ISSN: 2320-5407 Int. J. Adv. Res.

9(03), 683-691

Journal Homepage: - www.journalijar.com

Article DOI: 10.21474/IJAR01/12633

DOI URL: http://dx.doi.org/10.21474/IJAR01/12633

RESEARCH ARTICLE
FEASIBILITY STUDY FOR THE USE OF NATURAL MORDENITE IN PURIFICATION PROCESSES
OF WASTEWATERS FROM PHARMACEUTICAL POLLUTANTS

L.G. Eprikashvili, T.N. Kordzakhia, M.G. Zautashvili, I.M.Rubashvili, N.V. Pirtskhalava, M.A. Dzagania
and G.P. Tsintskaladze
Iv.Javakhishvili Tbilisi State University; P.Melikishvili Institute of Physical and Organic Chemistry.
……………………………………………………………………………………………………....
Manuscript Info Abstract
……………………. ………………………………………………………………
Manuscript History The present research concerns the possibility of adsorptive removal of
Received: 20 January 2021 the frequently used antibiotics – moxifloxacin and norfloxacin on
Final Accepted: 24 February 2021 natural zeolites – mordenite and its acid-modified form from aqueous
Published: March 2021 solutions. The adsorption of the above-mentioned antibiotics on the
selected natural zeolite samples was investigated under static and
Key words:-
Mordenite, Zeolite, Adsorption, dynamic conditions. Adsorption experiment under dynamic conditions
Pharmaceutical Pollutants, Water carried out using the specially constructed dynamic type of laboratory
Purification equipment. Based on the data of chemical, IR spectroscopic, X-ray
diffraction analyses, it has shown that when the zeolite adsorbent is
treated with an acid, an equivalent exchange of extra framework cations
for a hydrogen ion and dealumination occurs and silanol groups are
formed at the same time. The increase in the adsorption activity of
mordenite as a result of its treatment with acid is associated with an
increase in the pore size due to the unblocking of the adsorbent
aluminosilicate framework channels during dealumination.
Copy Right, IJAR, 2021,. All rights reserved.
……………………………………………………………………………………………………....
Introduction:-
Modern rates pace of development of various industries, which play a leading role in the global fuel and energy
balance, leads to sharply increasing man-made loads on all objects of the natural environment. The urgency of the
global problem of health and environmental protection contributed to the high interest of the world scientific
community in zeolites. Natural zeolites and zeolite-containing rocks, being a widespread and cheap mineral raw
material, have a unique spectrum of physical, physicochemical and adsorption properties, due to which they have
found wide application in the practice of cleaning various objects, in particular natural and wastewaters [1].

Adsorption systems, adsorbents aimed at reducing environmental risk, reducing energy intensity of processes,
refusal of special sorbents, etc., should be attributed to compliance with the principles of "green economy" [2,3].
This approach implies a high degree of minimization of expenses during water purification from toxic and harmful
components. Economic aspects of this process play a very relevant role, allowing the purification and additional
treatment of wastewater, thus, reducing the anthropogenic load on water bodies.

At present, 15 varieties of zeolite minerals have been identified in Georgia, but among them industrial significance
may have only: analcime, clinoptilolite-heulandite, phillipsite, laumontite and mordenite (MOR). The presence of
large reserves of natural zeolites in Georgia contributed to the study of adsorption properties of both initial and
nano-modified samples in order to create adsorption materials effective for the extraction of certain pharmaceutical
ingredients namely fluoroquinolones (FQs) – moxifloxacin (MOX) (C21H24FN3O4) and norfloxacin (NOR)

Corresponding Author:- L.G. Eprikashvili 683

Address:- Iv.Javakhishvili Tbilisi State University; P.Melikishvili Institute of Physical and Organic
Chemistry.
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(C16H18FN3O3) from wastewaters, as well as the study of adsorption process mechanisms of pharmaceutical
substances [4,5].

Fluoroquinolone antibiotics are synthetic antibacterial drugs with a 4-quinolone basic structure (Figure 1) which can
inhibit the proliferation of many Gram-negative and Gram-positive bacteria [4,5].

