Fuel 84 (2005) 1879–1883

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A pilot-scale flotation column to produce beneficiated coal fractions

having high concentration of vitrinite maceral
Juan Barraza*, Jorge Piñeres
Escuela de Ingenierı́a Quı́mica, Universidad del Valle, Ciudadela Universitaria Meléndez, Cali, Colombia

Received 25 October 2004; received in revised form 21 March 2005; accepted 22 March 2005
Available online 19 April 2005

Abstract
A pilot-scale flotation column was used to produce beneficiated vitrinite-rich fractions from two coal samples from south western
Colombia, Guachinte and Yolanda. The coal samples of less than 38 mm in size were processed in the flotation column at pH ranging from 7
to 11 using various concentrations of a particular frother. Results showed that, using a single stage separation, maximum mass yield of float
fractions was 84.6% w/w for Guachinte coal and 55.5% w/w for Yolanda. The maximum ash removals were 71.7 and 76.5% for Guachinte
and Yolanda coals, respectively. This corresponds to sulphur removals of 63.2% for Guachinte coal and 75.4% for Yolanda coal. The highest
concentration of vitrinite was obtained using Yolanda coal. It was in the order of 99.8% at neutral pH and when using the highest frother
concentration. This result is the highest concentration of vitrinite maceral reported in the literature using a pilot-scale flotation column.
q 2005 Elsevier Ltd. All rights reserved.

