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DOI 10.1007/s12633-016-9531-8
ORIGINAL PAPER
Preparation and Characterization of Precipitated Silica
using Sodium Silicate Prepared from Saudi Arabian Desert
Sand
Riyas Sharafudeen1 · Jihad Mohammed Al-Hashim1 · Mohammed Olian Al-Harbi1 ·
Ahmed Ibrahim Al-Ajwad1 · Ali Abdulaziz Al-Waheed1
Received: 25 June 2016 / Accepted: 21 November 2016
© Springer Science+Business Media Dordrecht 2017
Abstract The present study reveals a cost benefit process
in an open system for utilizing desert sand for prepar-
ing sodium silicate or precipitated silica. A simple alkali
fusion method has been developed to prepare sodium sili-
cate directly from sand and finally pure precipitated silica
by acid precipitation. The reaction weight ratio of alkali
to sand reaction parameters are studied for optimizing the
silica yield. About 80% pure precipitated silica has been
prepared in an open system at 150 ◦ C within 45 min. Wet
chemical methods, FTIR, TG-DTA, XRD and SEM tech-
niques are used to characterize the silica prepared from sand
available in Saudi Arabian deserts. In the XRD pattern, the
peak corresponding to silica was obtained at the diffraction
angle of 21.8◦ and it was found to be amorphous in nature.
Keywords Sand · Alkali fusion · Sodium silicate ·
Precipitated silica
1 Introduction
The most common raw material for electronic grade silica is
high purity quartz rock and beach sand is largely quartz. Sil-
ica is the dioxide form of silicon (SiO2 ) and occurs naturally
 Riyas Sharafudeen
riyaschem@rediffmail.com
1 Department of Chemical and Process Engineering
Technology, Jubail Industrial College, P.O Box 10099,
Jubail Industrial City 31961, Saudi Arabia
in the form of quartz and is a functional material that is
used to improve surfaces and mechanical properties of many
materials [1]. Technologies related to the production method
and applications of pure precipitated silica have been
studied and developed throughout the world in different
pathways.
Music et al. have reported that amorphous silica can be
precipitated from a commercial aqueous solution of sodium
silicate and the work has be used for further academic inves-
tigations, and also as a valuable commercial product [2].
Commercially available precipitated silica is manufactured
by the fusion of high purity caustic soda and silica sand
in furnaces at temperatures of 1300-1500 ◦ C and higher
to produce solid glass [3]. Tetraethylorthosilicate (TEOS)
is also widely used for production of commercial silica.
But these processes are very expensive and energy intensive
[4]. Recently, a large amount of precipitated silica has been
extracted from various types of bio-waste such as rice husk
ash [5], rice hull ash [6] and bagasse ash [7] etc. Several
techniques such as acid leaching or by gasification of rice
hull with a pilot flame in a modified fluidized bed as well as
by burning the rice hull ash at high temperature have been
reported for the extraction of silica [8, 9].
Sodium silicate (Na2 SiO3 ) is formed by melting sand
and sodium carbonate (soda ash). The industrial name of it
is waterglass. Soluble sodium silicates (or waterglass) are
solutions of water and soluble glasses manufactured from
varied proportions of Na2 CO3 and SiO2 . Sodium silicates
contain three components: silica–primary constituent, alkali
- sodium oxide and water. Hydrous and anhydrous proper-
ties of these components provide the end-user with varied
uses and applications associated with one or more of these
elements. Sodium silicates are silicate polymers. The higher