Figure 1:-The chemical structures of MOX (a) and NOR (b)

(a) (b)

The presence of fluorine atoms is a critical factor for high activity; the activity of this antibiotic increased by
approximately tenfold. So, they have been widely used in medical and veterinary practice. However, as a result of
antibiotic overuse, public concern about FQs has significantly been increasing in the past decades. The
environmental concern of FQ antibiotics residues in the aquatic environments is not only on their potential to
increase antibiotic resistance but also on their unfavourable ecotoxicity profile [6]. The presence of FQs residues in
effluents from households, hospitals, and pharmaceutical industries is a significant cause of acute and chronic
toxicity, as well as the emergence of resistant bacteria. Consequently, removal of FQ residues from the environment
is a crucial issue [7,8].

Adsorption method is a well-controlled process that allows to removing various contaminants up to almost any
residual concentration, regardless of the chemical stability of pollutants, the absence of secondary contaminants, and
the cost efficiency associated with the repeated use of the sorbent [9].

The adsorption method for removal of organic pollutants from wastewaters is based on the difference variety in
energies of Van der Waals interaction of dissolved substance molecules and solvent with solid adsorbent surface or
on formation of chemical bonds between dissolved substance and surface groups of adsorbent. The possibility of
adsorption of porous structure materials is also associated with the developed adsorption surface and its availability.
The competition of water binding and adsorption processes in aqueous solutions is caused by differentiation and
selection of adsorbents for removal of organic and inorganic substances from wastewaters [10].

Natural mordenite is a mineral with the formula of typical oxide – Na2O·Al2O3·10SiO2·6H2O. Idealized composition
of elementary cell is Na8[(AlO2)8(SiO2)40]·24H2O. Depending on geological conditions of deposits, sodium cations
can be partially replaced by potassium, calcium or magnesium cations. The ratio of SiO 2/Al2O3 in mordenite zeolites
varies between 8.3-10.7. Mordenite has a tetrahedral structure in which a silicon or aluminum atom is surrounded by
four oxygen atoms. Tetrahedrons are grouped in chains (Figure 2). Inside the chains, there are adsorption cavities
[11,12].
Figure 2:-Chains formed by mordenite tetrahedrons

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Figure 3:-Projection of the mordenite structure direction the main channels.

Mordenite structure is penetrated by a two-dimensional system of 8- and 12-membered channels. Some cations are
localized in eight-membered channels, and some - in large channels. Cations block narrow 8-membered channels,
and only large channels with diameter of 0.67 nm are open for the diffusion of molecules; Na-, Ca-mordenites are
unblocked after treatment with hot hydrochloric acid. Chemical modification provides ample opportunities for
regulating the molecular sieve and catalytic properties of mordenite. The limiting adsorption volume of both narrow-
porous and wide-porous mordenite varies between 0.076-0.09 cm3 g-1. The difference in the molecular-sieve
properties caused by the different arrangement of sodium cations, which in narrow-pore mordenite are located in
large twelve-membered channels (0.59-0.47 nm) and thus, narrow their effective diameter. In wide-pore ones they
are localized in the depths of niches composed double eight-membered rings (0.39-0.47 nm) and do not prevent the
penetration of large molecules into large channels [11-15]. The projection of the mordenite structure in the direction
of the main channels is shown in Figure 3.

Experimental:-
Natural mordenite with zeolite-phase content of 50-60% from Bolnisi-Ratevani deposit (Georgia) was used in this
study. The chemical composition of mordenite varies within narrow range, the ratio of Si/Al is within 4.5-5.5.
Chemical composition of the studied samples of mordenite is presented in Table 1. The analysis of the chemical
composition of natural and treated mordenite samples was carried out using Spectroscout XEP-04 (Germany).

