Soft Nanoscience Letters, 2011, 1, 97-104
doi:10.4236/snl.2011.14017 Published Online October 2011 (
Copyright © 2011 SciRes. SNL
Potential Application of Silica Aerogel Granules
for Cleanup of Accidental Spillage of Various
Organic Liquids
Vinayak G. Parale1, Dinesh B. Mahadik1, Mahendra S. Kavale1, A. Venkateswara Rao1*,
Pratap B. Wagh2, Satish C. Gupta2
1Air Glass Laboratory, Department of Physics, Shivaji University, Maharashtra, India; 2Applied Physics Division, Bhabha Atomic
Research Centre, Mumbai, India.
Email: *
Received April 26th, 2011; revised May 30th, 2011; accepted September 23rd, 2011.
The experimental work has been carried out to study the absorption-desorption properties of the silica aerogels, for
their use in oil spill cleanup application. For these studies, silica aerogel granules were prepared by two step acid–
base catalyzed sol–gel process, involving ambient pressure drying of alcogels, were made use for absorption & desorp-
tion studies of different organic liquids. The optimal molar ratio of precursors tetraethoxysilane (TEOS):Methanol
(MeOH):Oxalic acid:NH4OH:NH4F:trimethylchlorosilane (TMCS) was kept constant at 1:16.5:0.71:0.58:0.60:0.98,
respectively. In all, four alkanes, four aromatic compounds, four alcohols and three oils were used for absorption and
desorption studies of organic liquids. The absorption capacity of aerogel sample was quantified by measuring the mass
of the organic liquid absorbed by unit mass of the aerogel sample. The hydrophobic aerogel granules showed a very
high uptake capacity and high rate of uptake. The desorption of solvents and oils was studied by keeping the liquid ab-
sorbed aerogel granules at various temperatures and weighing them at regular time intervals until all the absorbed
liquid got totally desorbed. The Fourier transform infrared spectroscopy analysis showed that the aerogel structure was
not much affected by the solvent absorption, while the oil absorption led to the shrinkage, resulting in a dense structure
after desorption.
Keywords: Oil Spill Cleanup, Ambient Pressure Drying, Hydrophobic, Silica Aerogels
1. Introduction
Marine oil spills are the most important threat to the
coastal environment and ecosystem of the sea. Moreover,
oil spills are responsible for the great loss of energy re-
sources. They are formed mainly by occasional acciden-
tal episodes of super tankers, oil rig drilling, war and
natural events. Therefore, the ecological disasters result-
ing from oil spills have created a great need for cost ef-
fective cleanup systems. In recent years large numbers of
studies have been devoted to oil sp ill cleanup [1 ]. A wide
range of materials for oil remediation have actually been
employed such as dispersants, absorbents, solidifiers and
booms [2-8]. Dispersants simply disperse the oil to ac-
celerate the oil and separate it from the water by absorp-
tion. Absorbents collect the oil and separate it from the
water by absorption. Absorbent materials are attractive
for oil spill cleanup applicatio n because of the possibility
of collection and complete removal of the oil from the oil
spill site. The addition of absorbents to oil spill areas
facilitates a change from liquid to semi-solid phase and
once this change is achieved, the removal of the oil by
removal of the absorbent structure then becomes much
easier. Solidifiers react with the oil to form a cohesive,
solidified mass that floats on water and Booms are used
to trap the oil in small area [9].
The properties for good absorbent materials include
hydrophobicity and oleophilicity, high uptake capacity,
reusability and biodegradability of the absorbents [10].
