National Engineering School of Sfax

Department of Geolgy

AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL

APPLICATION

Internship Report

Released by :

 Yossra Hannachi

Under the supervision of :

 Ali Sdiri
 Elturki Saifeddine
Academic year :

2018/2019
AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

Table of contents

I. Intoduction....................................................................................................................................4
II. Generality about clays ..................................................................................................................4
A. Crystallographic structure .........................................................................................................4
B. Classification of clay minerals....................................................................................................5
1. 1:1 Clay Minerals....................................................................................................................5
2. 1:2 Clay minerals....................................................................................................................5
3. 2 :1 :1 clay minerals...............................................................................................................6
III. Geological context of Tunisia clays............................................................................................6
A. Geological presentation of the studied deposit........................................................................7
B. Lithological description of “Aleg” formation.............................................................................8
IV. Raw materials and techniques used..........................................................................................8
A. Raw materials............................................................................................................................8
B. experimental techniques for characterization..........................................................................9
1. mineralogical identification...................................................................................................9
2. Determination of pH............................................................................................................11
3. Determination of electrical conductivity.............................................................................11
4. Calcimetry............................................................................................................................11
5. total surface area.................................................................................................................12
6. measuring of the water content..........................................................................................13
7. Loss on ignition....................................................................................................................13
8. cation exchange capacity.....................................................................................................13
9. Infrared spectroscopy..........................................................................................................14
10. Purification of clays..........................................................................................................14
11. Laser granulometry..........................................................................................................15
V. PRESENTATION OF GEOPOLYMERS.............................................................................................16
A. Definition.................................................................................................................................16
B. Chemical structure...................................................................................................................17
C. Mechanism of geopolymerization...........................................................................................18

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

LIST OF FIGURES
Page
Fig. 1 : Deposit of J.Aïdoui 8

Fig. 2 : Localisation map of the studied clays ; ‘A:Aidoudi’ (E.Fakhfakh et al. 2005) 9

Fig. 3 : Sampling site (El Hamma ) 10

Fig. 4 : sampling site (Douiret) 10

Fig. 5 : centrifuge 16

Fig. 6 : laser granulometry apparatus 17

Fig. 7 : Diffractogram of a sodium-based geopolymer (Provis et al. 2005) 18

Fig. 8 : Coordination of silicon centers described by the rating, Engelhardt et al. (1987) 18

Fig. 9: Model of an aluminosilicate-based inorganic polymer based on the model of

Barbosa et al. (2000) supplemented by new elements, proposed by Rowles et al. (2007) 19

Fig. 10 : Mechanism of electropolymerization proposed by Duxson et al. (2007) 20

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

List of tables

Page
Tab. 1: The measured pH value 12

Tab. 2: The measured conductivity value 12

Tab. 3: The measured total limestone value 12

Tab. 4: Value of specific surface measured 13

Tab. 5: Value of water content measured 14

Tab. 6: Value of loss on ignition measured 14

Tab. 7: Measured cation exchange capacity 15

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

I. Intoduction

The perception of this internship fit with the enormous scientific researches, having as
paramount topic: clays and their miscellaneous fields of use.

Clays stem their interest from their specific properties such as plasticity, adsorbing, and
catalytic properties, they are used in many industries (oil and gas, chemistry, pharmacy,
refractory technology, ceramics ect,…).

For this reason, I carried out this internship within the institute of arid regions (regional
direction of Gabes) during the period : 15/06/2019 until 15/07/219.

It was a great opportunity to reinforce my academic training by assisting the workflow in the
laboratory and handling many operations ( depending on the availability of devices and
products ) to characterize physically and chemically 2 types of samples.

The present bibliographic research and experimental procedures are aimed to characterize,
physically and chemically :

Clays from Aleg formation (Coniacien-Santonian),[1], at Jebel Aidoudi (AYD),

located in ‘El Hamma’.

Clays with a lower Aptien age [2] which belong to Douiret formation (DRT),
In ‘Tataouin’.

II. Generality about clays :

A. Crystallographic structure :

The atomic structure of the clay minerals consists of two basic units, an octahedral sheet and a
tetrahedral sheet [3].

The octahedral sheet is comprised of closely packed oxygens and hydroxyls in which
aluminum, iron, and magnesium atoms are arranged in octahedral coordination . When
aluminum with a positive valence of three is the cation present in the octahedral sheet, only
two-thirds of the possible positions are filled in order to balance the charges.