Table 1:- Chemical composition of natural mordenite from Bolnisi-Ratevani deposit (Georgia) and acid-modified
samples.
Concentration
Oxides, % Initial MOR Modified MOR (with 5N Modified MOR (with
solution of HCl) 10N solution of HCl)
SiO2 71.64 76.18 88.53
Al2O3 9.955 9.828 3.184
CaO 4.137 2.257 0.3999
Fe2O3 2.614 2.577 1.631
Na2O 1.66 1.179 0.1353
K2O 1.313 1.47 1.247
MgO 1.109 0.8912 0.4318
TiO2 0.3012 0.3296 0.236
P2O5 0.06694 0.02415 0.0006924
MnO 0.05198 0.03122 0.008663
SO3 0.03272 0.002502 0.002502
Si/Al 6.34 6.84 24.45
ƩH2O 7.12 4.95 4.19

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Exchange cations are represented by calcium and sodium; potassium and magnesium are present in smaller
quantities. Chemical modification provides ample opportunities to regulate the molecular-sieve properties of
mordenite. The high value of the silicate module (Si/Al) determines the high thermal- and acid-resistance of the
mineral.

The X-ray diffraction analysis of the studied samples of mordenite (initial and acid-modified) was carried out using
X-ray diffractometer - Drone-4 (Russia). The obtained diffractograms are presented in Figure 4. The diffractogram
of the initial natural mordenite treated by boiling acids of different concentrations show that despite of changes in
the chemical composition, the crystal lattice of zeolite remains unchanged after acid treatment. The diffractogram of
natural (native) and treated boiling 5N solution of hydrochloric acid (HC1) zeolite is similar to the diffractogram of
original mordenite.

Figure 4:- X-rEay diffractograms of initial MOR (a), modified MOR with 5N HCl (b) and modified MOR with 10N
HCl (c).

Leaching of zeolites with acids is characterized by the fact that acid exposes the mineral frame, which preserves the
architecture of the zeolite. At the same time, the value of the silicate module increases. It should be noted that
treatment of mordenite with 10N HC1 increases this value to 24.45 (Figure 4), but the diffractogram of this sample
indicates the destruction of the crystal structure and the mordenite lattice becomes more defective, which is probably
a consequence of leaching.

Figure 5 presents IR spectra of mordenites – initial and acid-modified with 5N HC1 and 10N HCl. IR-spectrometric
study was performed using Agilent Cary 630 FTIR Spectrometer (USA) in the range of 350-1300 cm-1. Comparison
of the IR spectra of natural mordenite with an acid-treated sample (5N HCl) showed the presence of all
characteristic absorption bands of the aluminosilicon-oxygen framework of the zeolite. A somewhat different
spectrum is observed for the sample modified with 10N HCl, which is probably caused by the deformation of the
zeolite structure [13].

Figure 5:- IR spectra of initial MOR (a), modified MOR with 5N HCl (b) and modified MOR with 10N HCl (c).

(a)

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(b)

(c)

Along with the chemical and mineral compositions of natural zeolites, textural and structural characteristics are
fundamental in the study and development of adsorbents involved in various adsorption processes. Nano-
modification of natural zeolites with solutions of hydrochloric acid or alkali leads to a significant increase in the
values of physical-mechanical and textural characteristics: the specific surface area of the zeolite increases on
average up to five times, and the total pore volume doubles. To characterize the texture parameters of the studied
samples (specific surface area, volume of mesopores and total pore volume, pore-size distribution), the method of
low-temperature adsorption-desorption of nitrogen at 77.2 K was used. The procedure was carried out on the
equipment – Micromeritics Asap 2020 Plus Physisorption Analyzer (USA). The obtained isotherms were processed
by the Barrett-Joyner-Hallend (BJH) method [16, 17].

Among the studied mordenite samples, the natural mordenite sample is characterized by the lowest specific surface
area, density, porosity and total pore volume. Nano-modification of samples with acid solution is accompanied by an
increase in specific surface area (to 70.84 from 162.33 m2/g), volumes (to 0.086 from 0.097 cm3 g-1), pore
diameters, porosity and a decrease in true density. The most significant changes in the structure of the zeolite
occurred during its treatment with 10N boiling acid solution. By varying the type of modifying agent, it is possible
to form a porous structure at the level of micro-, meso- and macro-pores.

The adsorption capacity of zeolites was studied under static and dynamic conditions. Adsorption capacity of
mordenite samples by water vapour was studied by excitation (desiccant) method (pre-activation temperature 400
°
C) (Table 2). As it is obvious from the above data, modification of natural mordenite with 5N acid solution
increases its adsorption capacity by 7.3%, while treatment with 10N acid solution leads to its decrease (Figure 6)
[18-20].