Advanced material engineering techniques can structure
surfaces that allow dynamic tuning of their wettability all
the way from superhydrop hobic (i.e. repelling ) behaviour
to almost complete wetting (i.e. super hydrophilic) but
these surfaces only work with high-surface-tension liq-
uids [11]. Almost all organic liquids that are everywhere
Potential Application of Silica Aerogel Granules for Cleanup of Accidental Spillage of Various Organic Liquids
in human environment such as oils, solvents, detergents,
etc. have quite low surface tensions and thus easily wet
the hydrophobic surfaces. Silica aerogels possess low
surface energy; therefore it absorbs liquid which possess
surface energy less than the surface energy of aerogels
Silica aerogels, a class of mesoporous materials with
extremely high porosities (~98%) and high surface area
(700 - 1600 m2/g), have found potential applications in
thermal insulation, low dielectric constan t thin layer, low
refractive index glass, catalysts, absorbents etc. [13].
Aerogels are usually synthesized by hydrolysis and con-
densation of the silicon alkoxide followed by supercriti-
cal drying of the solvent from a wet gel. In supercritical
state of the solvent, the surface tension becomes zero and
hence the resulting aerogels fo und to be monolithic [14].
However, supercritical process is expensive and danger-
ous, which puts the restriction on the commercial scale
processing of the aerogels [15]. Therefore, attempts have
been made to synthesize the cost effective silica aerogel
by atmospheric pressure drying method involves me-
chanical shaking of alcogels, to accelerates the solvent
exchange process [16]. This method is commercially
attractive as a safer process compared to supercritical
drying process; however the total processing period is
only 36 h, which helps to reduce the production cost of
silica aerogel granules. The only disadvantage of ambient
pressure drying is the retrieved aerogel are in the form of
pieces instead of monolithic. But for oil spill cleanup
application, monolithic aerogels becomes pieces after
absorption of oil, therefore it is better to use pieces of
aerogels for oil spill cleanup application. The hydropho-
bic silica aerogels were found to be excellent absorbers
of organic liquids with high uptake capacity therefore it
can be used for oil spill cleanup application. In absorp-
tion and desorption studies all, fifteen solvents: four al-
kanes, four aromatic compounds, four alcohols and three
oils have been used to study the absorbtion capacity and
the rate of desorption of the liquids of the hydrophobic
2. Materials and Methods
2.1. Experimental Procedure
The synthesis of an aerogel involves two major steps: 1)
the preparation of the alcogel by two step acid-base
catalyzed sol-gel process and 2) the ambient pressure
drying of the wet gel to remove the solvent.
Initially, the tetraethoxysilane (TEOS) was diluted in
methanol (MeOH) solvent and was partially hydrolyzed
with water under acidic conditions with oxalic acid
(0.0005 M). The sol was stirred for 1h and kept for hy-
drolysis for 6 h. The molar ratio of TEOS:MeOH:Oxalic
acid:NH4OH:NH4F:TMCS was kept constant at 1:16.5:
0.71:0.58:0.60:0.98 respectively. After hydrolysis base
catalysts were added in the sol and after gelation, gel
kept in oven for 45 min., for strengthening the gel net-
work. After aging of the alcogels, they were cut into
small cubic pieces. The methanol was decanted out and
hexane was added. The methanol in the gel was ex-
changed with hexane at 50˚C. The alcogels in hexane
was shaked at 120 rpm for 4 h in a shaker (Remi instru-
ments, Mumbai, India). To make the gels hydrophobic,
the gels were immersed in a liquid mixture containing
7% TMCS of the 93% hexane for silylation and kept in
oven for 16 h at 50˚C. The unreacted TMCS was ex-
changed with the solvent by keeping again in the shaker
for 4 h at 50˚C with 120 rpm speed. Finally, the alcogel
pieces along with a little solvent were kept in the bottle.
The bottle was covered with aluminum foil with 8 - 10
small pin holes to allow the evaporation of the solvent.
These bottles were kept in the oven at 50˚C for 1 h and at
150˚C for 2 h. The retrieved aerogels were cooled to
room temperature and used for absorption and desorption
studies of va rious organic liq uids.
