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2023-CHIBANV Et Al
2023-CHIBANV Et Al
2023-CHIBANV Et Al
Case Report
A R T I C L E I N F O A B S T R A C T
Keywords: The challenge of the scientific community is to synthesize innovative, low-cost, and environmentally friendly
Cost estimation membrane materials for the treatment of industrial wastewater. The objective of this work is the elaboration and
Microfiltration membrane characterization of a new flat ceramic membrane based on a natural Moroccan phengite clay by the paste casting
Phengite clay
method for microfiltration applications. The ceramic membrane was sintered from 850 ◦ C to 1150 ◦ C for 2 hours.
Real-wastewater
The optimal membrane sintered at 1050 ◦ C has a porosity of 34.5%, an average pore diameter of 3.9 μm, water
Regeneration
permeability of 43.50 L/h m2 bar, mechanical strength of 26.7 MPa, and excellent chemical corrosion resistance
in acidic and basic media. The performance of the optimal membrane was evaluated by frontal microfiltration of
the pre-treated real wastewater (RWW3) from a local clothes washing. The obtained results show that the
removal percentage of electrical conductivity, total dissolved solids, and suspended matter is 66.2%, 71.8%, and
100% respectively. The cost of preparing the ceramic membrane was estimated at 3.5 $/m2, which is cheaper
compared to those commercially available. The high regeneration efficiency showed that demineralized water
was able to adequately clean the fouled microfiltration membrane by 82%. The obtained filtration results are
very promising and could allow the use of the membrane prepared from a locally available material as an
alternative process in the treatment of various sources of industrial wastewater.
* Corresponding author. Laboratory of Applied Chemistry and Environment, Faculty of Sciences, Ibnou Zohr University, Agadir, Morocco.
** Corresponding author. aboratory of Applied Chemistry and Environment, Faculty of Sciences, Ibnou Zohr University, Agadir, Morocco.
E-mail addresses: salek.lagdali@edu.uiz.ac.ma (S. Lagdali), s.iaich@uiz.ac.ma (S. Iaich).
https://doi.org/10.1016/j.cscee.2023.100388
Received 29 April 2023; Received in revised form 30 May 2023; Accepted 30 May 2023
Available online 1 June 2023
2666-0164/© 2023 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
S. Lagdali et al. Case Studies in Chemical and Environmental Engineering 8 (2023) 100388
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S. Lagdali et al. Case Studies in Chemical and Environmental Engineering 8 (2023) 100388
After the preparation of the ceramic membranes, a heat treatment The mechanical strength of flat ceramic membranes that were
step is essential in this process. Generally, heat treatment is divided into developed and sintered at different temperatures was evaluated using
two main parts: drying and sintering [26]. Fig. S2 shows the thermal the three-point flexural method. Rectangular samples with 60 mm × 20
program for the sintering of the produced flat membranes. The sintering mm × 5 mm dimensions were developed by the paste molding method
process has two steps: a step at 250 ◦ C and a step at the final sintering using the same formulation of pastes employed to manufacture our flat
temperature. Firstly, the temperature was increased by a firing rate of membranes. These specimens are sintered using the same thermal pro
2 ◦ C/min from room temperature to 250 ◦ C and then maintained at this tocol mentioned above. Subsequently, the flexural strength σ (MPa) was
temperature for 1 hour, then the temperature was increased by 4 ◦ C/min evaluated using a laboratory scale tool conforming to ASTM C674-88,
to the desired final temperature. Finally the membranes were sintered at and then calculated according to the following formula, Eq. (6) [1,23].
different temperatures (850 ◦ C, 900 ◦ C, 950 ◦ C, 1000 ◦ C, 1050 ◦ C, 3.F.L
1100 ◦ C, 1150 ◦ C) for 2 hours. The sintering temperature is necessary for σ= (6)
2.l.e2
the final consolidation of the flat ceramic membranes [27].
