International Journal of Coal Preparation and Utilization

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The enhanced flotation of coal by nanosilica

particles

Qingteng Lai, Yinfei Liao, Maoyan An & Zechen Liu

To cite this article: Qingteng Lai, Yinfei Liao, Maoyan An & Zechen Liu (2018): The enhanced
flotation of coal by nanosilica particles, International Journal of Coal Preparation and Utilization,
DOI: 10.1080/19392699.2018.1479261

To link to this article: https://doi.org/10.1080/19392699.2018.1479261

Published online: 25 May 2018.

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INTERNATIONAL JOURNAL OF COAL PREPARATION AND UTILIZATION
https://doi.org/10.1080/19392699.2018.1479261

ORIGINAL ARTICLES

The enhanced flotation of coal by nanosilica particles

Qingteng Laia, Yinfei Liaob, Maoyan Ana, and Zechen Liua
a
Key Laboratory of Coal Processing and Efficient Utilization of Ministry of Education, China University of
Mining and Technology, Xuzhou, China; bNational Engineering Research Center of Coal Preparation and
Purification, China University of Mining and Technology, Xuzhou, Jiangsu, PR China

ABSTRACT ARTICLE HISTORY

It is well known that the stability of hydration film on the particle surface Received 13 March 2018
affected the particle-bubble attachment in a flotation process. In this Accepted 17 May 2018
paper, the effect of attached nanosilica particles on the stability of liquid KEYWORDS
film around the coal particles was investigated by measurements of Flotation; induction time;
viscosity of the coal pulp and the bubble attachment time for coal EDLVO theory; hydration film
particles. The interaction energy between a nanosilica particle and a
coal particle was calculated using the EDLVO theory. Results showed
that the nanosilica-coal attachment was driven by hydration attraction.
And the stability of liquid film was weakened with the attachment of
nanosilica particles, which is probably due to the change of surface
roughness. In this case, the bubble-particle attachment time was
reduced and further improved the flotation recovery of coal.

Introduction
Flotation is the main method using the surface differences between valuable mineral and
gangue minerals in mineral processing field. The attachment efficiency is a crucial factor for
the flotation results. A number of models were proposed to estimate the probability of
bubble-particle attachment, such as Dobby and Finch (Dobby and Finch 1986, 1987) and
R-H Yoon (Yoon 2000). Besides, some researchers have studied the relationship between the
bubble-particle attachment time and the flotation results (Gu et al. 2003; Hewitt et al. 1993;
Scheludko 1976; Wang and Peng 2014; Yoon and Yordan 1991). The bubble attachment
time, first attributed to Sutherland (Sutherland 1948), has been demonstrated that attach-
ment between particles and bubbles will occur when the bubble attachment time is shorter
than the bubble-particle contact time. And the thinning of the liquid film is considered to be
the most crucial factor of bubble attachment time (Luttrell 1989). As mentioned above, the
focus of the discussion, in most of these studies, is based on the stability of hydration film.
The study of Derjaguin et al. (Derjaguin et al. 1984) indicated that the liquid film gradually
thinned until the occurrence of bubble-particle attachment. Miettinen et al. (Miettinen,
Ralston, and Fornasiero 2010) have studied the thinning process of liquid film by analyzing
particle surface forces including van der Waals force, electrostatic double layer force and
hydrophobic force. Another review of bubble-particle attachment has been given by
Scheludko (Scheludko 1976), in which the thinning liquid film was characterized in terms
of surface energy. Scheludko has proposed that the particles have to overcome the energy

CONTACT Yinfei Liao ruiyin@126.com

Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/gcop.
© 2018 Taylor & Francis
2 Q. LAI ET AL.