2.2 Reaction Mechanism
The hydrolysis and condensation of methanol diluted
tetraethoxysilane (TEOS) in the presence of oxalic acid,
NH4OH and NH4F is shown in the following chemical
2.2.1. Hy d rolysis
25 225
SiOC H4H OSiOH4C H OH
2.2.2. C ond ensation
 
The hydrophobicity was achieved by surface chemical
modification of alcogels by 7% trimethylchlorosilane
(TMCS) in hexane. The surface modification of the gel
with TMCS is shown in the reaction (3) [12,17].
Copyright © 2011 SciRes. SNL
Potential Application of Silica Aerogel Granules for Cleanup of Accidental Spillage of Various Organic Liquids
Copyright © 2011 SciRes. SNL
2.3. Methods of Characterization
The apparent density, % of volume shrinkage, % of po-
rosity and pore volume of the as prepared silica aerogels
were measured using following formulae [15].
% of volume shrinkage = 110
% of porosity = 11
Pore volume = 11100
where, Va and Vg are the volumes of the aerogel and al-
cogel respectively, ρs is the skeletal density (~1.9 g·cm–3)
and ρb is the apparent density.
Here, density measurements of granules were con-
ducted on the basis of mass of granules per unit volume
of cm3. Volume shrinkage of aerogels measured with
respect to alcogel volume which is assumed as 100%.
The aerogel granules were used to study absorption and
desorption capacity for different organic liquids. The
contact angle of water with surface of aerogel was meas-
ured by using the contact angle meter (Rame-Hart,
Model 500 F-1, USA). The surface chemical modifica-
tion of the aerogels was studied by using the Fourier
Transform Infrared Spectroscopy (Perkin Elmer Instru-
ments, Spectrum one, USA). The thermal stability of the
aerogel samples was characterized by TGA and DTA
analysis in the air atmosphere. The surface morphologi-
cal studies carried out by using field emission scanning
electron microscopy (FESEM). The absorption capacity
of the aerogel sample was studied by weighing the
aerogel sample by using a microbalance (10–5 g accuracy)
before absorption, immediately after absorption, and af-
ter total evaporation of the liquid from the sample.
3. Results and Discussion
3.1. Absorption Study of Organic Liquids by the
Hydrophobic Aerogels
The ambiently dried TEOS based silica aerogels possess
low density (0.062 g/cm3), high porosity (96.7%), pore
volume (15.2 cm3/g) and water contact angle (145˚).
These aerogel granules were used to study absorption
and desorption capacity for different organic liquids. The
absorption capacity of the aerogels was quantified by
measuring the difference between mass of aerogel gran-
ules before and after absorption of organic liquid. For the
present studies different, 15 organic solvents were stud-
ied which includes, viz., four alkanes, four aromatic
compounds, four alcohols, and three different kinds of oil
samples. The alkanes include hexane, heptane, octane
and cyclohexane; the aromatic compounds include ben-
zene, toluene, xylene and acetone; the alcohols include
methanol, eth anol, pro panol an d isobutanol; and th e three
oils include petrol, diesel and engine oil.
Table 1 shows the mass of various organic solvents,
alcohols and oils absorbed by unit mass of the aerogel
sample. It is observed that, the mass of iso-butanol ab-
Table 1. Mass of various organic liquid absorbed by unit mass of the aerogel sample.