where F is the force applied to the specimen in (N), L is the distance
2.4. Characterization techniques between the two specimens’ supports in (mm), l is the specimen width in
(mm) and e is the specimen thickness in (mm). The filtration experiment
The chemical composition of the clay was determined by X-ray was performed at the laboratory level using a frontal filtration pilot. The
fluorescence with a SIEMENS 300 instrument. The structural properties experimental setup is shown in Fig. S3. Experimental instruments made
of the raw and heat-treated clay were characterized by X-ray diffraction of transparent plastic were used for filtration at room temperature (25
(XRD) using a Philips X’Pert X-ray diffractometer operating with Cu Kα ± 1 ◦ C) and low pressure (0.1, 0.15, and 0.2 bar). The effective filtration
radiation (λ = 1.54056 Å). The surface morphology of the developed surface is 15.5 cm2 and the flat ceramic membrane is inserted hori
ceramic membranes (top view) was observed through scanning electron zontally into the membrane module. The membrane was immersed in
microscopy (SEM; JEOL JSM IT-100 type, Japan). Image J software distilled water for 24 hours before each filtration test to obtain a stable
version 1.44e was used to estimate the average pore diameter and pore flux [38]. The variation of the water height h between the surface of the
size distribution (PSD) of the membranes through the SEM images [30]. flat membrane and the water level in the feed tank allows the trans
The average pore diameter dave (μm) was calculated using Eq. (1) membrane pressure ΔP (bar) to vary. This pressure is calculated by the
considering that the membrane surface has a cylindrical porous texture following relationship, Eq. (7) [39].
[22,31,32].
ΔP = ρ.g.h (7)
⎡ ⎤0.5
3
∑n 2
with ρ being the density of water (g/cm ), h being the height of water
⎢ i=1 ni .di ⎥
dave = ⎢ ⎥ (1) (m), and g being the gravity field (N/Kg).
⎣ ∑ n ⎦
ni Distilled water was used to measure the water permeability of our
i=1
membrane. The permeate flux Jw is measured using the volume of
with n being the number of pores and di being the diameter of the ith permeate collected as a function of time. This magnitude can be calcu
pore (μm). We measure the diameter of the flat ceramic membranes lated by using Eq. (8) [40]. The permeability (LP) is calculated by
before and after the sintering process with a digital caliper, the applying Darcy’s law, which is based on the variation of the permeate
shrinkage (%) may be measured by Eq. (2) [33]. flux Jw as a function of the transmembrane pressure ΔP, Eq. (9) [41].
( ) V
Shrinkage =
D0 − D1
× 100 (2) Jw = (8)
D0 S.Δt
where D0 (mm) and D1 (mm) are the diameter of the green and the Jw = Lp .ΔP (9)
sintered membrane respectively. The porosity (%), water absorption 2
with Jw is the permeate flux (L/h.m ), S is the membrane filtration
(%), and bulk density (g/cm3) of the clay-based ceramic membranes surface (m2), V is the permeate volume (L), Δt is the sampling time (h),
were obtained by boiling water immersion according to ASTM C373-88. LP is the permeability (L/h.m2.bar), and ΔP is the transmembrane
To further explain the experiment, the samples were dried in an oven at pressure (bar). Chemical resistance tests are performed in the acidic and
110 ◦ C for 24 hours to determine the dry mass mdry (g), then placed in a basic media at room temperature (25 ± 1 ◦ C). pH = 1 and pH = 13.5
distilled water bath and boiled for 5 hours, taking care to cover the solutions were prepared using hydrochloric acid (HCl) and sodium hy
specimens with water, and using pins to separate the samples from the droxide (NaOH), respectively. The prepared membranes were pre-dried
bath’s bottom and sides. After boiling, the samples are placed in the bath at 80 ◦ C for 24 hours and then immersed in beakers containing acidic
for another 24 hours. Then the wet mass mwet (g) of each sample sus and basic solutions for 7 successive days. After washing with distilled
pended in water is determined. Finally, the saturated mass msat (g) of water and drying for 24 hours at 80 ◦ C the weight loss (%) is measured,
each sample is determined after softly wiping the surface with a lint-free which is indicated the chemical resistance of the membranes according
cloth or cotton towel to remove any excess water from the surface. Eqs. to the following formula, Eq. (10) [10,42].