barrier resulted from the intervening liquid film if the bubble-particle attachment is to
occur. Accordingly, reducing the thickness of the hydration film or weakening the stability
of the film plays an important role in improving flotation recovery. One of the causes for the
formation of the liquid film is the attraction of the hydrophilic functional groups to water
molecules. In the past decades, a large body of experimental evidence showed that the
attachment of reagents on the particle surface could enhance the hydrophobicity and hence
reducing the stability of liquid film (Hewitt et al. 1993; Newcombe and Ralston 1994).
Besides, it was also reported that the stability of the hydration film could be influenced by
the concentration of metal ions in the solution (Hancer, Celik, and Miller 2001; Li, Kanda,
and Higashitani 2004). The addition of electrolytes could compress the electric double layer
and then decrease the magnitude of stern layer charge, by which the electrostatic attraction
might be weakened and therefore the decreasing contribution of hydrated ions to the
liquid film.
However, as indicated by Drelich et al. (Drelich et al. 2011) and Zhang et al. (Zhang
et al. 2011), not only the surface chemical composition but also the surface roughness
contributed to the hydrophobicity of the solid surface. Surface microstructures have a
significant effect on the wettability of the solid, which can be observed from hydrophobic
plant leaves (Koch, Bhushan, and Barthlott 2009; Koch and Ensikat 2008), such as lotus
leaves and rice leaves. In the past decades, great progress has been made in the preparation
of superhydrophobic surfaces with micro nanostructures. The main preparation methods
included sublimation method (Nakajima et al. 2000), Sol-gel method (Tadanaga,
Morinaga, and Minami 2000), etching method (Youngblood and Mccarthy 1999) and
chemical vapor deposition method (Sun et al. 2003). However, the process of mineral
separation is mainly carried out in the liquid environment. Therefore, it is impossible to
construct the micro and nanostructures on the surface of the particle by the methods
mentioned above.
The aim of this study was to investigate the effect of surface roughness on the flotation
of coal samples. In this paper, the surface roughness was conditioned by the attachment of
nanoscale silica particles, which was investigated by EDLVO theory, measurement of pulp
viscosity, bubble attachment time and the contact angle of coal. It was expected to find a
new way to improve the flotation recovery.

Materials and methods

Materials and reagents
The coal sample used in this paper was pure coal, which was obtained form Daliuda
(Neimenggu, China). And the ash content of the experimental sample is 2.36%. The
detailed information about the coal sample is shown in Table 1. The size of the nanosilica
particle is about 75 nm. The contact angle of the nanosilica is 132°. The nanosilica
particles were prepared by Sol-gel method and were made hydrophobic modified by

Table 1. The analysis of coal sample.

Mad/% Aad/% Vad/% FCad% Ad/% Vd/% Vdaf/% Fcd/%
8.08 3.59 29.23 59.10 2.36 32.02 33.14 65.62
 INTERNATIONAL JOURNAL OF COAL PREPARATION AND UTILIZATION 3

siloxane coupling agent method (Gun’Ko et al. 2002; Krysztafkiewicz, Rager, and
Jesionowski 1997; Li, Kanda, and Higashitani 2004).
Diesel and kerosene (industrial grade) were used as the collector and frother, respectively.
Other chemicals used in this study were analytical reagents.

Methods
Flotation experiments
The flotation experiments were carried out with 74–125 μm size fraction using a labora-
tory Agitair flotation cell (1 L) with air flow rate of 0.1 m3/h at natural pH. For each
flotation experiment, 50 g of a coal sample was added into the cell and mixed with tap
water at 1800 rpm for 3 min without reagents addition. The solid ratio of the pulp was
about 5%. After 3 min conditioning, the desired amount of nanosilica particles was added
and mixed for 5 min. The concentrations of nanosilica in the tests are 0, 0.025, 0.05, 0.075
ppm, respectively. In order to avoid particle aggregation, the nanoparticles were sonicated
for 10 min before being added to the pulp. The collector (500 g/Mg) was addedand
conditioned for 3 min. Then the frother (400 g/Mg) was added to the slurry and stirred for
another period of 2 min. The flotation concentrate was collected for 5 min. Concentrate
and tailing were filtered, dried at 60°C, and weighed for the calculation of flotation
recovery.