Organic liquid Surface Tension (mN/m) Density of liquid (g/cm3)Calculated
Mass absorbed
q =
× V (g/g)
Mass absorbed
Hexane 18.4 0.649 10.47 10.00
Heptane 20.3 0.671 10.82 12. 00
Octane 21.62 0.694 11.20 12.50
Cyclohexane 24.95 0.799 12.89 12.84
Methanol 22.5 0.783 12.63 12.14
Ethanol 22.3 0.722 11.65 12.60
Propanol 23.78 0.795 12.83 13.65
Iso-Butanol 24.6 0.802 12.94 14.20
Benzene 29 0.868 14.00 14.52
Toluene 29 0.858 13.84 13.90
Xylene 28.9 0.870 14.04 13.58
Acetone 25.20 0.790 12.75 12.49
Petrol 26 - - 10.84
Diesel 30 - - 11.56
Engine oil 31.60 0.905 14.60 12.91
Potential Application of Silica Aerogel Granules for Cleanup of Accidental Spillage of Various Organic Liquids
sorbed was maximum (14.20 g) and methanol was
minimum (12.14 g) among the alcohols. Among the al-
kanes, the mass of cyclohexane absorbed was maximum
(12.84 g), while that of hexane absorbed was minimum
(10 g). In case of the aromatic compounds the mass of
xylene absorbed was minimum (13.58 g) and that of
benzene was maximum (14.52 g). Similarly, mass of
acetone absorbed by the aerogel granules was 12.49 g. In
oils, the mass of petrol absorbed was minimum (10.84 g)
and that of engine oil was maximum (12.91 g). The ab-
sorption capacity of the aerogel for each organic liquid
can be calculated by using the relation,
 (7)
where, q is the mass of organic liquid absorbed by the
be the density of aerogel sample and V is
the pore volume of aerogel. From table it is observed that
the calculated and experimental values of mass of or-
ganic liquid absorbed by unit mass of aerogel granules
are nearly same.
The mass of the organic liquid absorbed by an aerogel
mainly depends upon the surface chemical composition
of absorbent and surface tension of the liquid. The sur-
face modified silica alcogels possess non-polar -CH3
bonds at the ends of the SiO2 network. This can be
achieved by modifying surface with TMCS silylating
reagent, which converts its hydrophilic nature into hy-
drophobic one. The organic liquids taken in the absorp-
tion studies possess low surface tension. As per Neu-
mann’s theory of wettability [18], the material will ab-
sorb those liquids which possess low surface tension than
the surface tension of the material, which indicate that
the wettability of solid depends upon the surface tension
of the liquid used. The organic liquids possess very low
surface tension and therefore, they wet the aerogel sur-
face fully and get easily absorbed. Since the aerogels are
highly porous (96.7%), hence the liquid absorption is due
to the capillarity action. Aerogels are already proved to
be promising candidate in the field of oil spill cleanup
application [19]. Generally, aerogels are prepared by
supercritical drying of alcogels, but monolithic aerogels
possess high cost of production, therefore, attempt have
been made to prepare low cost aerogels. The absorption
capacity of ambiently dried silica aerogels shows nearly
equal as compared with the supercritically dried aerogels.
Figure 1(a) shows the photograph of beaker contains
water and engine oil and Figure 1(b) indicates that only
oil present in water is absorbed by the aerogels while
Figure 1(c) shows that the oil isolated by the aerogels
from water. It is clear that, the silica aerogel granule ab-
sorbs organic liquids around 13 to 15 times of its own
mass. Therefore, silica aerogels can be used for oil spill
cleanup applications.
Figure 1. (a) Engine oil and water in the beaker, (b) shows
that only oil present in water is absorbed by the aerogel
granules, (c) shows the separated water and oil absorbed
aerogels in beakers.
Copyright © 2011 SciRes. SNL
Potential Application of Silica Aerogel Granules for Cleanup of Accidental Spillage of Various Organic Liquids101
3.2. Desorption Rate of Organic Liquids at
Different Temperature
The time taken by the liquid for complete evaporation
from the aerogel pores starting from the moment of ab-
sorption is called desorption time. It was observed that
the organic liquids evaporate from the aerogel surface
gradually. The rate of desorptio n was estimated by meas-
uring the mass of the liquid absorbed by the aerogels at
regular time intervals till the liqu id got totally evapor ated
and the original mass of the aerogel was restored and
hence faster would be the evaporation. The variation of
surface tension of the liquid with its temperature [9], is
given by the fo l l owi n g rel a t i on,
0(1 )
 (8)
where 0
and t
are surface tension at 0˚C and t˚C,
is the temperature coefficient of surface
tension for the liquid. Figure 2 shows the desorption
time versus the temperature for petrol, propanol, benzene
and heptane. The surface tension of all the liquids de-
creases linearly with the rising temperature. It is ob-
served that as temperature increases desorption time de-
creases. It was also, observed that desorption time in-
creased from shorter chain (hexane) to the longer chain
(octane) organic liquids. This may be due to the fact that
the evaporation of liquids takes place in two stages. In
the first stage, molecules of liquid are brought from the
interior up to the surface, overcoming the surface tension
effect. During the second stage, they vaporize from the
surface depending on the vapour pressure of the liquid.
