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Floatability study of graphite ore from southeast Sulawesi (Indonesia)

Fenfen Fenda Florena, Fahmi Syarifuddin, Eko Sulistio Hanam, Nici Trisko, Eko Kustiyanto, Enilisiana, Anton
Rianto, and Ghenadi Arinton

Citation: AIP Conference Proceedings 1712, 050005 (2016);


View online: https://doi.org/10.1063/1.4941888
View Table of Contents: http://aip.scitation.org/toc/apc/1712/1
Published by the American Institute of Physics

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Floatability Study of Graphite Ore from Southeast Sulawesi
(Indonesia)
Fenfen Fenda Florenaa), Fahmi Syarifuddin, Eko Sulistio Hanam, Nici Trisko,
Eko Kustiyanto, Enilisiana, Anton Rianto and Ghenadi Arinton

Research Laboratory of PT Grafit Geologi Konsultan,


Jl. Tebet Barat raya 31B, Jakarta Selatan 12810, Indonesia.
a)
Corresponding author: fenfen.fenda@gmail.com

Abstract. Graphite ore obtained from Kolaka Regency, South East Sulawesi, Indonesia have been succesfully
investigated for beneficiation by froth flotation technique. Preliminary study have been done to determine the minerals
types, fixed carbon content and liberation size of the graphite. Graphite is naturally floatable due to its hydrophobic
property. Some suitable reagents are usually added to increase effectiveness of recovery. In this article, enrichment of
graphite by froth flotation was studied by investigating the effect of reagents concentrations, rotation speed and particle
size on the carbon grade and recovery of the concentrate. The carbon grade increased from 3.00% to 60.00% at the
optimum flotation conditions.

INTRODUCTION
Graphite is one of three forms of naturally found crystalline carbon; the other two are charcoal and diamond.
Graphite generally occurs in one of three forms: microcrystalline or amorphous; crystalline lump or vein; and
crystalline flake [1, 2]. Graphite has a unique role in different industries due to its various physical and chemical
characteristics. Graphite decompose at 600ºC in oxidizing conditions and melt at 3550ºC in non-oxidizing
conditions and vapor at 4500ºC, and it has a greasy texture [2]. Graphite is used mainly for foundry facings,
refractories, lubricants, pencils, batteries, brake linings, bearings, conductive coatings and crucibles [3]. Graphite
can easily be enriched by flotation because of its high natural hydrophobicity. There are several reports in the
literature reporting the flotation of different graphite ores. Beneficiation of graphite includes gravity concentration
and froth flotation.
Froth flotation process is a commonly used method for the purification of minerals. In the flotation process,
reagents give an effective separation and concentration results. Reagents in mineral processing are therefore
inseparable part of the flotation process. In commercial plants, the control of reagent addision becomes the most
important part of the flotation strategy. Classification of the reagents is based on the function of a particular reagent.
Reagents are divided into collectors, frothers and modifiers [4]. The addition of collector is to selectively form a
hydrophobic layer on a given mineral surface in the flotation pulp and thus provide conditions for attachment of the
hydrophobic particles to air bubbles and recovery of desired particles in the froth product. Hydrocarbon oils as a
nonpolar collector can be added for attaching the graphite. Separation process of this mineral must be brought in
contact with air bubbles so the graphite floats with the bubbles and attached to the surface [5]. Flotation process
depends on several factors, such as mineralogy of the graphite ore, the addition of some reagents, the equipment of
flotation system, particle size of the mineral, pulp density and speed rotation of flotation system. The assessment of
the carbon content can be determined by a simple LOI (Loss on Ignition) technique. The LOI technique calculates
recovery and grade of the carbon content. The aim of this study was to investigate the enrichment of graphite ore by
froth flotation.