The measurement of viscosity

Viscosity measurement of coal sample in the absence and presence of nanosilica was
conducted by VT550 (Germany). The coal samples were ground and sieved down to a
particle size of less than 15 μm. Mixed 1 g of coal with 30 ml deionized water and desired
amount of nanosilica were added into the suspension. The solid ratio of the pulp was
about 3%. Then, the prepared suspension was conditioned using a magnetic stirrer for 15
min. Before the measurement, the coal sample needs to be stirred for another 1 minute to
ensure the uniformity of suspension. The concentrations of the nanosilica were 0, 0.025,
0.05, 0.075 ppm, respectively.

The calculation of EDLVO

In solution medium, the extended DLVO theory (EDLVO) was widely used for calculating the
interface interaction energy for different minerals particles. The total energy of interaction (V)
between the surfaces of two particles can be expressed as the contribution of the electrostatic
interaction energy (VE) (Hogg, Healy, and Fuerstenau 1966; Piñeres and Barraza 2011), Van
der Waals interaction energy (VW) (Honaker, Mohanty, and Crelling 1996; Yoon and Mao
1996) and the hydration interaction energy (VH) (Christenson et al. 1993; Churaev and
Derjaguin 1985). The calculating equations are shown in Equation (1) to Equation (6). The
result of EDLVO calculation is presented in Figure 5.
V ¼ VH þ VW þ VE (1)
 
H0  H
VH ¼ 2πR1 h0 VH0 EXP (2)
h0
4 Q. LAI ET AL.

A123 R1
VW ¼  (3)
6H

 
πεa R1 R2 2 2ϕ01 ϕ02
VE ¼ ðϕ þ ϕ02 Þ 2
2
Pþq (4)
R1 þ R2 01 ϕ01 þ ϕ202

 
1 þ EXPðκHÞ
P ¼ ln (5)
1  EXPðκHÞ

q ¼ ln½1  EXPð2κHÞ (6)

Where the Equation (2) was used to calculate hydration interaction energy. The Equation (3)
was used to calculate Van der Waals interaction energy. The Equation (4) to The Equation (6)
were used to calculate electrostatic interaction energy. h0 is the decay length of hydration
interaction energy. V°H is the interface interaction energy constant. H0 is the balance distance
between nanosilica surface and coal particle surface. H is separation distance between a
nanosilica particle and a coal particle. A123 is the Hamaker constant for nanosilica particles
interacting with the coal particle in deionized water. R1 is the radius of the nanosilica particle.
R2 is the radius of coal particle. εa is the dielectric constant of the medium. ϕ01 and ϕ02
represent the Stern potentials of the nanosilica particles and coal particles, respectively. 1/κ is
the Debye length. Detailed parameters required for the calculation of extended DLVO is
shown in Table 3.

Measurement of contact angle

The contact angle of coal was measured using the sessile-drop technique with the equip-
ment of DSA100 (KRUSS, Germany). The procedure of preparing pulp is the same as that
in chapter 2.2.1. After that, the pulp was filtered, dried at 60°C for measurement of contact
angle. This measurement method has been applied in a previous paper (Piñeres and
Barraza 2011).

Measurement of bubble attachment time

The bubble-particle attachment tests were carried out with Induction 2015EZ (Oil Sands
Environmental Development and Services Inc, Canada). The sample (45–74 μm) was washed
three times with deionized water to eliminate the interference of fine impurities. Mixing the
sample with 10 ml deionized water. And the solid percentage was 20% by weight. The bubble
attachment time experiments were carried out after the sedimentation of pulp for 4 hours. The
similar method has also been reported elsewhere (Oats, Ozdemir, and Nguyen 2010; Ozdemir
et al. 2009).

Results and discussion

Flotation
The flotation recovery without reagent addition was 19.03%. And the flotation recovery
was improved with addition of reagents and nanosilica particles. As the Figure 1 shown,
 INTERNATIONAL JOURNAL OF COAL PREPARATION AND UTILIZATION 5

100

90

80

Flotation recovery (%)

70

60

50

40

30

20
0 200 400 600 800 1000
The addition of collector (g/t)

Figure 1. The flotation of coal in the presence and absence of nanosilica particles.

the flotation recovery of coal was increasing with the increase of collector concentrations.
However, it is interesting to find the recovery of coal could be improved significantly in
presence of nanosilica particles. For this reason, the measurement of viscosity, the
calculation of EDLVO and measurement of bubble attachment time were carried out to
investigate the possible mechanisms for the improved flotation recovery with the addition
of nanosilica particles.