Also, the vapour pressure decreases with increase in the
chain length and molecular weight of the organic liquid.
The vapour pressure (226 mm of Hg at 25˚C) for hexane
is very high which led to faster evaporation and that for
cyclohexane is very less (24.05 mm of Hg at 25˚C), and
Figure 2. Desorption rate of TEOS based silica aerogels at
different temperatures.
hence desorption time for cyclohexane is more. As a re-
sult it would be easy for the liqu id molecules to co me out
of the aerogel pores at higher temperatures due to higher
temperature gradient. But in case of oils more time is
required to evaporate fo r oil, from the aerogels due to the
oil with low vapour pressure.
The 30% volume shrinkage and some cracks is ob-
served after absorption of organic liquid and after de-
sorption, aerogels regains approximately 80% of its
original volume observed. During the evaporation of
liquid from the pores of the aerogel it exerts a capillary
pressure on the walls of the pore and is given by the
Laplace equation [20],
the surface tension of the liquid, θ is the con-
tact angle of the liquid with the aerogel surface and r is
the radius of the pore. Since, the organic liquid fully wets
the surface,
= 0 and therefore, the capillary pressure
equation beco mes,
The surface tension of is around 20 mN/m (depending
on the liquid) and pore radius of the aerogel is order of
tens of nm, the capillary pressure is very high which is of
the order of 106 Pa. Therefore, the solvent is in tension
and it induces a compressive stress (~106 Pa) on the
aerogel network. As a result, the aerogel shrinks during
desorption. As the liquid evaporates from the aerogel
pores, gradually the inward pull reduces due to decrease
in the pressure gradient and hence the aerogel starts to
regain its size. When liquid gets evaporated fully from all
the pores, the aerogel springs back to its original shape
and size retaining all its physical and hydrophobic pro-
perties. Therefore, these ambiently dried silica aerogels
can be re-used at least for thrice.
3.3. Comparative FTIR Studies of the Aerogels
before Absorption and after Desorption
Figure 3 shows the FTIR spectrum of silica aerogels
before absorption of any organic liquid while Figure 4
shows the FTIR spectra of the silica aerogel after desorp-
tion of propanol, petrol, heptane, engine oil, and benzene
at room temperature 28˚C. The prominent peak at around
1100 cm–1 in both figures, is due to the asymmetric
bending mode of silicon dioxide. The both FTIR spectra
showed strong peaks at 845 cm–1, 1100 cm–1 and 2970
cm–1 corresponding to Si-C, Si-O-Si and C-H bonds re-
spectively. Very small peaks observed at 3400 cm–1 and
1640 cm–1 corresponds to O-H bonding which indicates
Copyright © 2011 SciRes. SNL
Potential Application of Silica Aerogel Granules for Cleanup of Accidental Spillage of Various Organic Liquids
Figure 3. FTIR spectra of silica aerogel before absorption of
solvents and oils.
Figure 4. FTIR spectra of silica aerogel after desorption of
solvents and oils.
the hydrophobic nature of the aerogels [21]. From Figure
4 it is observed that the peak intensity of C-H bon ding is
increased for petrol and engine oil as compared to the
other organic liquids. Therefore, it can be concluded that
engine oil and petrol has not been totally desorbed from
the aerogel sample.
