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www.wjpps.com │ Vol 10, Issue 11, 2021. │ ISO 9001:2015 Certified Journal │
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Fatthee et al. World Journal of Pharmacy and Pharmaceutical Sciences
STUDY OF THE PROPERTIES AND MORPHOLOGICAL
STRUCTURE OF NATURAL ZEOLITE PREPARED FROM LOCAL
CLAY RAW
Firas Emad Fatthee*1
and Omar Musa Ramadhan2
1,2
Department of Chemistry, College of Education for Pure Science, University of Mosul,
Mosul, Iraq.
ABSTRACT
This study included the use of local clay raw, which is found in large
quantities in the Al-Qasr area of Nineveh Governorate, Iraq. The study
showed that it contains many important clay minerals its rich in clay
minerals, which are Montmorillonite (10%), chlorite (4%), Kaolinite
(9%), muscovite (20%) and illite (19%) which represent more than two
thirds of the clay raw, in addition to containing small quantities with
different percentages of non-clay minerals. Chemical treatments have
also proven their ability to remove impurities from clay raw, which
reduces its effectiveness, in addition to its ability to open pores and
channels, and this has been proven in BET and SEM analyzes. Natural
zeolite prepared from clay raw, many measurements were made (TG, DTA, XRD, XRF,
BET, SEM) which proved that natural zeolite was obtained with good qualities, as it can be
used as an ion exchanger or in the various catalytic processes.
KEYWORDS: Local clay raw, Chemical treatment, Natural zeolite, Surface area, SEM.
1. INTRODUCTION
Clay minerals may be rocky, sedimentary deposits, or the result of weathering of primary
silicate minerals, Clay minerals of sedimentary origin, which mainly include the clay mineral
Kaolinite, of varying particle size and usually of low crystalline structure, on the other hand
bentonite is a rock formed by hydrothermal changes, developed and available to volcanic
materials in an aquatic environment (shallow seas, brackish lakes), Most of the sediments are
WORLD JOURNAL OF PHARMACY AND PHARMACEUTICAL SCIENCES
SJIF Impact Factor 7.632
Volume 10, Issue 11, 1813-1826 Research Article ISSN 2278 – 4357
*Corresponding Author
Firas Emad Fatthee
Department of Chemistry,
College of Education for
Pure Science, University of
Mosul, Mosul, Iraq.
Article Received on
20 Sept. 2021,
Revised on 10 October 2021,
Accepted on 30 Oct. 2021,
DOI: 10.20959/wjpps202111-20551
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Fatthee et al. World Journal of Pharmacy and Pharmaceutical Sciences
rich in montmorillonite, and because of their diversity and composition, the catalytic activity
of natural clay materials varies according to their structural properties (Benny K.G. T. 2019).
The term „„clay” applies to the materials having a particle size of less than 2 µm, and also to
the family of minerals having similar chemical compositions and common crystal structural
characteristics (Velde, B., (1995). Clay has a variety of physical characteristics such as
plasticity, shrinkage under fire and under air-drying, fineness of grain, colour after firing,
hardness, cohesion, and capacity of the surface to take decoration (Odoma, A.N., & etal
(2013). Clays are hydrous aluminosilicates which composed of mixtures of finegrained clay
minerals, crystals of other minerals, and metal oxides (Mockovciakova, A., and Orolinova,
Z., (2009). On the basis of such qualities, clays are variously divided into classes or groups
such as smectites (montmorillonite, saponite), mica (illite), kaolinite, vermiculite, serpentine,
pyrophyllite (talc) and sepiolite etc (Shichi, T. and Takagi, K. (2000).
Clays and clay minerals have small particle size and complex porous structure with high
specific surface area, which allows strong physical, chemical interactions with dissolved
species. These interactions are due to the electrostatic repulsion, crystallinity, and adsorption
or specific cation exchange reactions. The highly porous surface area that possesses attractive
force suggests that the bonding power will also be high (Grim, R.E., (1962).