2nd Padjadjaran International Physics Symposium 2015 (PIPS-2015)


AIP Conf. Proc. 1712, 050005-1–050005-6; doi: 10.1063/1.4941888
© 2016 AIP Publishing LLC 978-0-7354-1359-7/$30.00

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MATERIAL AND METHODS

Regional Geology and Material


Recently, graphite mineral resources have been found in several areas of Indonesia. In this study, graphite ores
were obtained from Mekongga region in the concession of PT Mekongga Sejahtera located in Tamboli, Samaturu
District, Kolaka Regency, Southeast Sulawesi. The region is shown in Fig. 1. The metamorphic basement consisted
of graphitic phyllites, schists, greenschist, marble, amphibolites. Among of the metamorphic units, graphitic phyllite
is dominant lithology. Almost all of these units contain graphite in various grades. In the 11 Ha located to the south,
based on the drilling cores, graphitic phyllite in the shouthern part of mining concession is separated to be two main
ore body units. Both ore body units are separated by 13 m thick greenschist which are diping Southwest. The main
body situated below greenschist unit and located to the east of the area is characterized by some insertions of
graphite bearing schists.

(a) (b)

FIGURE 1. Tectonic setting of Southeast Sulawesi and the red box shows the location of PT Mekongga Sejahtera mining
concession in Southeast Sulawesi (a), 3D topography of PT Mekongga Sejahtera’s work in Site Tamboli, Samaturu District,
Kolaka Regenci, Shoutheast Sulawesi (b).

We used one of graphite bearing rock outcrops found in working area to accomplish the beneficiation study.
According to lithology description of the graphite ore outcrop as shown in Fig. 2, the graphite bearing rock exhibited
as schist rock with low weathered, medium to fine grained and metallic luster rock. The petrographic analysis is
shown in Fig. 3. Based on thin section petrographic analysis, the ore is composed by quartz, amorphous graphite,
flaky graphite and chlorite. Muscovite mineral spreads among the amorphous graphite mineral. The ore is
categorized as a schist rock.

(a) (b) (a) (b)


FIGURE 2. The out crop of graphite ore found in working FIGURE 3. Representative photomicrographs of the graphite
area, before (a) and after crushed (b). bearing rock. The presence of quartz, graphite and chlorite in :
plane polarized light photomicrograph (a), cross polarized
light photomicrograph (b).

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According to mineralogical analysis of graphite ore by using X-ray diffraction as shown in Fig. 4, non graphite
minerals are calcite (CaCO3), lipscombite (Fe1.176(PO4)(OH)0.57(H2O)0.43), lithium alumosilicate (LiAlSiO4), quartz
(SiO2), anatase (TiO2), and birnessite (K0.27(Mn0.98O2)(H2O)0.53). Table 1 shows the quantitative analysis of graphite
ore. Energy disspersive spectroscopy (JEOL JED-2300) were used to confirm the XRD result.

TABLE 1. The XRD Quantitative Analysis of Graphite Ore


Quant
No Compound Name Chemical Formula
[%]
1 Calcite CaCO3 75
2 Quartz SiO2 4
3 Lipscombite Fe1.176(PO4)(OH)0.57(H2O)0.43 8
4 Lithiumalumosil LiAlSiO4 5
i t
5 Anatase TiO2 4
6 Birnessite K0.27(Mn0.98O2)(H2O)0.53 1
7 Graphite C 3

FIGURE 4. The XRD of graphite ore

Methods
Flotation is a process of separation and concentration based on differences in the physicochemical properties of
interfaces. In froth flotation, the flotation takes place on a gas-liquid interface. The minerals that are easily wetted by
water are called hydrophilic minerals, whereas the minerals that have water-repellent characteristic are called
hydrophobic materials. Graphite is one of the hydrophobic mineral due to its water-repellent characteristic, this
characteristic can be indicated by its greasy texture. Hydrophobic minerals are selectively attached to the surface of
gas bubbles rising through suspension, are thereby separated in the form of froth.
The hydrophobic and hydrophilic characteristic can be modified by adding surfactants. A surfactant which
makes the surface hydrophobic, is called a collector. Because water is a polar compound, nonpolar collector such as
hydrocarbon should be added in suspension. Frothers are surface-active chemicals and usually be added to form
froth bed on the pulp and influence kinetics of bubble-particle attachment. The attachment of the bubbles and
hydrophobic material to the surface of liquid is determined by the interfacial energies between the solid, liquid, and
gas phases that can be determined by the Young/Dupre Equation :