The measurement of viscosity

In the near part of the particle, with the decreasing distance between water molecules and
particle surface, water molecules are arranged more closely. The layer of water is difficult
to disperse due to the strong interaction between the surface of the particle and the water
molecules. Therefore, a liquid film is formed around the particles, which play a main role
in the bubble-particle attachment process. The existence of liquid film on the surface of
particles has also been reported elsewhere (Grabbe and Horn 1993; Yoon and Vivek 1998).
As reported by Grahame (Grahame 1947), there is a shear plane between the stern layer
and the diffusion layer, and the thickness of the hydration film is approximately equal to
the distance between the slip surface and the surface of the particle. As the diffusion layer
does not move along with the particles, the surrounding liquid causes a resistance to the
movement of the particles. The resistance was affected by the thickness and stability of the
liquid film. And the anti-shear ability of the suspension also increases with the increase of
resistance.
The concentrations of the nanosilica are 0–0.075 ppm in pulp, which is to ensure that the
nanosilica itself does not affect the viscosity of the solution. As the Figure 2 shown, with the
addition of nanoparticles, the viscosity of the pulp showed a decrease. In the viscosity tests, a
maximum viscosity of the pulp was obtained without the addition of nanoparticles, while the
viscosity of pulp was decreased in the presence of nanoparticles. It has been studied by Song et al.
(Song et al. 2005) and Zhou et al. (Zhou et al. 2008), the viscosity of suspension is susceptible to
6 Q. LAI ET AL.

40

35

30
0 ppm

Viscosity (mPas)
25 0.025 ppm
0.05 ppm
20 0.075 ppm

15

10

0 100 200 300 400 500

Shear rate (1/s)

Figure 2. The effect of nanoparticles on the pulp viscosity.

hydration ability of particles, strong hydratability is expected to enhance the strength of the
hydration film and reduced the amount of free water, both of which directly contribute to the
increased slurry viscosity. The definitive factors of suspension viscosity mainly involve particle-
particle interaction, space force and electric double layer (Tadros 1992). The surface potential of
the sample was expected to remain a constant value at the same pH value of pulp. Besides, the
space force normally induced by organic polymers or other macromolecules that bridged the
particles. The maximum nanoparticles concentration added in the experiment are 0.075 ppm,
which indicated that there is no possibility of chemical substances changing the wettability.
Therefore, the possible cause of the decreased pulp viscosity is the changed stability of liquid film
on the particle surface. The attachment of nanoparticles have constructed a nanoscale roughness
on the surface of a particle and hence the decreased stability of the hydrated film. Besides, the
amount of particles adsorbed on the surface of coal particles increases with the increased
concentration of nanoparticles in the solution, which leads to the more obvious instability of
the hydration film. The positive effect of surface structure on the hydrophobicity of solid has also
been reported by Koch et al. (Koch, Bhushan, and Barthlott 2009), in which the conclusion was
drawn from the study of natural hydrophobicity plant. A detailed review of hydrophobic surface
design has been given by Extrand (Extrand 2002). The hydrophobicity of particles can be
improved by the preparation of micro nanostructures on the surface of particles. There are
two main models for the correlation between surface roughness and hydrophobicity. Wenzel
(Wenzel 1936) is the first one to take into account the surface roughness in the influencing factors
of wettability. The Wenzel model could be applied in the case of thermodynamic stability system.
In this model, the liquid needs to overcome the surface energy barrier to achieve a complete
coverage. Another typical model is Cassie and Baxter model, in which the presence of micro-
structure caused the air to remain in the gap between the protuberances. The stability of liquid
film was weakened due to the presence of residual gas on the solid surface. In this study, a similar
effect of nanoparticles was observed on the stability of liquid film that located on the surface of
coal particles.
As Figure 3 shown, the apparent viscosity decreased with the increase of shear rate. It
was noted, however, that the decreasing rate of apparent viscosity is not uniform in the
 INTERNATIONAL JOURNAL OF COAL PREPARATION AND UTILIZATION 7

