of manganese would have stayed in intervals of 10 seconds. Finally, the samples
slime phase. Therefore, removal of slimes were dried, weighed and analyzed for Mn
was skipped in MGS and flotation tests. grade.
For MGS tests, carried out at the Approximately 300 grams samples were
Department of Mining Engineering of Dokuz used in the flotation tests. Flotation
Eylül University, optimum working experiments were carried out in a 2 L
conditions achieved from the preliminary flotation cell. Optimum flotation test
tests were 180 rpm drum speed, 4o incline conditions are seen in Figure 5. Both
rate and 2.2 L/min washing water. In these potassium oleate and sodium oleate were
955
2%D\DW0$OWÕQHU67RS
used as collector in order to improve the

performance of the flotation process.
Test Conditions Crushing + Grinding

Stirring speed: 1400 rpm
Pulp density: 15% solids
pH: 10
Kerosene + Diesel Oil:
Rougher Tailings
124 g/ton
Na2SiO3: 500 g/ton Flotation
Potassium Oleate: 150 g/ton
Sodium Oleate: 150 g/ton
10 min. conditioning and
12 min. flotation time
pH: 9
Potassium Oleate: 35 g/ton 1. Cleaning Middling 1
Sodium Oleate: 35 g/ton Flotation
pH: 9 2. Cleaning
Potassium Oleate: 35 g/ton Middling 2
Flotation
pH: 9 3. Cleaning Middling 3

Potassium Oleate: 35 g/ton Flotation
6 min. flotation time Concentrate
Figure 5. Flowsheet of the Flotation Tests

3 RESULTS
Results of the high intensity dry magnetic When the samples from Antalya region
separation tests are given in Table 3. were used for preliminary flotation tests, no
Although a concentrate with 35% Mn grade success was achieved at all. Therefore,
was recovered, desired yield could not be results of the flotation tests of the samples
obtained by high intensity dry magnetic taken from Kayseri region are only presented
separation tests. in this study (Table 5).
As a result of the MGS tests, manganese A concentrate with 27.14% Mn and
grade of the concentrate was 41.24% Mn and 44.64% recovery could be obtained after
recovery was 78.72% for Antalya sample three cleaning.
working at the optimum conditions. Nevertheless, increasing the further
However, both grades and recoveries of cleaning stages of the flotation was
the concentrate, 22.48% Mn and 28.02% unsuccessful since the grade of the
yield, from Kayseri region manganese ores concentrate was almost the same after the
were lower than Antalya samples. MGS test three stages of cleaning.
results are presented in Table 4.
956
Table 3. Results of High Intensity Dry Magnetic Separation Tests
Feeding (-2.8+1 mm)

Weight Fe2O3 Mn Mn Yield
Product
(%) (%) (%) (%)
1st Magnetic 12.5 16.16 35.00 61.64
2nd Magnetic 8.8 17.70 17.95 22.25
Middling 17.4 9.23 3.10 7.61
Non-Magnetic 61.3 5.08 0.98 8.50
Feed 100.0 8.29 7.10 100.00
Feeding (-1+0.5 mm)
Product
(%) (%) (%) (%)
1st Magnetic 11.0 17.13 34.93 30.19
2nd Magnetic 12.9 17.09 31.87 32.29
Middling 17.1 15.69 20.34 27.33
Non-Magnetic 59.0 5.70 2.20 10.19
Feed 100.0 10.13 12.73 100.00
Feeding (-0.5+0.150 mm)
Product
(%) (%) (%) (%)
1st Magnetic 5.6 17.12 29.92 13.37
2nd Magnetic 16.4 15.69 29.71 38.87
Middling 23.3 15.69 21.95 40.80
Non-Magnetic 54.7 5.70 1.59 6.96
Feed 100.0 10.30 12.53 100.00
Table 4. Results of the MGS Tests for Antalya and Kayseri Manganese Ores
Antalya Sample
Product
Weight (%) Mn (%) Yield (%)
Concentrate 48.96 41.24 78.72
Tailings 51.04 23.98 21.28
Feed 100.00 25.65 100.00
Kayseri Sample
Product
Weight (%) Mn (%) Yield (%)
Concentrate 17.40 22.48 28.02
Tailings 82.60 12.17 71.98
Feed 100.00 13.96 100.00
957
2%D\DW0$OWÕQHU67RS
Table 5. Flotation Test Results of Kayseri Manganese Ores
Product Weight (%) Mn (%) Yield (%)

Concentrate 22.96 27.14 44.64
Tailings 77.04 10.03 55.36
Feed 100.00 13.96 100.00
4 CONCLUSIONS Corathers, L. A. and Machamer, J. F., (Kogel, J. E.)