γlv cos θ = ( γsv – γsl ) (1)

where γlv is the surface energy of the liquid/vapor interface, γsv is the surface energy of the solid/vapor interface,
γsl is the surface energy of the solid/liquid interface, and θ is the contact angle of interfacial tension between liquid
and vapor [5]. The contact angle is affect to the attachment of the bubbles. If the contact angle is very small, then the
bubble does not attach to the surface. While a very large contact angle results in very strong bubble attachment. A
contact angle near 90° is sufficient for effective froth flotation in most cases.
In this study, the froth flotation experiment was conducted in a flotation machine, with cell-volume 40 L using
27 kg of ore. Fuel diesel oil (C12H23 with cetane values 51-52 was used as collector, pine oil was used as frother, and
sodium silicate (Na2SiO3) was used as depressant. The effect of rotation speed (980, 1100, 1500 rpm), addition of
pH modifier (7, 9, 11) and particle size (-80, -150, -200 mesh) were studied.

EXPERIMENTAL SET-UP AND PROCEDURE


The representative ground ore pulp from the ball mill discharge of size mesh 80 was taken in agitation cell. The
apparatus provides recirculation and agitation to maintain thorough mixing for 1 hour. The pulp density was choosen

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3 L/kg (liquid to solid ratio). Na2CO3 (varied) was added to adjust the appropriate pH condition. Subsequently,
sodium silicate (1 l/t) was added to the pulp to depress the gangue minerals. Further, the pulp was conditioned with
1 l/t of diesel oil (C12H23) as collector and 1 l/t of pine oil as frother. The experimental procedure of beneficiation
process is shown in Fig. 5.

FIGURE 5. Experimental procedure of beneficiation process

RESULTS AND DISCUSSION


The SEM-EDS analysis of graphite concentrate is shown in Fig. 6. Based on SEM-EDS analysis, we can see that
carbon content from the concentrate is 61.61%. Some minerals composed by silicon, aluminium, iron, magnesium,
potassium and calcium remain as the impurities of concentrate. It is safely to say that the impurity is dominated by
the elements of silicon and oxygen that compose the silica mineral.

(a) (b)

FIGURE 6. SEM-EDS analysis of graphite concentrate

Effect of rotation speed


The effect of rotation speed was shown in Fig. 7. The maximum fixed carbon grade (59.64%) was achieved
when the rotation speed was fixed at 980 rpm, but the fixed carbon recovery is only 41%. Both of fixed carbon grade
and fixed carbon recovery are on the lowest points at 1500 rpm. The maximum fixed carbon recovery reached its
highest point (55%) at 1100 rpm with 59.26% of fixed carbon grade. It is noteworthy that proper rotation speed is

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needed to achieve both of fixed carbon grade and recovery. As the rotation speed is too slow, the liberated graphite
in the solution is attached easily to the top, but some part of the graphite still sink on the bottom due to the lack of
attachment power. Meanwhile, the concentrate has the lowest fixed carbon grade at the highest rotation speed. The
undesirable gangue minerals are attached together with the liberated graphite to the surface causing poor graphite
purity of the concentrate. Because of over speed, the attached graphite may be pulled back from the surface flotation
tank resulting a decrease of fixed carbon recovery.

FIGURE 7. Effect of rotation speed on fixed carbon grade and recovery

Effect of particle size


Based on empirical study, the effectivenes of reagents depends very much on the nature and type of mineral
present in the ore, as well as the ionic composition of the pulp. Selective adsorption of particular reagents depends
also on the particle size of the mineral present in the pulp. The optimum particle size by which graphite might be
separated with the maximum grade and recovery was achieved on size of -180 micrometers as shown in Fig. 8. This
result is in accordance with the prior liberated size analysis of the graphite in the host rock. On this size, the graphite
is liberated from its host rock, though it is more difficult to liberate all of the graphite. Coarse sized graphite ore
causing a large proportion of graphite is locked into its host rock and the separation produced poor results. The same
results are given by excess of fine sized graphite ore (down to 125 μm). It reduces the graphite size and therefore
coats other undesirable gangue minerals and recovered with the graphite concentrate, thereby reducing the grade of
the graphite. The gangue minerals could be attached by the graphite and prevent graphite attached to the air bubbles
resulting the recovery of graphite decreased.