(3)–(5) were used for calculating the porosity, water absorption, and ( )
bulk density of water, respectively [34–37]. Weight loss =
m0 − m1
× 100 (10)
m0
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S. Lagdali et al. Case Studies in Chemical and Environmental Engineering 8 (2023) 100388
Table 2 using pre-treated real wastewater RWW3. The initial permeate flux of
Chemical composition of raw phengite clay distilled water (Jw0, L/h.m2) was recorded for 180 minutes at 0.2 bar.
by XRF. RWW3 was passed through the membrane with similar experimental
Oxides wt.% conditions to produce permeate flux (Jp, L/h.m2). After 1 hour of
SiO2 40.330
washing the membrane with demineralized water, it was repassed with
Al2O3 13.537 distilled water (Jw1, L/h.m2). Additionally, Eqs. 14–17 were used to
Fe2O3 6.044 calculate the flux recovery rate (FRR (%)), total flux decline rate (TFR
CaO 11.676 (%); total fouling), reversible flux decline rate (RFR (%); reversible
MgO 4.488
fouling), and irreversible flux decline rate (IFR (%); irreversible fouling)
SO3 0.318
Na2O 0.650 [9,44].
K2O 2.948 ( )
Jw1
TiO2 0.690 Flux recovery rate = × 100 (14)
P2O5 0.139 Jw0
ZnO 0.012
( )
Mn2O3 0.155 Jp
Cr2O3 0.013 Total flux decline rate = 1 − × 100 (15)
Jw0
SrO 0.026
L.O.Ia 18.620 ( )
Total 99.646 Jw1 − Jp
Reversible flux decline rate = × 100 (16)
a
Jw0
Loss on ignition at 1000 ◦ C.
( )
Jw0 − Jw1
where m0 (g) and m1 (g) are the masses of the membrane before and Irreversible flux decline rate = × 100 (17)
Jw0
after the chemical contact respectively.
3. Results and discussion
2.5. Application of frontal microfiltration
3.1. Characterization of raw phengite clay powder
The elaborated optimal ceramic membrane’s performance was
assessed using real wastewater filtered through a 100 μm sieve (RWW3). 3.1.1. XRF analysis
The microfiltration tests were performed at a constant pressure of 0.2 The chemical composition of the raw phengite clay in mass per
bar for 3 hours. The feed tank was refreshed every 30 minutes to reduce centages (wt.%) of the oxides is presented in Table 2. The loss on igni
and adjust for the concentration effect. The physicochemical parameters tion (L.O.I) is calculated at 1000 ◦ C for the raw clay. The clay is mainly
of the permeate such as flux, pH, electrical conductivity, suspended composed of a large amount of silica oxide (40.330%), alumina oxide
matter, and total dissolved solids were measured every 30 min of (13.537%), calcium oxide (11.676%), and iron oxide (6.044%). These
filtration. A multiparameter instrument (HACH HQ40d, U.S.A) was used oxides were found to be the main constituents of the raw clay. This
for measuring the pH and electrical conductivity of the feed and group of oxides represents about 71,587% of the total, which explains
permeate solutions. The total dissolved solids were measured with a the physical and mechanical properties of this natural clay. The SiO2/
mobile TDS meter type TDS-3 Korea. The suspended matter was detec Al2O3 mass ratio is about 3, indicating that the phengite clay is an
ted by filtering using a 0.45 μm pore size membrane. The suspended aluminosilicate [41]. A very small amount of other oxides such as MgO
matter concentration in mg/L is calculated using the differential mass (4.488%), SO3 (0.318%), Na2O (0.650%), K2O (2.948%), TiO2
ratio of the filtered water volume, Eq. (11) [6]. (0.690%), P2O5 (0. 139%), ZnO (0.012%), Mn2O3 (0.155%), Cr2O3
(M1 − M0 ) (0.013%), and SrO (0.026%) as impurities were also detected.