2006. Manganese, Industrial Minerals & Rocks:
Even though a concentrate with 35% Mn Commodities, Markets and Uses, pp. 631.
grade was obtained by dry magnetic Fuerstenau, M. C., Han K. N. and Miller, J. D.,
separation method, further studies should be (Somasundaran, P.), 1986. Flotation Behavior of
carried out for the optimization to obtain Chromium and Manganese Minerals, in Advances
marketable manganese product. in Mineral Processing, Chapter 17, SME Inc.,
Littleton, pp. 289.
Manganese beneficiation by using MGS Goldberg, Yu. S., Semioshko, V. M. and Uvarov,
was unsuccessful for Kayseri manganese V. S., 1968a. Obogashch. Polez. Iskop. No. 3,
samples but a concentrate with 41.24% Mn pp. 37.
and 78.72% yield could be recovered from Goldberg, Yu. S., Semioshko, V. M. and Uvarov, V.
Antalya manganese samples. S., 1968b. Obogashch. Polez. Iskop. No. 3, pp. 14.
Flotation experiments with Kayseri Kharlamov, V. S. and Kirnosov, E. G., 1966. Izv.
Vyssh. Ucheb. Zaved., Gorn. Zh., 9 (11), pp. 163.
samples resulted in low recovery yield. The Kharlamov, V. S., Kirnosov, E. G. and Makarov, V.
desired yield and concentrate could not be N., 1966. Dobycha, Obogashch. Pererab., No. 2,
obtained by flotation method since pp. 63.
manganese minerals were superbly coated Kurova, M. D., 1970. Obogashch. Rud., Vol. 14, No.
with slime sized impurities such as calcite, 2, pp. 12.
hematite, quartz etc. Therefore, flotation McCarroll, S. J., 1954. J. Min. Eng., Vol. 6, No. 3,
pp. 289.
reagents were not effective for flotation. Song, S., Lu, S., 1994. Hydrophobic Flocculation of
Also, Na2SiO3 used for depressing silicates Fine Hematite, Siderite and Rhodochrosite
did not show the expected depressing effect. Particles in Aqueous Solution, Journal of Colloid
and Interface Science, v. 166, Issue 1, pp. 73-80.
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958
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Investigation of the Usability of Oleic Acid as Extractant in
Copper Extraction from Aqueous Solutions
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ÖZET Hidrometalurjide solvent ekstraksiyonu liç çözeltilerinden metal kazanmak veya

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copper from sulphate solutions by LIX 864 in
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Sole, K.C., Hiskey, J.B., (1995). Solvent extraction
of copper by Cyanex 272, Cyanex 302 and
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S., Basri, M., Wan Yunus, W.M.Z., (2005).
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Chapter - H

FLOTATION & SURFACE CHEMISTRY

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Constrained Multivariable Control of a Pilot Flotation Column at

D.E.Calisaya, A.Riquelme, A.Desbiens, É.Poulin

ABSTRACT A 15 cm diameter by 732 cm height, fully automated pilot column was

1 INTRODUCTION concentrate cleaning, is simply not measured

Fraction of Wash Fraction of wash

Figure 1. Schematic diagram of advanced control of a flotation column

3 EXPERIMENTAL SET-UP & TESTS

3.1 Experimental Set-up

and contain two conductivity electrodes, prediction error minimization method

0 20 40 60 80 100 120 140

0 20 40 60 80 100 120 140

0 20 40 60 80 100 120 140

0 20 40 60 80 100 120 140

Minerals and Metallurgical Processing, Vol. 3,

Maldonado, M., Desbiens, A. Poulin, É., del Villar,

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Recovery of Lithium Rich Mica from Mineral Waste

Z. Iqbal, N. A. Rowson, S. Blackburn

1 INTRODUCTION Previous reports (J. R. Hawkes, 1987)

2 RESULTS AND DISCUSSION

Figure 5: Flotation recovery of Li2O, constant

Using froth flotation a 0.47% lithium

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Fractional Method of Sulfide Copper Ore Processing

1 INTRODUCTION We looked for solution of this problem in

2 MINERALOGICAL DESCRIPTION machine with variable flotation cell volume

Table 1. Flotation results by flow sheet on Figure 1

Table 2. Flotation results by flow sheet on Figure 2

Table 3. Flotation results by flow sheet on Figure 3

Table 4. Flotation results by flow sheet on Figure 6

Table 5. Flotation results by flow sheet on Figure 5

4 TRIAL RESULT ANALYSIS of copper minerals is extracted, though very

II concent f lotation 2 min

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Figure 1. Pilot Scale MGS (Wills and Napier-0XQQ