Zeolites are crystalline aluminosilicates with physical and chemical properties, including the
loss and absorption of water and other molecules. In addition, they act as molecular sieves
and replace their constituent cations without any change in their structural composition. The
unique and distinct physical and chemical properties of zeolites make them extremely useful
in many diverse applications. Including agricultural engineering, environment, manufacturing
and industrial processes (Hardi, GW, & etal 2020)
Zeolite is a hydrated quaternary alumina silica porous crystalline mineral with a three-
dimensional skeleton, Composed of [SiO4]-4
and [AlO4]-5
tetrahedrons (Stanislav, T., & etal,
2014) These two types are bonded to each other by oxygen atoms in this way which form an
open three-dimensional framework containing channels and cavities filled with metal ions
(usually alkaline or alkaline earth metals) and freely moving water molecules (Cheetam, D.
2014)
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Fatthee et al. World Journal of Pharmacy and Pharmaceutical Sciences
Swedish mineralogist named Axel Fredrik Cronstedt in 1756 was the first to discover zeolite
and gave it this name. The word zeolite is composed of two Greek words “zeo” = boil &
“lithos” = stone meaning boiling stone through heating minerals, as the water is removed
when heated (Gottardi, G and Galli, E. 1985)
The general chemical formula for natural zeolite is
zeolites have attracted a great deal of interest among researchers and scientists due to their
flexibility and adaptability, after their discovery in 1756 by Axel Fredrik Cronstedt.
Especially widely used in industry. Zeolites have been used in the separation of straight-chain
hydrocarbons from branched-chain hydrocarbons, chemical sensors in industrial process
control, environmental and indoor air quality monitoring, effluent and automatic exhaust
control, medical monitoring, air separation and heavy metal removal.
Zeolite was first used as an adsorbent in 1777 by Fontana and Shell, due to its sorption
properties as it was applied in a variety of processes used to solve environmental problems.
Later, zeolites were used as good absorbent materials for particles such as H2O, NH3, H2S,
NO, NO2, SO2, and CO2 (Moshoeshoe, M., & et al 2017).
They are used as substitutes for phosphates in laundry detergents, as absorbents for
purification and separation of materials, and as catalysts. Total global consumption of zeolite
is estimated at 5 x 106 tons/year, including about 1.8 x 10
6 tons of synthetic zeolite and 2.9 x
106 tons of natural zeolite (2008) and that the main application areas of zeolites are as
adsorbents, catalysts and ion exchange materials (Hagen, J. 2015)
2. Experimental Part
2.1 Choosing of raw clay
The clay used in our study was obtained from the village of Al-Qasr located in Al-
Hamdaniya district of Nineveh Governorate, 100 gm of clay raw is placed in a manual mortar
for the purpose of preparing the clay raw and in order to prevent or reduce the effect of
crystalline structures on the heat resulting from the grinding process, add 10 cm3 of ethanol to
the clay raw during the grinding process and after each grinding process, the ore is sifted
using a sieve (300 mesh) periodically so that the ground ore is not subjected to further
grinding and then dried in an electric oven for (6-8) hours at a temperature of 130 ° C and
then kept for a purpose Study by Thermogravimetric analysis (TG) differential thermal
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analysis (DTA) X-ray diffraction(XRD) and X-ray fluorescence (XRF) (Pansu, M. and
Gautheyrou, J. (2006), Ghazal, R. Y. (2001)
2.2 Chemical treatment of clay raw to get a natural zeolite
The carbonate is initially removed from the clay raw by treating it with hydrochloric acid
(10%) with heating for three hours (Carver, RE, (1976). And then, the iron is removed by
treating the clay raw with a solution of (0.15M H2C2O4) In the presence of (0.5M H2SO4) and
heating to a temperature of 100°C and stirring the mixture using a magnetic stirrer for 90
minutes (Carver, RE, (1976), (Toro, L., and Veglio, F., (1994), as for the amorphous silica is
removed by treating crude clay with a solution (0.5 M NaOH) with heating for five hours and
then filtered, washed well with distilled water and then dried using an electric oven at a
temperature (130°C) and dried, and after these treatments we get Nature Zeolite (NZ) and
kept it in sealed bottles for the purpose of measurements on them by Thermogravimetric
analysis (TG) differential thermal analysis (DTA), X-ray diffraction(XRD) X-ray
fluorescence (XRF), BET Technique and scanning electron microscopic (SEM) .
3. RESULTS AND DISCUSSION
For the purpose of identifying the components of clay raw from clay minerals and non-clay
minerals, it was studied by X-ray diffraction (Figure 1), as it was found by analyzing the
diffraction patterns of clay ore that it consists of Montmorillonite, Chlorite, Kaolinite,
Calcite, Hematite, Quartz and Gypsum, in addition to muscovite and Illite that were
diagnosed. In the clay raw in this study by (X,Pert High Score Plus) the values of [°2Th.] and
atomic distances d-spacing [Å] measured in can be observed as shown in Table (1).