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

When only two-thirds of the positions are filled, the mineral is termed dioctahedral. When
magnesium with a positive charge of two is present, all three positions are filled to balance the
structure and the mineral is termed trioctahedral. The second structural unit is the silica
tetrahedral layer in which the silicon atom is equidistant from four oxygens or possibly
hydroxls arranged in the form of a tetrahedron with the silicon atom in the center [3].

These tetrahedrons are arranged to form a hexagonal network repeated infinitely in two
horizontal directions to form what is called the silica tetrahedral sheet.

The silica tetrahedral sheet and the octahedral sheet are joined by sharing the apical oxygens
or hydroxyls to form what is termed the 1:1 clay mineral layer (e.g. kaolinite) or the 2:1 clay
mineral layer (e.g. illite) as discussed in the following sections. The structure and composition
of the major industrial clays,( e.g. kaolins, smectites, and palygorskite–sepiolite), are very
different even though they are each comprised of octahedral and tetrahedral sheets as their
basic building blocks.

B. Classification of clay minerals

1. 1:1 Clay Minerals

The 1:1 layer minerals contain one tetrahedral and one octahedral sheet in their basic
structural unit. This two-sheet mineral type is represented by the kaolin group : kaolinite,
dickite, nacrite, and halloysite [4].

They are combined to form a unit in which the tips of the silica tetrahedrons are joined with
the octahedral sheet. All of the apical oxygens of the silica tetrahedrons point in the same
direction so that these oxygens and/or hydroxyls,[4] which may be present to balance the
charges, are shared by the silicons in the tetrahedral sheet and the aluminum in the octahedral
sheet.

2. 1:2 Clay minerals

The joining of two tetrahedral sheets (one from each side) to one octahedral sheet produces a
three-sheet mineral type, which is called 2:1 and is represented by the mica, vermiculite
groups, and smectite.

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

The most common smectite mineral is calcium montmorillonite, [3,4], which means that the
layer charge deficiency is balanced by the interlayer cation calcium and water. The basal
spacing of the calcium montmorillonite is 14.2 A˚ . Sodium montmorillonite occurs when the
charge deficiency is balanced by sodium ions and water and the basal spacing is 12.2 A˚.

3. 2 :1 :1 clay minerals

Chlorites are a group of minerals that exhibits a basic 2:1 layer structure similar to that
described for talc or pyrophyllite, but with an interlayer brucite- or gibbsitelike sheet, which
forms a 2:1:1 structural arrangement. Isomorphic substitutions within the interlayer hydroxide
sheet create a net positive charge that balances the negative charge arising from the 2:1 layers.

III. Geological context of Tunisia clays

The inventory of smectitic clays in southern Tunisia showed that three units lithostratigraphic
rocks are likely to give rise to deposits of smectitic clays. It’s about :

Alternations of Meider and Aleg formation aged "Coniacian-Campanian "at J.

Aïdoudi in the region of El Hamma [5,6].

The average member of the Abiod formation aged "Upper Campanian- Lower
Maastrichtian" at Jebel Stah (O.Tfal), Orbata (O. ksab and O. Labaed) [5] and
Hamadi in the Gafsa region.

from EL Haria formation aged “maastrichtien- paléocène” in Chebika, to Oum

Khchab, at Jebel Stah (sector 100) et Sehib (O. Djej et O. Kharoubet) [7].

Laboratory work that investigated the potential of J. Aïdoudi clay for possible industrial uses
has shown that this clay is interesting for the clarification of phosphoric acid [8]. The same
clay activated at hydrochloric acid was proved suitable for the bleaching of vegetable oils [9].
In the field of environmental protection, the clay of J. Aïdoudi has shown encouraging
results. Indeed, its activation product with sulfuric acid has been tested with success in the
retention of Pb2 + ions in aqueous solution [9]. J. Aïdoudi's clay has shown also the

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

performance for the recovry of gas[10]. Moreover, other reviewing evaluate its adsorptive
capacity on the removal of several heavy metals in aqueous systems [1].

The smectitic clays of J. Stah (El Haria formation) were also tested with success, after
activation with hydrochloric acid, in the fading, as well, oils plants and minerals [6,7].

The deposit of J. Aïdoudi is actually exploited by ‘SIREX’ society. Few years ago, it was the
only gisement (Meider alternations) tapped. The extracted clay is a mixture of
montmorillonite and beidellite [11].