35

30

0.075 ppm
25
0.05 ppm

Viscosity reduction rate

20
0.025 ppm
0 ppm
15

10

-5
100 200 300 400 500
Shear rate (1/s)

Figure 3. The effect of nanoparticle on the viscosity reduction rate.

process of increasing the shear rate. Besides, the maximum values of lowering rate for each
nano-particle concentration were obtained at different shear rates. As can be seen from
Figure 3, the maximum lowering rate occurred at the point of 250 s− without the addition
of nanoparticles. The highest lowering rate in the presence of 0.075 ppm nanoparticles
corresponded to a shear rate of 70 s−. It is clear that the required shear rate for the highest
lowering rate was decreasing with the increased concentrations of nanoparticles among
the four curves. These differences mentioned above might be related to the weakened
shear resistance of the suspension in the presence of nanosilica. As the rotor moves at low
speed, the surrounding liquid will rotate with the rotor. Meanwhile, the liquid near the
rotor will drive its outer liquid layer to rotate together due to the presence of interaction
between liquid molecules. Since the nanoparticles were attached to the surface of coal
particles, the stability of the liquid film was weakened and therefore diminishing global
motion characteristic of suspension. In this case, the velocity gradient was easily presented
between the sections that parallel to the rotor. Therefore, the required shear rate with the
addition of nano-particles was lower than that without nano-particles.

The calculation of EDLVO

As can be seen from Figure 4, Van der Waals force is an attractive force. The value of Van
der Waals energy is −2.95621E-19 J at the separation distance of 0.1 nm while it is
−5.91242E-21 J at the position of 5 nm. It was observed that the magnitude of Van der
Waals energy was decreasing with the increase of separation distance. On the contrary, the
electrostatic interaction force is repulsive at all separation distances. This is due to that
both the nano-silica particles and the coal surface are negative in the suspension of natural
pH value. It should be noted that the curve of the total energy coincided almost with that
of the hydration interaction energy. It is concluded that the hydration interaction energy
is the predominant energy, while the nanosilica particles are interacting with a coal
particle. With the increase of separation distance, the magnitude of hydration interaction
8 Q. LAI ET AL.

0.0

Electrostatic interaction energy WE (10-19J)

Total energy of the interface (10-17J)

1
-0.1

Hydration interaction energy

Van der Waals energy VW
-0.2
0

-0.3
Vw
-1
VE
-0.4
VH
-2 VTotal
-0.5

-0.6
-3

-0.7
0 5 10 15 20 25 30 35 40 45 50 55
Distance (H) between coal particles and nano-silica particles (nm)

Figure 4. EDLVO energy between a coal particle and a nanosilica particles versus inter-surface separa-
tion distance.

Figure 5. The schematic of bubble motion in the process of induced time measurement.

energy increased gradually. It is interesting to find the trend of the values is in disaccord
with other articles related to DLVO theory (Oats, Ozdemir, and Nguyen 2010; Piñeres and
Barraza 2011). This is probably due to that nanoparticles have a particularly large specific
surface area and a high surface energy (Nanda et al. 2003). In particular, at a short
separation distance, the hydration attraction is so strong that Van der Waals energy and
electrostatic interaction could be neglected. However, the effect of Van der Waals energy
and electrostatic interaction energy played a main role in the total interaction energy with
the increase of separation distance (H). At the position of H = 34 nm, the total interaction
energy changed to repulsive force. It indicated that the effect of the large specific surface
area was weakened gradually with the increase of separation distance. Besides, at a long
separation distance, the liquid film was formed around the particle surface (Grabbe and
Horn 1993; Yoon and Vivek 1998), which may weaken the interface interaction. However,
it could be concluded that the nanosilica particles do attach to the surface of the coal
particles.
 INTERNATIONAL JOURNAL OF COAL PREPARATION AND UTILIZATION 9

Measurement of contact angle

Table 2 showed the contact angle values of the coal sample treated by nanosilica and
untreated sample. The maximum mass ratio of nanosilica to graphite is 1.5:1000000
among the four samples. It was observed clearly that the contact angle of coal samples
was not improved in the presence of nanosilica particles. The possible cause for the results
is that the amount of nanosilica is too small to affect the wettability energy of the coal.
And the contact angle is the characterization of the wettability energy of the overall
samples instead of a single particle (Hong et al. 2011; Mohammadi-Jam, Burnett, and
Waters 2014). Therefore, the possibility that the improved recovery was the result of
improved chemical hydrophobicity on coal surface can be ruled out in the presence of
nanosilica.