Table (1): Shows the values of atomic distances d-spacing [Å] and angles [° 2Th.] of the
local clay raw.
No. [°2Th.] d-spacing [Å] Intensity No. [°2Th.] d-spacing [Å] Intensity
1 5.105039 17.31076 13.90369 15 39.65368 2.27295 219.7622
2 6.0607 14.58315 87.94697 16 42.70146 2.11752 28.99203
3 8.905255 9.9303 47.41321 17 43.40119 2.08499 118.9994
4 12.38128 7.1491 19.64136 18 47.77308 1.90389 127.6286
5 19.96729 4.44685 158.9125 19 48.74387 1.86822 159.9247
6 21.08227 4.21412 101.0263 20 50.31783 1.81341 39.8764
7 23.29723 3.81824 85.07286 21 56.81545 1.62049 18.36637
8 24.52859 3.62928 48.51737 22 57.59005 1.60052 60.14033
9 26.87501 3.3175 521.9465 23 60.27626 1.53547 43.67696
10 27.97613 3.18938 62.66291 24 61.82385 1.5007 51.89584
11 29.6653 3.01151 904.6009 25 64.83923 1.438 45.35107
12 35.19212 2.5502 98.09603 26 65.87627 1.41786 33.42675
13 36.1873 2.48232 153.8002 27 68.45914 1.37053 32.00934
14 37.44958 2.4015 41.20396 28 73.02008 1.29577 27.77394
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Figure (1) shows the X-ray diffraction of local clay raw.
After studying the X-ray diffraction patterns of clay minerals and non-clay minerals their
percentages were calculated as shown in the table (2).
Table (2): Show the Percentage Ratio of clay minerals and non-clay minerals of raw
clay.
Clay and Non
Clay Minerals Percentage Ratio %
Montmorillonite 10%
Chlorite 4%
Muscovite 20%
Kaolinite 9%
Gypsum 12%
Ittite 19%
Quartz 6%
Calcite 13%
Hematite 7%
It appears from the table (2) that the local clay raw is rich in clay minerals, which are
Montmorillonite (10%), chlorite (4%), Kaolinite (9%), Muscovite (20%) and Illite (19%)
which represent more than two thirds of the clay raw in addition to containing small
quantities with different percentages of non-clay minerals.
Table (3) shows the percentages of local clay raw components in the form of oxides obtained
from XRF analysis in comparison with different natural clay minerals (Talaat, H.A., & etal
(2011) (Nayak, P.S. and Singh, B.K., (2007) (Njoku, V.O., & et al (2011) (Bosco, S.M.D., &
et al (2006) (Villegas, R.A.S., & et al (2005).
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Table (3): Shows XRF analysis in comparison with different natural clay minerals.
Natural clays Metal Oxide (weight %)
SiO2 Al2O3 Fe2O3 CaO Na2O K2O MgO MnO TiO2
Local clay raw 44.012 9.494 6.754 13.551 0.675 1.495 7.244 0.055 0.491
Egyptian clay 50.65 30.31 4.61 0.27 0.16 --- 0.20 --- 1.65
Indian clay 48.12 43.54 2.48 0.83 --- --- 0.50 --- 0.40
Nigerian clay 48.62 34.82 2.88 0.10 0.06 0.94 0.23 --- 0.01
Tunisia clay 52.50 18.20 3.00 2.81 1.78 1.50 2.45 --- ---
China clay 46.22 38.40 0.68 0.86 --- --- 0.37 --- ---
Brazilian clay 59.57 22.28 11.31 0.72 0.01 2.83 2.83 ---- 1.03
In order to know the thermal stability of the raw, the heating ranges, the amount of adsorbed
water and the water contained within the channels, as well as when the calcination process
occurs, as we can identify what the clay raw contains of water particles and its types, in
addition to the possibility of identifying the minerals calcite and dolomite, which consist
mainly of carbonates and bicarbonates, As clay ores begin to lose crystallization water
molecules at a temperature of (120-110)˚C and at a temperature of (250)˚C, these raw
materials lose all water molecules within the structural channels, but when the temperature is
raised to (360-350)˚C These ores lose the hydroxyl groups present within their structures in
the form of water molecules, as all two hydroxyl groups (-OH) turn into a water molecule
(H2O) and leave one oxygen atom bound within the crystal structure of these raw materials,
and the calcination process for carbonates begins at a temperature of (450)˚C as it loses
carbon dioxide (CO2) and works to convert the elements associated with it into an oxide
form, and this process continues to a temperature of (700)˚C approximately (Brobely, GP,
2007), and Figure (2) shows TG and TG analysis DTA for clay raw.