Fig.1 : Deposit of J.Aïdoui

A. Geological presentation of the studied deposit

The southern Tunisian Atlas settle at the edge of two orogenic domains differing by their
deformation style: the stable Saharan platform in the South and the Tunisian Atlas folded in
North. It is formed by morphostructural alignments E-W already poured to the south,
generally inflected in N 60, cut by two large shear corridors: the fault of Gafsa and Negrine-
Tozeur accident of average direction N120-130 dexter.The structural device is characterized
by a lozenge to trapezoidal well set with N80-90 medium direction narrow zones that are
highly deformed and separated by broad, flat-bottomed synclines forming vast plains [12].

The southern Atlas of Tunisia has large outcrops of clay formations attributed to Upper
Cretaceous and Cenozoic. Previous work, including those of Jamoussi (1991 ; 2001) and
Fakhfakh (2006) showed that the clay terms of the Aleg and El Haria formations have a
relatively constant mineralogy. At Aïdoudi, the Aleg formation and its Meider equivalent is

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

characterized by a significant fraction of smectite associated with low amount of kaolinite and
illite. The associated minerals are quartz, calcite, feldspars and dolomite.

These formations contain clay levels very rich in smectites; they have been the subject of
geological maps and samples in particular Jebel Aïdoudi (Fig. 2).

Fig. 2 : Localisation map of the studied clays ; ‘A:Aidoudi’ (E.Fakhfakh et al, 2005)

B. Lithological description of “Aleg” formation

At J. Aïdoudi, dominate the Aleg formation and its equivalent Meider. This is a thick series
clay-marly limestone intercalation [14] which settle between the summit of the Zebbag or
Fahdene formation and Abiod formation. The age of this formation is “coniacien -Lower
Campanian”.

IV. Raw materials and techniques used

A. Raw materials

The clay samples used were obtained in the southern atlas from different locations :
The AYD sample of “Coniacian-Lower Campanian” age was taken from
Jebel Aïdoudi (El Hamma region).

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

Fig. 3 : Sampling site (El Hamma )

The (DRT) sample of lower Aptien age was taken from Douiret formation in
(Tataouin region).

Fig.4 : sampling site (Douiret)

B. experimental techniques for characterization

1. mineralogical identification

 Principle of mineralogical analysis by X-ray diffraction

Any crystallized body can be analyzed by X-ray diffraction because its atoms are arranged
according to specific crystalline planes. An X-ray beam is diffracted on a lattice of crystalline
planes according to Bragg's law:

nλ = 2d sin θ

With:

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

λ: wavelength of the X-radiation

d: spacing between 2 successive parallel planes of the crystal lattice (distance reticular)

θ: diffraction angle between the incident beam and the plane network

Thus, for a given X-ray source (λ), scanning at an angle of incidence (θ) of a representative
preparation of a sample, provides access to the knowledge of all the lattice spacings (d) of this
sample.

Powder method

The powder method consists in conducting the mineralogical analysis by diffraction of

X-rays on the total rock. It allows to determine the global mineralogy (minerals clay
and mainly associated minerals) raw samples of clays dried and finely ground.
Oriented Aggregates Method

The oriented aggregates method is based on the trend of mineral particles clay to be
oriented preferentially, by sedimentation, parallel to the basic plans (001), which
promotes X-ray reflection and gives very intense (001) lines. This method requires
separation of the fraction smaller than 2μm which is carried out according to the steps
following:

• disintegration of the clay with distilled water;

• removal of coarse material by wet sieving on a 63 μm mesh screen;
• Decarbonation by cold etching with hydrochloric acid (0.1N), or hot if clay contains
dolomite. The end of the attack is indicated by the stop of effervescence;
• washing with distilled water;
• oxygenated water (30V) attack for the removal of organic matter,
especially humic compounds;
• successive washes and deflocculation by centrifugation (10 min at 2500 rpm);
• recovery of the clay suspension (supernatant) less than 2 microns;
Once recovered, this fraction is deposited on glass slides until drying.
For each sample, 3 slides may be prepared and analyzed after various treatments:
- a normal slide simply dried in the open air whose diagram will serve as a reference;
- a slide treated with ethylene glycol;
- a slide heated at 550 ° C for 2 hours [15].

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

2. Determination of pH

The pH determination of the clays studied was carried out according to the following method:
10 g of clay are dispersed in 50 ml of distilled water, then mechanically stirred for two hours.

The pH of the solution is then determined by a laboratory pH meter.

Tab. 1: The measured pH value

Sample pH
AYD 8,38
DRT 7,96
3. Determination of electrical conductivity

The determination of sample’s electrical conductivity follows the present method : 10 g of

clay are dispersed in 50 ml of distilled water, mechanically stirred for one hour, then filtered.