Suspended matter = (11)
Vw
3.1.2. XRD analysis
where M0 is the mass of empty membrane (mg), M1 is the mass of To identify the influence of thermal treatment on the mineralogical
membrane and residue after oven drying at 105 ◦ C/24 h (mg) and Vw is composition of phengite clay, XRD analysis was used on both the raw
the volume of filtered water (L). The rejection factor (%) for all exper sample and samples treated at different temperatures. The obtained XRD
imental parameters was calculated using the following relationship, Eq. diagrams are presented in Fig. 2. It should be noted that the XRD
(12) [2,35]. analysis of our raw clay was carried out in another research work [45],
( ) and the results obtained reveal the existence of several crystalline pha
XFeed − XPermeate
Rejection = × 100 (12) ses, such as quartz (Q), calcite (C), phengite (Ph), dolomite (D),
XFeed
vermiculite (V) and hematite (H). From the diffractograms of
850–900 ◦ C, we note the total decomposition of calcite and the disap
where XFeed and XPermeate are the experimental parameters of the feed
pearance of reflections of vermiculite and hematite. On the diffracto
and permeate respectively.
gram of 950 ◦ C we observed the dehydroxylation of phengite and the
appearance of the albite phase (A; NaAlSi3O8). As the temperature rises
2.6. Membrane regeneration and anti-fouling performance analysis
to 1000–1050 ◦ C, the diffractograms show the disappearance of dolo
mite and the start of crystallization of the new ceramic phase of mullite
After a filtration process, the membrane is completely washed with
(M; 3Al2O3,2SiO2). When the temperature increases to 1100–1150 ◦ C,
demineralized water or any appropriate cleaning solution (e.g., alkali or
the diffractograms indicate the elimination of albite caused by fusion at
acid solution) to eliminate the foulant and restore the original perme
about 1100 ◦ C [46], and the predominance of the mullite phase.
ability. The cleaning solution chosen is determined by the foulant va
riety as well as the nature of the membrane. The cleaning efficiency (%)
can be calculated by Eq. (13) [43]. 3.2. Characterization of the phengite clay membrane
( )
Water permeability after cleaning
Cleaning efficiency = × 100 (13) 3.2.1. Visual appearance of flat membranes
Water permeability before filtration
Fig. 3 illustrates the sintered ceramic membranes at different tem
The anti-fouling behavior of the optimal membrane was evaluated peratures from 850 ◦ C to 1150 ◦ C. The membranes’ surfaces are
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S. Lagdali et al. Case Studies in Chemical and Environmental Engineering 8 (2023) 100388
Fig. 2. XRD of phengite clay at different sintering temperatures (A: Albite, D: Dolomite, M: Mullite, Ph: Phengite, and Q: Quartz).
3.2.2. Shrinkage
The shrinkage of the membranes was calculated using the diameter
dimensions before and after the sintering process. During thermal
treatment, shrinkage is often related to the weight loss and densification
of the ceramic membranes [14]. Fig. S4 presents the percentage of
shrinkage of flat ceramic membranes sintered at various temperatures
(850 ◦ C–1150 ◦ C). It is observed that sintering temperature has a sig
nificant effect on shrinkage. As seen in the figure, when the sintering
temperature increases from 850 ◦ C to 1150 ◦ C, the shrinkage of the
membranes also increases from 1.3% to 8.6%. The densification process
(the internal rearrangement of the membrane) explains the increase in
shrinkage, which is confirmed by the SEM images. Several studies have
shown the same increasing shrinkage percentage evolution with sin
tering temperature [47,48]. The deposition of UF and NF layers becomes
more perfect when the shrinkage of the membrane supports is lower to
avoid cracking and deformation of the filter layer [28].
Fig. 4. Variation of porosity and mechanical strength with sintering
3.2.3. Porosity and mechanical strength
temperature.