Figure (2) shows TG and DTA of clay raw.
Natural zeolite is multi-mineral and contains many impurities, which are mostly quartz,
feldspar and hematite, and the presence of these impurities makes it impossible to use it in
industrial processes, so most types of natural zeolite are useless (Akolekar, D., & et al 1997).
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Clay crude was taken and grinded well, then some chemical treatments were carried out for
the purpose of removing ineffective components that reduce the catalytic activity and thus be
useless. At first, the moisture content was measured, which amounted to 4%, and then the
clay raw was treated with hydrochloric acid for the purpose of removing carbonates. Because
its presence has a negative effect on the catalyst preparation process, as the carbonate
removed amounted to 18.125%. After that, the clay raw was treated with (0.15M H2C2O4)
and (0.5M H2SO4) for the purpose of removing iron, as the percentage of iron removed was
11%, and then the clay raw was treated with a solution of (0.5 M) sodium hydroxide for the
purpose of removing amorphous silica. It reached 15.9% and after removing all the
ineffective components of carbonate, iron and amorphous silica, the natural zeolite was
obtained.
From the application of TG natural zeolites, it gives us a clear idea of the amount of adsorbed
water present on the surface or inside the pores or channels. The adsorbent water and
hydroxyl groups (-OH) gradually and successively within a range of temperatures ranging
between (100-400°C), and this loss applies to most types of zeolites, as it is clear from Figure
(3) that the natural zeolite when heated from (100-130 ˚C) loses (1.8-3.2%) of its weight and
the reason for this is the loss of water of crystallization and when the temperature is raised to
(230-260˚C) loses (5.1-5.3%) of its weight due to the loss of water molecules within the
internal channels of the catalyst, and when heating continues to (300-360 ˚C), we notice that
the loss (5.8-6%) of its weight is due to the loss of the remnants of water molecules present
within the pores and channels, in addition to the loss of hydroxyl groups located Within the
structure of the catalyst in the form of water molecules, the process of heat raising and weight
loss continues to a temperature of 700 °C (Brobely, GP, 2007). The measurements showed
that the processes of losses at different temperatures are endothermic.
Figure (3) shows TG and DTA of natural zeolite.
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In order to identify the contents of natural zeolite from clay minerals and non-clay minerals,
it was studied by X-ray diffraction. Figure (4) It was found by analyzing the diffraction
patterns of the clay raw that it consists of Montmorillonite and kaolin in addition to
Muscovite and Illite with percentages of more than (70%) and low percentages of each of
Hematite, Quartz and Gypsum. The values of [°2Th.] and atomic distances d-spacing [Å]
measured of the diffraction patterns of each of the minerals diagnosed in the natural zeolites
prepared in this study can be observed by (X,Pert High Score Plus) program and the
percentages ratio of each mineral in Table (4) and Table (5) respectively.
Figure (4) shows the X-ray diffraction of natural zeolite.
Table (4): Shows the values of atomic distances d-spacing [Å] and angles [° 2Th.] of the
Natural zeolite.
Intensity d-spacing [Å] [°2Th.]
43.000940 9.95767 8.880729
15.266430 7.01536 12.618270
179.646900 4.42438 20.069730
188.108900 4.19677 21.170450
929.762100 3.30897 26.945590
100.710700 3.20084 27.874010
105.366400 3.00670 29.713870
112.882800 2.57753 34.807070
100.737600 2.43850 36.860690
71.708950 2.11823 42.686330
27.628740 1.97595 45.928870
130.894100 1.81028 50.410870
31.226250 1.66354 55.217680
95.589400 1.53746 60.189930
67.180880 1.49956 61.875780
63.257340 1.36981 68.499970
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Table (5): Show the Percentage Ratio of clay minerals and non-clay minerals for
Natural zeolite.