3.4. Surface Morphological Studies of Aerogels
The field emission scanning electron microscopy (FE-
SEM) image of the two-dimensional surface morpho logy
of the retrieved silica aerogels is as shown in Figure 5.
From the FESEM it is clear that there is uniformity and
homogeneity of SiO2 particle and porous network [22].
Such uniform and homogeneous nano-structured particle
Figure 5. FESEM image of the aerogel before absorption of
oil or organic liquids.
and pores results in high absorption of the organic liquids.
From few selected areas of the material under scan
shown statistical average colloidal particle size of the
silica found around 30 to 40 nm and the po re size around
70 to 100 nm. The silylation process might be leading to
increase in pore sizes of the silica network. The surface
morphology is important as the wettability of a surface is
dependent on its chemical composition and surface to-
3.5. Thermal Stability Analysis of Silica Aerogels
Figure 6 shows the typical TGA and DTA profiles for
the TMCS modified silica aerogel sample. The notice-
able weight loss was observed at around 380˚C in TGA
curve, accompanied with an exothermic peak in the DTA
curve. The sudden weight loss at around 380˚C is due to
the decomposition of alkyl (-CH3) groups where as the
exothermic peak in DTA curve is due to the oxidation of
Figure 6. Thermo gravimetric and differential thermal
analysis (TG-DTA) of aerogels.
Copyright © 2011 SciRes. SNL
Potential Application of Silica Aerogel Granules for Cleanup of Accidental Spillage of Various Organic Liquids103
alkyl groups. It indicates that the thermal stability of
TMCS modified silica aerogels is up to 380˚C and ab ove
this temperature the aerogel will show hydrophilic nature
[23]. Hence present study reveals that the hydrophobic
aerogels are thermally stable up to 380˚C and are suitable
for their use for absorption and desorption of various
organic liquids present in water.
4. Conclusions
The ambient pressure dried TEOS based hydrophobic
silica aerogel granules were obtained by the two-step
sol–gel process using TMCS as the hydrophobic reagent
for surface chemical modification. The optimal molar
ratio of precursor chemicals TEOS:MeOH:Oxalic acid:
NH4OH:NH4F:TMCS was kept constant at 1:16.5:0.71:
0.58:0.60:0.98, respectively. The retrieved silica aerogel
granules were deployed for absorption and desorption
studies of various organic liquids. The absorption studies
reveal that the hydrophobic silica aerogel granules absorb
organic liquids approximately 13 times and different oils
nearly 12 times with respect own mass of silica aerogel
materials. The mass absorbed by aerogels were found to
be depend upon the density and surface tension of the
given organic liquids and oils. The desorption time of
aerogel decreased as temperature increased and aerogel
regains its original structure around 80% after the total
desorption of organic liquid. In case of oil samples par-
ticularly diesel and engine oil, some traces might be pre-
sent in samples and their presence has been verified from
FT-IR studies. SEM studies of aerogel shows the uniform
and homogeneous nano-structured pores results in high
uptake capacity of organic liquids due to capillarity ac-
tion. This indicates that ambiently dried silica aerogel
granules can be used to clean the organic liquids in case
of there is accidental spillage during transport of vehicles
on roads as well as accidental spillage of organic liquids
in sea water. The hydrophobic nature of aerogels can be
retained up to temperature of 380˚C as indicated by the
thermal analysis studies and hence such aerogels can
efficiently applied for potential application of absoption
and desorption of accidental spillage of organic liquids
and oils.
5. Acknowledgements
The authors are highly thankful to the Board of Research
in Nuclear Sciences (BRNS), Department of Atomic En-
ergy (DAE), Mumbai, India for the funding this work
under major research project No. 2008/37/47/BRNS/
2502 dated 28/01/2009. The authors D. B. Mahadik and
M. S. Kavale are highly grateful to the DAE-BRNS
Mumbai for the Junior Research Fellowship.
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