Keywords: Vitrinite maceral; Column flotation; Colombian coals

1. Introduction macerals have differences in both hydrophobicity and

Beneficiated coal is usually produced in treatment plants
where mineral matter is decreased and organic matter is
increased [1]. However, nowadays the trend is to beneficiate
coal in order to concentrate maceral groups.
Several researchers [2–4] have shown that macerals have
some chemical properties which can increase the aggregated
value of the coal. Liptinite, for instance, can be used as raw
material for chemical products. Vitrinite can be a raw
material for liquefaction and gasification processes; whereas
inertinite is a basic material to produce activated carbon and
graphite.
Macerals separation is usually carried out at laboratory
scale based on the difference in the gravitational or surface
properties of the macerals. Although macerals separation by
centrifugation has some advantages, this technique is
limited to laboratory scale [5]. Due to the fact that coal
* Corresponding author. Tel: C57 2 3312935; fax: C57 2 3392335.
E-mail address: jubarraz@univalle.edu.co (J. Barraza).
0016-2361/$ - see front matter q 2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.fuel.2005.03.021
electrokinetics surface properties, flotation process could
be implemented to produce concentrated coal macerals [2].
A study [6] was carried out to measure contact angle on
several coal samples in order to quantify the hydrophobicity
of individual coal maceral. It was found a hydrophobicity
decreasing order liptiniteOvitriniteOinertinite having a
typical range of contact angle of 90–130, 60–70 and 25–408,
respectively. This decreasing order of hydrophobicity
agrees well with the lithotype and maceral flotability results
obtained from previous investigations utilizing
conventional flotation cells [2,6,7].
Process to float coal involves conventional cell and
column flotation. The former uses big air bubbles, which
produces high turbulence; whereas the latter can separate
fine coal particles owing to the use of small air bubbles,
which create a quieter environment. A deep layer of frother
and the addition of wash water at the top of the column, give
also an additional improvement in selectivity between
hydrophobic and hydrophilic particles, as well as in the
amount of hydrophobic particles.
The aim of this work was to obtain float coal fractions
having high concentration of vitrinite maceral using a pilot
scale flotation column.
1880 J. Barraza, J. Piñeres / Fuel 84 (2005) 1879–1883
2. Experimental
Two bituminous coal samples from South western
Colombia, Guachinte and Yolanda, were used in this
study. The coal samples were ground and sieved down to
!38 mm. Those analyses were carried out in accordance
with ASTM methods. Maceral content in a v/v mineral-
matter free basis was obtained by using a Leitz microscope
equipped with a 32! magnification oil-immersion lens and
a 10! magnification eyepiece. A point counting device was
attached to the microscope semi-automatic stage which
allowed 500 separate maceral points to be counted for each
analysis.
A 5 cm diameter conventional flotation column of
5 m high and made from acrylic material was used in
this study. Pulp feeder point was placed at 120 cm
below the top. In order to increase the pulp residence
time, a flow of recirculated tails was located at 65 cm
of distance below the feeder. Both, frother and air were
supplied at 38 cm of distance above the bottom of the
column. The bubbler, made from ground glass, was
17 cm long.
All runs were carried out using a single separation
stage and a pulp concentration of 2.5% w/w. Three-
millilitre of collector (creosote oil) were added to the
pulp. In order to have a good distribution of bubbles
through out the column, a 1.7 bar airflow of 2.15 l/min
was used. The frother (Lauril ether sulphate of sodium)
mixed with air, was added by means of a peristaltic
pump at a flow of 42.2 ml/min. Three different
concentrations of frother were used: 0.0075, 0.0100
and 0.0125% v/v. The pulp was fed into the column at
a flow rate of 2.92 l/min and the tails at 2.4 l/min. This
guaranteed a constant interface level at 23 cm above the
feeder position which aided to produce a stable foam.
pH used were 8.0, 9.5 and 11.0. To obtain those figures,
NaOH 1.1 N standard was used. Blank run (without
addition of NaOH) was carried out to evaluate the effect
of NaOH presence. It produced a pH of 7.1 for
Guachinte coal and 7.5 for Yolanda coal, respectively.
pH under 7 was not used due to column flotation
material (acrylic) and pump material (iron cast) are not
suitable for acidic conditions.
Although the flotation process is a function of several
factors such as particle size, oxidation, rank of coal,
pulp concentration, pulp residence time, and air flow;
Table 1
Proximate and petrographic analyses of parent coals
Parent coal Proximate analysis, wt%, db
Ash VM FC
Guachinte 9.8 47.4 42.8
Yolanda 15.6 23.2 61.2
mmf, Mineral matter free; db, dry basis.
pH of pulp and frother concentration were selected as
control variables since they were the most significant in
preliminary tests. Response variables included mass
yield of float fractions, ash, sulphur and maceral content
of floats. All runs were made in duplicate. The
experimental error based on repeated experiments was
G2% for mass yield data, G0.5% for ash, G0.1%
sulphur, G2.0% for maceral content and mineral matter
and G0.02% for vitrinite reflectance.
3. Results and discussion
3.1. Proximate and petrographic analysis of parent coals
Table 1 shows proximate and petrographic analysis of
the parent coals. Results show that Guachinte coal is higher
in volatile matter than Yolanda coal. However, Yolanda
coal exhibits higher ash and sulphur content than Guachinte
coal. Heat values are related to ash content. Guachinte coal
has higher heat value. It may be due to its lower ash
percentage.
In terms of maceral concentration, results in Table 1
show that both parent coals have approximately similar
inertinite content. However, Yolanda coal has higher
vitrinite content than Guachinte coal. Guachinte coal
exhibits low concentration of liptinite and Yolanda coal
virtually none, which could be due to it was counted some
liptinite as mineral matter. Results in Table 1 show also that
Yolanda coal presents higher vitrinite reflectance than
Guachinte coal. It means that Yolanda coal has higher rank
than that of the Guachinte, and as expected the volatile
matter content of samples correlates well with its vitrinite
reflectance.
3.2. Effect of pH and frother concentration on mass yield,
ash and sulphur content of floats
The effect of both pH and frother concentration, on mass
yield, ash and sulphur content of floats on a dry basis is
shown in Table 2. Using a single stage, mass yields of float
fractions from Guachinte coal were in the range
54.1–84.6%. The highest yield (84.6%) was found using a
frother concentration of 0.0100% v/v and a pH of 9.5. A
relatively high mass yield (70.1%) was also obtained using a
normal pH of 7.1 (without NaOH presence) and the highest
Maceral content, vol%, mmf Rank, vol% Calorific Sulphur,
value, kJ/kg wt%, db
Vitrinite Liptinite Inertinite VRo HHV ST
76.9 18.8 4.3 0.47 5727.4 1.6
96.8 0.0 3.2 0.80 5607.9 2.4
 J. Barraza, J. Piñeres / Fuel 84 (2005) 1879–1883 1881