Clay and Non
Clay Minerals Percentage Ratio %
Montmorillonite 14%
Muscovite 26%
Kaolinite 13%
Gypsum 9%
Ittite 20%
Quartz 12%
Hematite 8%
In order to identify the percentages of the components of the prepared natural zeolite and the
rest of the prepared catalysts, which are in the form of oxides, by measuring fluorescent X-
rays, as we note from the Table (6) shows that the proportions of the elements included in the
composition of natural zeolite, which are in the form of oxides, consist of silica SiO2 with a
percentage of (49.174%) and alumina with a percentage of (9.75%) with the presence of
different percentages of sodium oxide Na2O, potassium oxide K2O, calcium oxide CaO and
oxide Magnesium MgO, which is present in the structural interface of zeolite in the form of
exchangeable ions (Ma+2
, Ca+2
, Na+1
, K+1
) With the presence of some impurities that cannot
be removed under the conditions of the study (Ugal, J.R., & et al., (2010).
Table (6): Shows XRF analysis of Natural zeolite.
Sample Metal Oxide (weight %)
SiO2 Al2O3 Fe2O3 CaO Na2O K2O MgO MnO TiO2
Natural zeolite 49.174 9.752 7.281 0.961 0.479 1.774 5.224 0.029 0.78
The BET method is one of the traditional methods that has a clear advantage in facilitating
analyzes, calculating the surface area, and evaluating the size of pores and channels (Naito,
M., & etal 2018). This technique relies on the use of nitrogen gas N2, as it is possible to use
other gases such as CO2, Ar and water However, nitrogen has a boiling point of (77˚K, -
195.79˚C), (Toth, J., (2001). The results showed that the natural zeolite possess a large pore
size and a good surface area Table (7) Figure (5) which enables its to carry out the catalytic
action through The adsorption of the reactants on the outside surface or inside the pores and
channels, and the required reaction occurs, followed by the desorption of the resulting
material molecules, which gives them good selectivity towards the catalytic reactions.
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Table (7): Shows the results of the BET analysis of the prepared natural zeolite sample.
Analysis Data Measurements
88.2760 m²/g BET Surface Area
553.8514 m²/g Langmuir Surface Area
0.1868 cm³/g Pore Volume
6.556405 nm Pore Size
-B-
-A-
-D-
-C-
Figure (5) (A) surface area by BET method, (B) surface area by Langmuir method, (C)
represents the pore volume in the case of adsorption and (D) represents the pore volume
in the case of desorption of the prepared natural zeolite.
The scanning electron microscope technique is one of the types of electron microscopes that
produces an image of the sample by scanning it with a focused beam of electrons that interact
with the atoms in the sample, which results in different signals containing information about
the topography and composition of the sample (McMullan, D., (1998) in addition to the
spectroscopic analysis in which the elemental composition of the model appears, the analysis
may be carried out. Figure (6) represents the spectroscopic analysis of the elemental
components of natural zeolite.
The natural zeolite prepared by this technique was measured, as the measurement showed
that it consists of grains of different irregular shapes, and some of these grains have formed
aggregated with each other grains of larger size. Zeolite has good specifications and
properties, and the size of these grains ranges between (32.17 nm to 87.78 nm), and this gives
us an indication of the good specifications of this zeolite Figure (7).
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Fatthee et al. World Journal of Pharmacy and Pharmaceutical Sciences
Figure (6) Spectral analysis showing the elemental composition of natural zeolite.
-B-
-A-
-D-
-C-
Figure (7) SEM image of natural zeolite (A = 1µm B = 2µm C = 500 nm D = 200 nm)
4. CONCLUSION
This study shows that the local clay ore has many important characteristics, including its
availability in large quantities, in addition to containing many clay minerals, The chemical
treatments conducted on the local clay raw led to the removal of impurities and opening
channels and pores The XRF analysis shows presence of different percentages of sodium
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Fatthee et al. World Journal of Pharmacy and Pharmaceutical Sciences
oxide Na2O, potassium oxide K2O, calcium oxide CaO and oxide Magnesium MgO, which is
present in the structural interface of zeolite in the form of exchangeable ions (Ma+2
, Ca+2
,
Na+1
, K+1
) The BET analysis results showed that the natural zeolite possess a large pore size
and a good surface area and SEM analysis showed crystalline nature.
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