Fig. 4 shows the variation of porosity and mechanical strength as a
function of sintering temperature. For the porosity, Fig. 4 illustrates two
homogenous without any sort of macro defects or ruptures. The mem
steps, the first one is in which the porosity increases from 30.3% to
branes keep the same cylindrical structure and vary in color from brick
34.5% by the increase of the sintering temperature from 850 ◦ C to
red to dark yellow when the sintering temperature increases from 850 ◦ C
1050 ◦ C. This evolution is explained by the release of CO2 from the
to 1100 ◦ C. In other words, the more the sintering temperature is
decomposition of calcium carbonates, and the combustion of organic
increased, the darker the color of the membrane will become. The
matter that exists naturally at high temperatures [49], then we observe
change in color of the flat ceramic membranes after the heat treatment is
in the second stage a decrease from 34.5% to 17.1% when the
caused by iron oxide oxidation [35]. In addition, the color of the
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S. Lagdali et al. Case Studies in Chemical and Environmental Engineering 8 (2023) 100388
Fig. 5. SEM micrographs of the surface of sintered membranes at (a) 850 ◦ C, (b) 900 ◦ C, (c) 950 ◦ C, (d) 1000 ◦ C, (e) 1050 ◦ C, (f) 1100 ◦ C, and (g) 1150 ◦ C.
6
S. Lagdali et al. Case Studies in Chemical and Environmental Engineering 8 (2023) 100388
Fig. 6. (a) The average pore diameter of the membranes as a function of sintering temperature, and (b) pore size distribution of the optimal membrane sintered at
1050 ◦ C/2h.
Fig. 7. Evolution of water flux, (a) as a function of time at different pressures, and (b) as a function of applied pressure.
temperature increases from 1050 ◦ C to 1150 ◦ C. This is due to the [33]. Then the water absorption decreases from 19.3% to 7.8% when the
densification of the porous structure and the agglomeration of the grains temperature varies from 1050 ◦ C to 1150 ◦ C. This decrease is explained
with the increase of the sintering temperature [50,51]. The sintering by the densification phenomenon of the ceramic material [28]. This
temperature can also be stated to have a considerable influence on the allows the formation of a high-density ceramic membrane and improves
porosity of the membranes. The optimal sintering temperature chosen to its mechanical properties. The presence of alkaline and alkaline-earth
continue our study is 1050 ◦ C, due to the highest porosity (34.5%). The oxides such as MgO, Na2O, and K2O favors the formation of glassy
optimal ceramic membrane must have good mechanical strength and be phases strongly responsible for the reduction of water absorption by
strong enough to resist all the hydraulic pressures applied during the filling the pore volume of the membrane materials [35]. On the other
filtration process. The mechanical strength of the ceramic membranes hand, an inverse behavior was recorded for the bulk density, which
increases from 14.9 MPa to 29.5 MPa when the sintering temperature decreased from 1.81 g/cm3 to 1.77 g/cm3, when the temperature in
increases from 850 ◦ C to 1150 ◦ C with the optimal membrane exhibiting creases from 850 ◦ C to 1050 ◦ C. Then increases from 1.77 g/cm3 to 2.2
a value of 26.7 MPa. The increase is primarily attributable to the g/cm3 when the temperature increased from 1050 ◦ C to 1150 ◦ C which
densification and vitrification of some phases, namely amorphous silica, was due to the formation of a very viscous silica phase that facilitated
and albite, as well as the crystallization of more resistant phases, such as the crystallization of mullite [52]. In addition, it also indicates the for
mullite [14,35]. A similar progression was identified for the membranes mation of a solid ceramic body through the densification of the material.
fabricated from natural Moroccan clay [50]. These results are in perfect Bulk density and porosity are inversely proportional, therefore the re
agreement with the SEM images. sults of density confirm the results of porosity [28].
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S. Lagdali et al. Case Studies in Chemical and Environmental Engineering 8 (2023) 100388
Fig. 8. (a) Permeate flux of RWW3 as a function of filtration time, (b) pH of RWW3 permeate as a function of filtration time, and (c) rejection of suspended matter,
TDS, and electrical conductivity of the RWW3 as a function of filtration time, (Experimental conditions: ΔP = 0.2 bar, T = 25 ◦ C).