The conductivity of the solution is determined by a laboratory conductivimetre.

Tab. 2: The measured conductivity value

Sample conductivity (μS/cm) Temperature (°C )

AYD 4,2
28,8
DRT 1604
4. Calcimetry

The total limestone content of the samples is determined by the following method:
1- introduction of 1 g of sample into a 250 ml Erlenmeyer flask.
2-addition of 25 mL of 0.5n sulphiric acid and 125 mL of water.
3-Stirring for 1 hour in a water bath at 90°C.
4-addition of 5 drops of mixed indicator (prepared previously) and titration with 0.5 n NaOH:
the gradual addition of NaOH until the first turn from red to green, then titrate drop by drop
until the second turn - marking the point of equilibrium - from green to red. note the volume.

5-Each series of sample is filled with a double witness. (Laboratory manual in soil science)
 Calculs:

% CaCO3 = (Vt - Ve) mL * t meq / mL * 50 mg CaCO3 / meq * 1 / P g soil * 0.1

with:

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

Vt : volume control NaOH

Ve : volume NaOH sample
T : titre excate of NaOh
P : sample weight (= 1 g)
0.1: conversion mg /g to percentage
 % CaCO3 = (Vt-Ve) * t * 5
Tab. 3: The measured total limestone value

Sample Content of CaCO3

AYD 7,8%

5. total surface area

The clay minerals have the characteristic of being in the form of very small particles. They
thus have a very large contact area with the liquid phases in which they are. This surface is
generally characterized by the concept of specific surface (Ss) which corresponds to the total
surface (external and internal) of a solid, related to the unit of mass. It is expressed in m² / g.

The measurements involve the absorption of molecules on the surfaces of the solid to be
measured. The calculation of the specific surface of the clays was carried out by the method
of the task to the blue of methylene, its principle is to suspend 10g of clay materials in powder
form in 100ml of distilled water, then after stirring for 2 to 3 hours, add successively drops of
methylene blue until complete saturation of the particles clay.

The saturation check is done by "a task test" and it is reached one once the dark blue task is
surrounded by a clear blue halo, which persists.

SC= 20,93*(Ncc/Ps)
With :
Sc : specific surface (m²/g)
NCC : Volume of bleu methylene solution (mL)
PS : Weight of dry clay used (g)
Tab. 4: Value of specific surface measured

Sample Specific surface (m2/g)

AYD 29,5
6. measuring of the water content

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

The water content is determined by difference in weight before and after drying:
(1) Introduction of 5g of fresh soil or dried in a previously tared tare box (Tare = T) and
weigh with lid (Gross weight = Pfr or P air).
(2) Drying at 105 °C in the stove up to constant weight.
(3) Weighing: let the sample cool in a desiccator then weigh. ( Laboratory manual in soil
science)
 Calculs
W%= 100*(Ph-Ps)/Ps
With :
Ph: mass of the dried sample
Ps: mass of the wet sample

Tab. 5: Value of water content measured

Sample water content (% )

AYD 10,17
DRT 4,25

7. Loss on ignition

Loss on ignition is determined by the gravimetric method. A test sample of 1 g previously

dried (P1) is calcined in an oven at 1000 ° C for one hour and weighed (P2).

The difference in weight (P1-P2) corresponds to the loss on ignition. This translates the
departure of the water of constitution, the decomposition of sulphides, carbonates and organic
matter.

Tab. 6: value of loss on ignition measured

Sample Loss on ignition (g)

AYD 0,2
DRT 0,1

8. cation exchange capacity

The determination of the cation exchange capacity (CEC) with ammonium acetate at pH 7 is
carried out in 3 phases, in particular:
(1) saturation of the adsorbent complex by the NH4 + ion and extraction of exchangeable bases.

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

(2) washing the earth with alcohol in order to eliminate the saturating NH4 + solution filling the
porosities
(3) NH4 + assay after quantitative desorption by k+.
The exchange reactions can be carried out by successive equilibration, centrifugation and
decantation (discontinuous methode) or by percolation (continuous method).
The NH 4 + assay is by Kjeldahl distillation or by potentiometry with an ammonia specific
electrode.
Tab. 7: Mesured cation exchange capacity

Sample CEC (méq/100 g)

AYD 39,1

9. Infrared spectroscopy

Fourier transform infrared spectrometry (I.R.T.F.) is an analytical technique molecule to

obtain information on chemical bonds and structure molecular of the analyzed materials.