the degree of polymerization the greater the proportion of
oxygen shared between [SiO4 ]2− tetrahedra and hence the
smaller the Na2 O:SiO2 ratio. A range of different SiO2 and
Na2 O polymers can exist. Hence it is one of the important
determinants of the properties and functional activity of a
particular type of sodium silicate [10].
It is extensively used in the manufacturing of detergents,
silica gel, cardboard, paper, textiles, paints, adhesives, pot-
tery, sanitary ware, refractories, foundry and wood process-
ing industries because of its very good binding, adhesive,
bleaching and sizing properties. It is also used as an elec-
trolyte in keeping fine particles in suspension (in water)
without allowing them to settle. Sodium silicate is one of
the binders that is commonly used in self-setting sands. It
is equally well applicable in loose and liquid self-setting
sands, sometimes also in liquid self-setting sands for the
investment casting process. Hardeners for these sands can
be materials in either solid (e.g. CaO, SiO, CaC2 ) or liquid
form (e.g. esters of acidic acid) [10].
Silica gel is an adsorbent prepared from the coagula-
tion of a colloidal solution of silicic acid. The term silica
denotes the compound silicon dioxide and encompasses its
various forms including crystalline silicas, vitreous silicas
and amorphous silicas. The term “Gel” merely indicates the
condition of the material at one stage of its manufacture.
It is a highly porous structure, characterized by uniformity
of the arrangement of the pores and their sizes. The pore
area of silica gel varies with the method of manufacture.
Silica gel is widely used as a desiccant. Its role as a cata-
lyst support, as a flatting agent in coatings and as a selective
adsorbent in column chromatography is well established. It
Fig. 1 Sodium silicate
formation during the reaction of
sand with sodium hydroxide in
the ratio of 2.5 at different
temperature and time
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has application in modification of viscosities and thixotropy
of liquids. Silica gel may also be used for the waste water
treatment, atmospheric moisture control, purification of
gases and for petroleum refining [3].
In the present study, it was decided to prepare and ana-
lyze sodium silicate through an open system reaction using
sodium hydroxide directly from Saudi Arabian desert sand
at different temperatures. The silica was precipitated from
the sodium silicate prepared. The results obtained in the
study are reported in this paper.
2 Experimental
The raw material used in this study was the desert sand col-
lected from the eastern province of Saudi Arabia, Al-Ahsa.
Sodium hydroxide (Panreac) and sulfuric acid (alpha-98%)
along with common laboratory glassware were also used in
the study.
2.1 Sodium Silicate Preparation from Sand
The sand collected was first washed with water to remove
any suspended and soluble impurities. After washing, the
sample was dried in an air oven at 110 ◦ C for 3 hours. The
dried sand was ground using a mortar and pestle and then
separated using U.S.A Standard Testing Sieves into differ-
ent sizes such as 850, 600 and 425 microns. The reaction
with sodium hydroxide was performed with sand of each
particle size at different weight ratios of 1.5, 2.0 and 2.5 as
per the following procedure.
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used for quantitative chemical analysis by titrating using

standardized sulfuric acid.

2.2 Preparation of Precipitated Silica from Sodium

Silicate

The filtrate collected from the above procedure was ana-

lyzed for silicate content by wet chemical methods and the
silica was precipitated by treating with 2M sulfuric acid.
The precipitated silica was then filtered using suction filtra-
tion and dried in an air oven at 110 ◦ C for 3 hrs. The dried
silica was then ground well and analyzed using FTIR, XRD
and SEM analysis. The results obtained are discussed in the
Fig. 2 Precipitated silica obtained at neutral pH
following sections.

2.3 Instrumentation Used for Characterization

10 g of sand was weighed into a 250 mL Pyrex glass.
The required amount of sodium hydroxide according to the
weight ratio was weighed out and directly reacted with sand.
The above mixture was heated at different temperatures of
80, 100 and 120 ◦ C with magnetic stirring at 100 rpm for
different times of 30, 40, 50 and 60 minutes. After the reac-
tion time, the mixture was leached with distilled water and
the residue was removed by filtration and washed with hot
water. The residue was then dried and weighed for cal-
culating the % conversion. The filtrate was collected and
The X-ray powder diffaction patterns were analyzed using
a bench-top X-ray diffraction (XRD) instrument (Rigaku,
U.S.A).
The FTIR spectrum was obtained using a Nicolet 8700
FTIR spectrometer (Thermo Scientific), the transmission
was measured in the mid-IR region of 400 - 4000 cm−1 .
pH values were measured with a 3510 Bench-Top
pH Meter from Jenway with a working range up to
pH ∼14.

Fig. 3 TG-DTA curve for 10.00

precipitated silica prepared from 10.00
sand
38.2Cel
9.65mg
5.00
9.50
301.1Cel
0.00 -0.14uV