Table 2 Regarding sulphur content, in general, sulphur content of

Mass yield, ash, and sulphur content of floats as a function of pH and frother floats is lower than that of the parent coals. No appreciable
concentration
differences among sulphur content figures are observed. The
Coal Mass Ash, Ash Sulphur, Sulphur lowest sulphur content for Guachinte and Yolanda were 1.1
samples yield, wt%, db removala, wt%, db removalb, and 1.4%, respectively, which was achieved without
wt%, db wt%, db wt%, db
addition of NaOH and by using a frother concentration of
Guachinte 0.0075% v/v. Those results produced the highest sulphur
Parent 9.8 1.6
8.0/0.0075c 80.8 6.6 45.2 1.2 38.4
removal for Guachinte (63.2%) and for Yolanda coal
8.0/0.0125 69.9 6.8 51.7 1.3 41.9 (75.4%).
11.0/0.0075 70.3 5.8 58.6 1.2 47.7
11.0/0.0125 72.3 6.9 48.8 1.3 43.1
9.5/0.0100 84.6 6.7 42.5 1.3 34.1 3.3. Effect of pH and frother concentration
7.1/0.0075d 54.1 5.1 71.7 1.1 63.2 on floats maceral content
7.1/0.0125d 70.1 6.5 53.6 1.2 48.7
Yolanda Floats maceral content results as a function of pH and
Parent 15.6 2.5
8.0/0.0075c 53.1 11.2 61.8 1.8 60.2
frother concentration are given in Table 3 In general,
8.0/0.0125 46.5 12.9 61.4 1.9 64.3 vitrinite maceral content of floats is higher than that of the
11.0/0.0075 34.4 12.2 73.2 1.7 75.9 parent coal, whereas liptinite, inertinite and mineral matter
11.0/0.0125 34.4 12.0 73.5 1.7 76.3 are lower. However, liptinite maceral content of floats of
9.5/0.0100 55.5 10.5 62.7 1.7 62.1
Yolanda is higher than that of the parent coal.
7.5/0.0075d 43.3 8.5 76.5 1.4 75.4
7.5/0.0125d 46.6 11.1 66.9 1.4 73.5 Vitrinite concentration of float fractions for Guachinte and
a
Yolanda was in the range 89.9.1–95.2% and 96.9–99.8% v/v,
Ash removal, %Z[1K(yield)(float ash)/(feed ash)]!100.
b respectively. The highest vitrinite concentration (99.8%) was
Sulphur removal, %Z[1K(yield)(float sulphur)/(feed sulphur)]!100.
c
Coal samples obtained at pH/frother concentration. found using a frother concentration of 0.0125% v/v and a pH
d
pH obtained without addition of NaOH. of 7.5 (without addition of NaOH). This result is the highest
concentration of vitrinite maceral reported in the literature
frother concentration of 0.0125% v/v. This result is using a pilot-scale flotation column.
important from point of view of maceral production and It was generally observed that for all the conditions of pH
reactive cost, especially the cost of NaOH. The range of and frother concentration used, vitrinite concentration of
float mass yields found from Yolanda coal was between float fractions from Yolanda coal were higher compared to
34.4 and 55.5% using a pH of 9.5 and a frother those obtained from Guachinte coal. Despite of that, the
concentration of 0.0100% v/v. column flotation process was more effective to concentrate
It was generally observed that for the various conditions vitrinite in Guachinte coal than that of the Yolanda coal.
of pH and frother concentration used, mass yields of float
Table 3
fractions from Guachinte coal were higher compared to Petrographic analysis of floats as a function of pH and frother concentration
those obtained from Yolanda coal. This behaviour may be
due to the fact that the air bubbles have a higher probability Coal Vitrinite, Liptinite, Inertinite, Mineral
samples vol%, mmf vol%, mmf vol%, mmf matter,
to catch the organic particles from Guachinte coal since it vol%
has higher organic matter content than Yolanda coal.
Guachinte
In terms of ash, results in Table 2 indicate that, in
Parent 76.9 18.8 4.3 12.2
general, ash content of floats is lower than that of the parent 8/0.0075a 88.9 7.9 3.2 7.1
coals. No appreciable differences among ash content figures 8/0.0125 95.2 3.1 1.6 7.9
of floats are observed. The lowest ash content for Guachinte 11/0.0075 89.9 7.1 3.0 9.6
and Yolanda coal floats were 5.1 and 8.5%, respectively. 11/0.0125 90.3 6.7 3.0 4.3
9.5/0.0100 90.4 7.3 2.4 7.2
This was achieved without addition of NaOH and by using a 7.1/0.0075b 90.3 8.2 1.4 1.6
frother concentration of 0.0075% v/v. 7.1/0.0125 89.1 8.9 2.1 4.0
Despite the little differences in floats ash content, there Yolanda
are some variations in the percentages of ash removal, Parent 96.8 0.0 3.2 33.5
which can be observed in Table 2. The highest ash removal 8/0.0075a 96.9 1.9 1.2 5.0
8/0.0125 98.7 1.1 0.2 9.6
for Guachinte (71.7%) and for Yolanda coal (76.5%) was
11/0.0075 98.6 0.2 1.2 8.6
obtained without addition of NaOH and using the lowest 11/0.0125 99.1 0.9 0.0 3.5
frother concentration. 9.5/0.0100 98.7 0.5 0.4 7.1
From the above results, it appears that the best conditions 7.5/0.0075b 99.2 0.8 0.0 2.8
used in this work to obtain float coals having low ash 7.5/0.0125 99.8 0.2 0.0 4.8
content are normal pH (without addition of NaOH) and the a
Coal samples obtained at pH/frother concentration.
b
lowest frother concentration, 0.0075% v/v. pH obtained without addition of NaOH.
1882 J. Barraza, J. Piñeres / Fuel 84 (2005) 1879–1883