 Principe

The absorption bands in the spectral range of the infrared come from the interaction of
the electrical component of the incident electromagnetic radiation with the electric
dipoles of unsymmetrical bonds.

Infrared is interested in the excitations of the vibration levels of the links with character
covalently present in the molecules. From its origins, infrared served as a method semi-
empirical structural analysis. There is a correlation between the absorption maxima of some
bands and organic functions. As a result, we may have information about the deformations of
the bonds and the skeleton of the compound to be studied. The absorption bands are many nd
different for each compound.

10. Purification of clays

The purification of clays is determined by the following method:

1. Introduction of a quantity of raw clay (100 g) into an Erlenmeyer flask

2. add enough distilled water, let stand a little, mix well (for a few minutes with vertical
magnetic stirrer + stir bar)

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

3. Decantation overnight

4. The transfer of the upper part using a pipette into an Erlenmeyer flask (here we will have 3
phases from top to bottom water, clay more or less pure and finally impurities) we just take
the upper part of the clay.

5. A sufficient amount of distilled water is added to the Erlenmeyer flask of 3.

6. Repetition decantation 3 times

 Decarbonation:

8. 10% HNO3 is gradually added until the disappearance of effervescence Elimination of

organic matter

9. We do the same with hydrogen peroxide H2O2

10. Centrifuge at 4500 (r.p.m) 3 to 4 times until complete elimination of hydrogen peroxide
and nitric acid

11. Leaving to air dry for one week or oven at 105 ° C for 20 hours.

Fig.5 : centrifuge

11. Laser granulometry

Laser granulometry is a technique based on light diffraction. According to Fraunhofer's
theory:

 Non porous and opaque spherical particles are considered.

 These particles have a diameter greater than the wavelength.
 The particles are far enough apart Particles are animated by a random movement .
 Particles diffract light with the same efficiency regardless of their size.

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

When a laser beam illuminates a particle, diffraction fringes can be observed. According to
Fraunhofer, the intensity of the diffracted radiation and the diffraction angle depend on the
size of the particles. The smaller the particle is, the larger the diffraction angle.

Fig. 6 : laser granulometry apparatus

V. PRESENTATION OF GEOPOLYMERS

A. Definition

The geopolymers are aluminosilicate inorganic polymers obtained by activation at ambient

temperature, of a low-calcium alumino-silicate source by an alkaline hydroxide solution [16].
Geopolymers are constituted of a network of aluminums and silicates tetrahedrons linked
together by oxygen atoms bridging. The lack of charge caused by the presence of aluminum
in coordination tetraedric requires the presence of M + cations  (Na+, K+…), charge
compensators in the structural cavities of the material to maintain electrical neutrality within
thematrix. The final material appears as amorphous or semi-crystalline X-ray with a scattering
scale centered around 29 ° (Figure 7), highlighting the quasiamorphic character of the
material [17]. These materials are often described as zeolitic precursors [17;18].
However,zeolite synthesis requires a higher liquid / solid ratio leading to a kinetic reaction
and crystallinity differ from geopolymers [18].

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

Fig. 7 :Diffractogram of a sodium-based geopolymer (Provis et al. 2005)

B. Chemical structure

Given the amorphous nature of geopolymers, the spectroscopy paramagnetic nuclear allows to
describe more precisely the structure of these materials. To facilitate the description of
aluminosilicate structures, Engelhardt et al. introduce the following notation, Qn (mAl), where
n is the number of coordination of the central silicon atom, m the number of neighboring
aluminum atoms and with 0 m n 4.

Figure 8 illustrates this notation for n = 4, which is the coordination generally observed for
silicon in geopolymers.

Fig. 8 : Coordination of silicon centers described by the rating, Engelhardt et al. (1987).
Barbosa et al. [20] then proposed a new model describing the geopolymer structure, based on
silicon NMR. This model describes the structure order within a short distance of the
geopolymers. The structure contains aluminum tetrahedral and silicon distributed randomly
forming cavities of sufficient size to receive the alkaline cations. This arrangement leads to
silicon atoms in Q4 (2Al) and in Q4 (3Al), but with a predominance of the latter. However, the

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

model proposed by Barbosa et al. [20] suggests that the Na + cation is now only in hydrated
form.

Rowles et al. [21] have therefore proposed a more comprehensive model, based on NMR of
aluminum, silicon and sodium (Figure 9). In this model, sodium is present in a hydrated form
in the cavities of the geopolymer but also in a form less hydrated as a charge compensator,
able to intervene as a trainer or Polymer network modifier.