Table 2:- Adsorption capacity by water vapour on mordenite samples at 18 °C.

Sample Adsorption a, mmol / g
Initial MOR 3.363

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Modified MOR (with 5N solution of HCl) 3.608

Modified MOR (with 10N solution of HCl) 3.069

Investigation of adsorption properties of natural and modified samples of mordenite in relation to selected FQ
antibiotics was carried out under dynamic conditions on the specially designed dynamic type equipment. The change
of FQ antibiotic sorbate concentration at the outlet of adsorption column was determined by the validated HPLC
method [5]. The HPLC analysis was performed using LC-20AD Prominence Shimadzu HPLC System (Japan) and
HPLC column – Agilent SB-C18 4.6×250 mm, 5 µm (USA). To prepare model aqueous test solutions of each FQ
antibiotic – moxifloxacin and norfloxacin, the analytical standards (MilliporeSigma) and "Aqua FX" water
purification system, analytical balance – LEX-210 were used. All the measuring equipment have been properly
calibrated.

Figure 6:- Modification of the initial mordenite with HCl [19].

The concentration of the sorbate (FQ antibiotic) in the adsorbent before the start of the process is zero, the
concentration of the sorbate in the input stream is constant.

The dynamics of sorption processes considers the spatio-temporal distribution of components between the phases of
the system (one of which is solid), which occurs when these phases move relative to each other.

Experimental study of adsorption dynamics usually has two purposes: to check the adequacy of the model of the
experiment and to obtain information from the output curves of adsorption needed to select adsorbents, their sizes
and design. Adsorption process is characterized by probabilistic functions of particle distribution between mobile
and solid phases, on the basis of which concentration distribution curves are found. For practical calculation of
adsorption processes, a number of generally accepted simplifications were used in the work: 1) only one component
of the flow is adsorbed; 2) The mobile phase is incompressible, and the concentration of adsorbed substance is so
low that changes in flux density due to adsorption loss can be ignored; 3) The flow is moving in one direction at a
constant flow rate [11,14].

The dynamic characteristics of the adsorption process were studied using the above-mentioned equipment which
consists of three parts: 1) a glass adsorption column, 2) a cylindrical electric furnace, 3) a high-pressure pump. In
dynamic condition through the prepared zeolite samples placed in a glass adsorption column, the studied FQ
antibiotic sorbate solution at a concentration of 1.0 mg mL-1 was passed. The experiment was carried out at room
temperature (22±3 °C), with the flow rate of 1.0 mL min-1. When analysing the results obtained with the experiment,
approximate test solutions for problems of equilibrium and non-equilibrium frontal dynamics of adsorption were
used.

Results And Discussion:-

On the basis of experimental data, adsorption output curves describing the dependencies of adsorbed sorbate
concentration growth behind the zeolite layer in time were constructed (the ratio of effluent concentration to influent
concentration of the sorbate - C/C0 versus time) which are shown in Figure 7.

The experiment was carried out until the adsorption capacity of the zeolite layer was fully worked out, i.e. until the
sorbate concentration equal to its concentration in the initial solution (influent solution) appeared at the outlet of the
adsorption column. The dynamic characteristics of adsorption of moxifloxacin and norfloxacin calculated from
experimental data are summarized in Table 3, 4.

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Figure 7:- Output adsorption curves of NOR on initial mordenite (a), on mordenite activated with 5N HCl (b), on
mordenite activated with 10N HCl (c) and MOX on initial mordenite (d), on mordenite activated with 5N HCl (e),
on mordenite activated with 10N HCl (f)

The dynamic adsorption capacity of the adsorbent layer (a d) characterizes the amount of substance absorbed before
the moment of "breakthrough" (τb) and attributed to the mass of loading of the entire adsorbent. From the "moment
of breakthrough", extracted substance appears in the outgoing stream and its concentration begins to increase
progressively. Between the time of protective action of the sorbent layer and the length of the adsorbent (L) there is
a dependence determined by the formula of N. A. Shilov [11]:
τb=K×L-τo A.1

where K is coefficient of the protective action, showing the time taken by the 1 cm high adsorbent layer retains the
absorbed substance in a stationary mode, cm, τo is time loss of protective action associated with the initial period of
formation of the sorbate distribution curve, min; L is height of loading of the adsorbent layer (in this case 24 cm).