Fig. 9. (a) RWW1, RWW2, and RWW3 before and after MF treatment, and (b) RWW3 microfiltration mechanism using our optimal ceramic membrane, (Experi
mental conditions: ΔP = 0.2 bar, T = 25 ◦ C).
morphology. It can be seen that the surface of the ceramic membranes 850 ◦ C, 900 ◦ C, and 950 ◦ C are weakly sintered and the grains of the clay
does not show any defects such as micro-cracks, which confirms that the powder are not well compacted with each other. This confirms the in
membranes are of very good quality. The ceramic membranes treated at crease in porosity (from 30.3% to 31.7% respectively). At 1000 ◦ C,
8
S. Lagdali et al. Case Studies in Chemical and Environmental Engineering 8 (2023) 100388
Table 3 start of material densification. The same evolution has been observed in
Physicochemical characteristics of feed and permeate recovered after 3 hours of several works [54,55]. Fig. 6b represents the pore size distribution of the
microfiltration, (Experimental conditions: ΔP = 0.2 bar, T = 25 ◦ C). optimal sintered membrane at 1050 ◦ C. The figure shows that the
Physicochemical characteristics RWW3 membrane has a single peak, which represents a unimodal distribution
Feed Permeate Rejection (%)
of the pore size. The average diameter is about 3.9 μm. Note that 78.6%
of the pores have a diameter d < 3.9 μm.
pH 8.4 8.7 –
Electrical Conductivity (μS/cm) 3616 1224 66.2
TDS (ppm) 2170 612 71.8 3.2.7. Permeability of the optimal ceramic membrane
Suspended matter (mg/L) 40 0 100 Permeability is an essential property to verify the performance of the
prepared ceramic membrane. Fig. 7a illustrates the evolution of water
flux measured at three different pressures (0.1, 0.15, and 0.2 bar) during
sintering becomes increasingly significant due to the phenomenon of 180 min. According to Fig. 7a, when the pressure varies from 0.1 to 0.2
densification, but is still not satisfactory to obtain excellent cohesion bar the water flux varies from 4.77 to 8.52 L/h.m2. The two fluxes
between the clay powder grains. When the temperature rises to 1050 ◦ C, measured at 0.15 and 0.2 bar decrease slightly with time until they have
the membrane has a uniform porous structure and the pores between the established a stable flux after 60 minutes, and the flux measured at 0.1
grains are relatively large, which is explained by the better porosity bar remains stable during the filtration. Fig. 7b shows a linear evolution
(34.5%). At 1100 ◦ C we observed that the densification continues its of the water flux when the pressure increases from 0.1 to 0.2 bar. This
evolution due to the partial vitrification of the amorphous silica and confirms the verification of Darcy’s law [56]. Pressure is the only driving
some impurities present in the clay material [19,35]. Vitrification force for permeation. The water permeability of the sintered ceramic
already dominates at the final sintering temperature of 1150 ◦ C and the membrane at 1050 ◦ C/2h obtained through the slope of the line is 43.50
pores are almost partially closed, which explains the low porosity value L/h m2 bar.
(17.1%) [8,53].
3.2.8. Chemical resistance
3.2.6. Average pore diameter and pore size distribution The corrosion chemical resistance of the optimal ceramic membrane
The average pore diameter of the elaborated ceramic membranes sintered at 1050 ◦ C was shown in Fig. S6. Two media were chosen to
and the pore size distribution of the optimal membrane were evaluated evaluate the weight loss for 7 days, acidic (HCl; pH = 1) and basic
through the Image J software. Fig. 6a presents that the average pore (NaOH; pH = 13.5). The ceramic membrane lost 4.6% of its weight after
diameter increases from 2.1 μm to 12.3 μm when the sintering tem immersion in the acidic solution. Then in the basic medium, the ceramic
perature varies from 850 ◦ C to 1150 ◦ C. The opening of the pores with membrane has excellent chemical resistance, and the weight loss does
temperature is caused by the agglomeration of the clay grains and the not exceed 0.6% during 7 days. The same evolution of chemical
Table 4
Comparison of the properties of the manufactured membrane with those of various MF membranes.