Fig. 9: Model of an aluminosilicate-based inorganic polymer based on the model of

Barbosa et al. (2000) supplemented by new elements, proposed by Rowles et al. (2007).

C. Mechanism of geopolymerization

At the present time, the reactions of geopolymerization remain complex and poorly defined.
However, it is recognized that the formation of geopolymers proceeds according to a
mechanism of dissolution / restructuring / polymerization leading to a solid material [22,23].
The kinetics of each step depends on the source alumino-silicate, the silica concentration, the
nature of the alkaline cation, the value of the pH and the amount of water used in synthesizing
the geopolymers. Reactions put in game are therefore divided into several successive stages:

 Dissolution / hydrolysis: This first step is to dissolve the solid source alumino-silicate
with high pH alkaline solution. At the beginning of the process, alkali hydroxides
diffuse on the surface of alumino-silicate particles and interact with these to form
silanol and aluminol groups. Then, it follows the phase of dissolution, that is, breaking
the Si-O-Si and Si-O-Al bonds of the compound to form reactive entities Si (OH) 4
and Al (OH) 4 in the solution [24].

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

 Restructuring: In the second step the dissolved species in solution react between
them to form oligomers whose size varies according to the alkali cation used. This
Step determines the microstructure and pore distribution in the material [16,25].

 Polycondensation: The increase of the concentration of oligomers in the phase. The

aqueous solution leads to their polycondensation to form Si-O-Si and Si-O-Al bonds.
Thisreaction leads to the formation of a three-dimensional macromolecule [23].

Duxson et al. [26] proposed a model summarizing the reactions of electropolymerization

(Figure 9). This model is based on the knowledge acquired on the zeolite synthesis. The first
stage involves the dissolution of the aluminosilicate source by the alkaline solution, to form
the silicates and aluminosilicates. The solution resulting is quickly saturated and it follows the
formation of a gel caused by the condensation of the different species. The time it takes to
reach the supersaturation depends on the composition parameters and the synthesis
conditions. The gel formed can then reorganize and rearrange itself until a three-dimensional
network is formed.

Fig. 10 : Mechanism of electropolymerization proposed by Duxson et al. (2007).

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AIDOUDI’S CLAY CHARACTERIZATION FOR INDUSTRIAL APPLICATION

Bibliographical references
[1] Sdiri, A., Higashi, T., Hatta, T., Jamoussi, F., & Tase, N. (2011). Evaluating the
adsorptive capacity of montmorillonitic and calcareous clays on the removal of several heavy
metals in aqueous systems. Chemical Engineering Journal

[3] Murray, H. H. (2006). structure and Composition of the Clay Minerals and their Physical
and Chemical Properties. Applied Clay Mineralogy - Occurrences, Processing and
Application of Kaolins, Bentonites, Palygorskite-Sepiolite, and Common Clays, 7–31.

[4] A.D. Karathanasis. Clay minerals. United States Department of Agriculture Forest
Service, Aiken, South Carolina, U.S.A

[5] ABDELJAOUED S., « Etude sédimentologique et structurale de la partie Est de la Chaîne

Nord des Chotts (Tunisie méridionale) », Thèse de doctorat de spécialité en Géologie, Faculté

des Sciences de Tunis, 1983, 148 p.

[6] JAMOUSSI F., “Les argiles de Tunisie. Etude minéralogique, géotechnique et utilisations

industrielles”, Thèse d'Etat .université Tunis El Manar, Fac. Sc. Tunis, 2001. 437 p.

[7] JAMOUSSI F., “Etude géologique et géotechnique de substances minérales utiles de la

région de Gafsa”, Thèse Doc. Spéci. Géol. Fac. Sc. Tunis, 1991, 298 p.

[8] CHARFI A. ET LOUHAÏCHI M.L., “Recherche d’une argile bentonitique pour la

défluoration et la clarification de l’acide phosphorique”, Rapport interne S.A.E.P.A. Projet de
cartographie du sud tunisien, 1982, p. 44.

[9] CHAARI I., FAKHFAKH E., CHAKROUN S., BOUZID J., BOUJELBENE N., FEKI
M., ROCHA F., JAMOUSSI F., “Lead removal from aqueous solutions by a Tunisian
smectitic clay”, Journal of Hazardous Materials, Vol. 156, 2008, p. 545-551.

[10] BEN ZINA M., BELLAGI A., “Détermination du pouvoir adsorbant d'un matériau
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