Measurement of bubble attachment time

As described in the introduction section, the bubble attachment time is closely related to
the floatability of minerals. As reported by Sutherland (Sutherland 1948), it is necessary
that bubble attachment time is shorter than contact time for the bubble-particle attach-
ment. In flotation process, the contact time of particles is usually related to the flotation
equipment and the physical properties of the feeding. And the magnitude of bubble
attachment time was controlled mainly by the stability of liquid film regulated by hydro-
phobicity properties and microstructure on the solid surface. The liquid film at the
collision point between the bubble and the particle surface is gradually drained during
the collision process. The particles could attach to the bubble surface successfully only if
the liquid film was thinned to a certain thickness within the contact time. If the particle
was covered with a stable liquid film, the time required for the thinning of the film would
be extended, which means that the bubble attachment time increases with the stabilization
of the liquid film around the particle surface.
As the Figure 6 shown, the bubble attachment time was shortened with the increase of
the concentrations of nanoparticles. The bubble attachment time is 150 ms without the
addition of nanosilica particles. With the addition of nanosilica particles (40 ppm), the
bubble attachment time is reduced to 60 ms. This is in agreement with the predicted
results that poor stability of liquid film was obtained with the attachment of nano-
particles. In bubble-particle collision process, the draining rate would be improved with
unstable liquid film, that is, the time required to thin to the effective collision thickness is

Table 2. Contact angle of coal samples.

Concentration of nanosilica particles in the sample (ppm) 0 0.025 0.05 0.075
Contact angle (Distilled water) 49.5 50.2 48.7 50.7

Table 3. The parameters for the calculation of EDLVO.

R1 R2 V°H h0
75 nm 74 μm −1.57E-03 1.00E-08
H0 A123 εa Κ−1
1.24E-08 2.36497E-21 6.95E-10 C−2J−1m−1 0.056 nm −1
10 Q. LAI ET AL.

Figure 6. The effect of nano-particles on the bubble attachment time for coal particles in suspension.

shorter than that with the stable film. In recent years, in the case of constant contact time,
shortening the bubble attachment time by adding reagents was considered as an effective
way to improve the flotation recovery (Xu et al. 2018; Ye and Miller 1988). However, most
of these studies are concerned with the surfactant that consists of two main parts:
hydrophilic groups, hydrophobic groups. Hydrophobicity of particle surface becomes
increasingly pronounced with the attachment of surfactant, leading to a thinner liquid
film around the particle and hence a shorter bubble attachment time.

Conclusion
The flotation experiments were carried out with the pure coal sample. With the addition
of nanosilica particles, the flotation recovery of coal is significantly higher than that
without nanosilica. According to the calculation of EDLVO, hydration attraction played
a dominant role among the three components (Electrostatic interaction energy, Van der
Waals interaction energy, and hydration interaction energy) of total interaction energy
due to the high surface energy caused by the particularly large specific surface area of
nanoparticles. The nanosilica particles were successfully driven to the surface of the coal
particles in the presence of hydration attraction. With the attachment of nanosilica, the
stability of liquid film was reduced, resulting in decreased viscosity and shorter bubble
attachment time. And the flotation recovery of coal was increased with the decrease of
bubble attachment time at constant conditions. It was concluded that the possible way to
increase the flotation recovery is to change surface roughness of particles.

Funding
This research was supported by the Natural Science Foundation of Jiangsu Province (BK20150192).
The authors also acknowledge the assistance of Project Funded by the Priority Academic Program
Development of Jiangsu Higher Education Institutions.
 INTERNATIONAL JOURNAL OF COAL PREPARATION AND UTILIZATION 11

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