947.3Cel
-3.36uV
9.00
Heat flow uV

-5.00

TG mg
-10.00
605.6Cel
-8.82uV
8.50

-15.00
371.9Cel
8.14mg

-20.00 67.2Cel
8.00
-18.85uV

866.4Cel
-25.00 7.71mg

7.50
-30.00
100.0 200.0 300.0 400.0 500.0 600.0 700.0 800.0 900.0
Temp Cel

Fig. 4 FTIR spectrum of precipitated silica prepared from sand
Thermal analyses were performed using the high per-
formance simultaneous Differential Thermal Analyzer
(TGA/DSC) Q600 with alumina as the reference material.
Scanning Electron Microscopic studies were performed
using a J.S.M.-5600 instrument by placing the sonicated
sample dispersion in acetone on a copper stud, drying in air
and made conducting by gold (99%) sputtering.
3 Results and Discussion
The quantitative analysis of sodium silicate samples pre-
pared revealed that the reaction of sand with sodium hydrox-
ide in the ratio of 1.5 and 2.0 sodium silicate formation was
very low compared to the ratio of 2.5. The sodium hydroxide
may be the limiting reactant in the 1.5 and 2.0 ratios hence
the reaction of sand with sodium hydroxide requires excess
Fig. 5 XRD pattern of
precipitated silica prepared from
sand
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sodium hydroxide for the higher yield of sodium silicate.
The conversion of sand to sodium silicate is also dependent
on reaction time. At 60 minutes, the reaction was found to
be almost complete. The precipitation of silica depends on
factors such as duration of precipitation, the addition rate
of acid, the temperature of precipitation, concentration and
pH [11]. The reaction of sand with sodium hydroxide in the
ratio of 2.5 at 120 ◦ C for 60 minutes has produced higher
yield of the sodium silicate. Figure 1 shows the sodium
silicate formation during the reaction of sand with sodium
hydroxide at different temperature and time.
It is evident from the figure that reaction at 120 ◦ C for
60 minutes has produced about 80% of sodium silicate.
The composition of sodium silicate formed was analyzed
by titration. 20 mL of sodium silicate sample consumed 4.9
mL of 2M sulfuric acid. The composition ratio of sodium
oxide in the sample was calculated to be 0.60, which is very
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Fig. 6 SEM micrographs of
precipitated silica prepared from
sand
close to the composition of sodium oxide in the sodium sil-
icate. Hence the quantitative analysis reveals the formation
of sodium silicate by reaction of Saudi Arabian desert sand
with sodium hydroxide in the ratio of 2.5. At about neutral
pH (between 6.5 to 7.5), the addition of sulfuric acid results
in the precipitation of silica in a gel-like mass as shown in
Fig. 2. The gel was then broken with stirring with water and
filtered and weighed for its conversion.
Thermogravimetric analysis results of the precipitated
silica sample showed in Fig. 3 reveals that between 300 to
600 ◦ C, the amorphous silica transforms to crystalline silica.
It is also supported by the endothermic peaks in the DTA
studies in the same temperature range. The mass loss in the
thermogram and endothermic peak observed below 100 ◦ C
is due to the loss of both bound and free water of hydration
from the precipitated silica.
The FTIR spectrum of precipitated silica prepared from
sodium silicate is shown in Fig. 4.
In the fingerprint region, the spectrum shows a broad
and intense band around 1095 cm−1 , characteristic of the
anti-symmetric stretching vibration of the Si-O-Si and a
less intense band between 835 to 801 cm−1 is due to Si-O-
Si symmetric stretching vibrations. These are characteristic
strong bands for silica and there are peaks around 3460
cm−1 and 1637 cm−1 which may also be bands due to
associated water molecules, the bound water which is not
removed during the oven heating in the precipitated silica.
The water in the silica lattice often gives rise to sharp bands
from Si-OH bond formation through intramolecular hydro-
gen bonding. From the above discussion it is clear that silica
was precipitated from sand.
The XRD pattern of precipitated silica shown in Fig. 5
reveals the amorphous nature of the silica. There are dif-
fused peaks corresponding to the [111], [220] and [311]
planes of silica. A broad diffused peak appearing about
2θ = 23.2◦ indicates the formation of silicon dioxide in the
amorphous form.
Scanning electron micrographs of precipitated silica are
shown in Fig. 6. It is clear from the micrographs that the
particles are highly agglomerated and spherical shaped and
appear porous in nature. The water in the silica lattice has
formed the Si-OH bond through intramolecular hydrogen
bonding as supported by the XRD studies.
4 Conclusions
The sand from Al-Ahsa, eastern region of Saudi Arabia
when reacted with sodium hydroxide in different ratios to
the sand, the ratio of 2.5 of sand to sodium hydroxide
has produced sodium silicate in good yield. The following
conclusions are made from this study:
Sodium silicate can be produced using the Saudi Ara-
bian sand by reacting with sodium hydroxide directly in
open systems. The reaction between sand and sodium sili-
cate depends on the ratio of sand to sodium hydroxide, the
reaction time and temperature of reaction. The optimum
condition for the higher yield of silicate is 120 ◦ C for 60 minutes.
Precipitated silica can be made from the silicate at neutral
pH.
Acknowledgments This work was done as part of the Industrial
Chemistry Technology curriculum student project in Jubail Industrial
College. We express our thankfulness to the management of Jubail
Industrial College for the valuable support in successful completion of
the project. We would also express our gratitude to CSIR laboratory
Trivandrum for providing analytical information.
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