The equilibrium adsorption capacity of the sorbent layer depends on the nature of the sorbate and adsorbent (a eq) and
was calculated by the formula [11]:
aeq=W×τb ×Co+W×∆τ×Co×φ/V A.2

where, W is the volumetric flow rate of the sorbate influent solution, cm3 min-1; τb is time of protective actions of the
sorbent layer, min; Co – initial concentration of pollutant (influent concentration), mg mL-1; Δτ is the difference in
sorbent layer performance time to complete saturation - τeq, i.e., the time of occurrence of the maximum
(equilibrium) concentration and breakthrough concentration - τb through the sorbent layer, min; φ is the coefficient
of the symmetry of the output curves or the distribution curves, V – the mass of the loaded adsorbent.

The height of the working layer - Lo, determined from the output curves reflecting pollutant concentration rises
behind the adsorbent layer with time, is an important characteristic of the dynamics of the adsorption process. The
value of Lo, the length of the mass-transfer zone, was determined on the basis of the obtained output curves
according to the equation reported in the papers. The efficiency equilibrium adsorption capacity of the adsorbent
layer (the degree of utilization of the adsorbent) – η, % is determined by the ratio of the dynamic adsorption capacity
of the layer to the equilibrium adsorption capacity of the sorbent layer (Table 3, 4) [4, 11].

Table 3:- The dynamic characteristics of NOR adsorption on initial and modified MOR.
Some dynamic characteristics of Antibiotic - norfloxacin

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antibiotics adsorbtion Initial MOR Modified MOR (with Modified MOR (with 10N
5N solution of HCl) solution of HCl)
Height of working sorbent layer – Lo, 39.84 30.00 47.59
cm
Dynamic adsorption activity of sorbent 0.14 0.17 0.09
layer to antibiotic – ad, mg/g
Equilibrium adsorption activity of 00.9 0.12 0.05
sorbent layer to antibiotic – aequi., mg/g
Degree of utilization of the sorbent – η, 64.29 70.59 60.00
%

Table 4:- The dynamic characteristics of MOX adsorption on the initial and modified MOR.
Some dynamic characteristics of Antibiotic - moxifloxacin
antibiotics adsorbtion Initial MOR Modified MOR (with Modified MOR (with 10N
5N solution of HCl) solution of HCl)
Height of working sorbent layer – Lo, 15.60 14.88 16.56
cm
Dynamic adsorption activity of sorbent 0.12 0.13 0.10
layer to antibiotic – ad, mg/g
Equilibrium adsorption activity of 0.09 0.10 0.07
sorbent layer to antibiotic – aequi., mg/g
Degree of utilization of the sorbent – η, 75.00 76.92 70.00
%

Experimental data obtained FQ antibiotics adsorption on the studied mordenite samples in dynamic conditions
indicates an improvement in the process of adsorption of NOR and MOX by the sample of mordenite modified with
5N hydrochloric acid solution. The efficiency of the equilibrium adsorption capacity of the sorbent layer (η)
increases. The height of the working layer (Lo) decreases, which increases the repeatability of sorbent "elementary"
volumes in the process of repeated acts of sorption-desorption. The obtained data clearly demonstrates the influence
of the pharmaceutical pollutant nature and chemical structure on the process of its extraction from the aqueous
solution by zeolite.

Conclusion:-
It has been established that natural and acid-modified (5N HCl) mordenite can be proposed as an eco-friendly,
highly efficient adsorbent for the extraction of a fairly wide range of organic substances from aqueous medium,
including pharmaceutical pollutants. Most adsorption processes are carried out in equipment with a fixed dense
layer. It should be noted that the use of granular zeolites (mordenite) in close-packed adsorbers is very effective for
removing ecologically significant concentrations of many pharmaceutical pollutants and many other toxic organic
compounds. From the economic point of view, it is very important that it is possible to recycle the used high-silica
sorbents after their regeneration by the oxidation method, because such zeolites are resistant to oxidizing agents
(such as hydroxyl radicals, ozone, etc.), and can be regenerated without removing them from the adsorber.

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