FIGURE 8. Effect of particle size on fixed carbon grade and FIGURE 9. Effect of pH on fixed carbon grade and recovery

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Effect of pH
As the graphite is a naturally hydrophobic mineral and will float easily, the separable properties are normally
improved by the addition of reagents and alkaline condition. Graphite can be attached with hydrocarbon to form a
nonpolar bonding. Water is a polar compound so that it can interact with a polar reagents such as pH modifier to
form a ionic bonding. The effectivenes of the frothers is dependent on pH. The purpose of pH modifier is to regulate
the ionic composition of the pulp by changing the concentration of the hydrogen ion in the pulp. As the result,
interaction between collector and graphite is improved and vice versa, it reduces collector interaction with gangue
minerals. Figure 10 showed the effect of pH modifier addition on fixed carbon and recovery. The addition of pH
modifier effect both recovery and grade of the fixed carbon. The addition of pH modifier up to 11 pH condition
affects the attachment of carbon content. In Fig. 9 we could see that both optimum grade and recovery were
achieved on 9 pH condition. The smallest recovery was achieved in 11 pH condition.

CONCLUSIONS
Graphite ore beneficiation was successfully introduced to separate graphite with another minerals. The results
which presented in the previous section showed that optimum rotation speed was 1100 rpm, with -180 micrometers
ore size and 9 pH condition. The carbon grade increased from 3.00% to 60.00% at the optimum flotation conditions.
Further graphite concentrates grade can be purified by chemically leaching out the impurities from the concentrate
by our next research.

ACKNOWLEDGMENTS
This work has been supported by PT Mekongga Sejahtera. We are thankful to Assoc. Prof. Dr. Eng. I Made
Joni, head of Laboratory of Nanotechnology Research Center, DRPM, University of Padjadjaran for analyzing the
minerals content of powdered graphite samples by XRD. Thanks to Dr. Ir. Joko Soesilo, M.T, head of Petrographic
Laboratory, Departement of Geology, University of Pembangunan Nasional Veteran for supplying the petrographic
analysis of the graphite bearing rock samples.

REFERENCES
1. C.J. Mitchell, “Industrial minerals laboratory manual: flake graphite,” British Geological Survey Technical
Report WG/92/30 (1993).
2. I. M. Joni, C. Panatarani, D. Hidayat, Setianto, B. M. Wibawa, A. Rianto and H. Thamrin, “Synthesis and
dispersion of nanoparticles, and Indonesian graphite processing,” in Padjadjaran International Physics
Symposium 2013 (PIPS-2013), AIP Conference Proceedings 1554, edited by I Made Joni et.al. (American
Institute of Physics, Melville, NY, 2013), pp. 20-26.
3. O. Kaya and M. Canbazoglu, “The Enrichment of Turkey Kastamonu-Inebolu Graphite Ore by Flotation,” in
Balkan Mineral Processing Congress, Delphi, Greece. 2007, pp. 291-296.
4. Z. Meng and D. Shujuan, Advance Journal of Food Science and Technology 6(8), 989-993 (2014).
5. S. K. Kawatra, “Fundamental principles of froth flotation,” in SME Mining Engineering Handbook, edited by
Peter Darling (Society for Mining, Metallurgy, and Exploration, Inc, U.S, 1956), pp. 1517- 1531.
6. Srjan M. Bulatovic, “Classification of flotation reagents”, in Handbook of flotation reagents: Chemistry,
theory, and practice, (Elsevier science and technology books, 2007), pp xi.

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