Fig. 3. Photography of maceral in Guachinte parent coal.

Fig. 1. Photography of maceral in Guachinte coal. Sample obtained without

NaOH addition (pH 7.1) and frother concentration of 0.0075% v/v.

It means that the increasing percentage for Yolanda coal (on

the basis of vitrinite concentration in parent coal) was 3.1%
whereas Guachinte coal was 23.8%.
Photographs of parents and floats having high concen-
tration of vitrinite are shown in Figs. 1–4. Comparisons
between photographs confirm that exist high concentration
of vitrinite maceral in floats.
Liptinite concentration of floats from Guachinte coal is
lower than that of the parent coal, whereas liptinite in floats
from Yolanda is higher. It may be due to Guachinte coal
could present low resinite (which conforms liptinite and has
hydrophobicity [2]), whereas Yolanda has high resinite
content.
Mineral matter concentration of floats is also lower than
that of the parent coal. Mineral matter decreased in
Guachinte coal from 12.2 to 1.6% v/v, whereas for Yolanda Fig. 4. Photography of maceral in Yolanda parent coal.
coal was from 33.5 to 2.8% v/v. Those results are in
agreement with ash concentration of floats, which are lower
than those of the parent coal. It is shown by comparing
Figs. 1 and 2, which have low presence of mineral matter,
with Figs. 3 and 4, having high presence of mineral matter.

4. Conclusions

The column flotation separations showed different mass

Fig. 2. Photography of maceral in Yolanda coal. Sample obtained without
NaOH addition (pH 7.5) and frother concentration of 0.0075% v/v.
yields, ash and sulphur concentration of floats for the
Yolanda and Guachinte coals and hence optimization of the
operation condition (pH and frother concentration) is
required for each coal.
Pilot-scale test using column flotation separations
indicated that it is effective in producing concentrates with
a vitrinite-rich fraction. The highest vitrinite concentration
(99.8%) was found using a frother concentration of
0.0125% v/v and a pH of 7.5 (without addition of NaOH).
 J. Barraza, J. Piñeres / Fuel 84 (2005) 1879–1883
This result is the highest concentration of vitrinite maceral
reported in the literature.
Acknowledgements
The authors would like to acknowledge the support of
Colombian Institute of Science and Technology (Colcien-
cias) through the research program ‘Young Researchers’.
The assistant of Miss Astrid Blandon for performing the
petrographic analysis at Universidad Nacional de Colombia
(Medellin) is also acknowledged.
1883
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