Membrane material Sintering Porosity Pore Permeability (L/ Mechanical Feed (Concentration/ Applied Rejection Reference
temperature (%) size h.m2.bar) strength (MPa) Turbidity/Suspended pressure (%)
(◦ C) (μm) matter) (bar)
Natural Moroccan clay 1100 28.11 2.5 928 17.5 Tannery beam house 0.14 99.80 [20]
and phosphate effluent (760 NTU)
Raw seawater (120 99.62
NTU)
Synthetic solution of 99.86
aluminum chloride (at
high pH) (725 NTU)
Natural kaolin clay 1250 27 0.73 20 28 Cuttlefish effluent (335 3 99 [24]
NTU)
− 9
Natural kaolin clay 850 34.5 2.28 6.12 × 10 (m 7.1 Methylene 10 1.5 99.07 [25]
Pa− 1 s− 1) blue dye mg/L
100 93.45
mg/L
Natural Moroccan 950 52.11 1.70 1433.46 21.68 Agro-food effluent 0.12 97 [27]
perlite (224 NTU)
Tannery effluent (36 96
NTU)
Natural magnesite clay 1100 48.15 1.12 922 6.1 Industrial textile 0.12 99.9 [28]
wastewater (144.5 ±
0.6 NTU)
Pyrophyllite clay 1150 40.50 0.80 1000 30 Raw seawater (20 1 99.40 [41]
NTU)
Mineral coal fly-ash 800 51 0.25 475 19.5 Textile dye wastewater 1 98.72 [54]
(45.5 NTU)
Alumina membrane - - 0.2 1022 – Beamhouse effluent 1 98–99 [64]
(commercial (132 NTU; suspended
ceramic membrane) matter = 4.32 g/L)
Textile effluent (219 89–94
NTU; suspended
matter = 6.50 g/L)
Dicing effluent (132 100
NTU; suspended
matter = 2.74 g/L)
Natural Moroccan 1050 34.5 3.9 43.50 26.7 RWW3 (suspended 0.2 100 This work
phengite clay matter = 40 mg/L)
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S. Lagdali et al. Case Studies in Chemical and Environmental Engineering 8 (2023) 100388
Fig. 10. (a) Permeability of the membrane after washing with demineralized water, (b) clogged and washed membrane, (c) Jw0, Jp, and Jw1 as a function of filtration
time (Experimental conditions: ΔP = 0.2 bar, T = 25 ◦ C), and (d) fouling parameters.
resistance as a function of time has been reported in the literature [20, cake. Furthermore, this cake gives additional hydraulic resistance to the
57,58]. The loss of mass in the concentrated NaOH solution is negligible, membrane, which finally leads to the fouling of the membrane [39]. This
demonstrating its potential use in the pretreatment of highly alkaline fouling behavior is commonly encountered in the microfiltration process
media. In addition, chemical cleaning of our membrane with an alkaline as reported by Iaich et al. [6]. Fig. 8b shows the evolution of pH as a
solution at ambient temperature is preferable to cleaning with an acidic function of filtration time. The pH values remain constant during the
solution. The results of chemical resistance obtained indicate, that the microfiltration process. It should be noted that the pH goes from 8.4 in
ceramic membrane elaborated at 1050 ◦ C is efficient and desirable for the feed to 8.7 in the permeate and thereafter we noticed stability. This
microfiltration applications of industrial or urban wastewater. evolution could be explained by the elimination of the bio-organic
matter present in RWW3, which generally has an acid character [28,38].
3.3. Microfiltration of RWW3 Fig. 8c presents the variation of TDS, suspended matter, and elec
trical conductivity removal with filtration time. The TDS rejection rate
In the present study, we used the optimal membrane to conduct a increases from 26.3% to 71.8% after 3 hours of filtration. This evolution
practical application of frontal microfiltration of pre-treated real can be linked to the adsorption of TDS on the filtration surface. On the
wastewater RWW3. The objective was to evaluate the purification per other hand, the suspended matter was completely removed. This
formance of our membrane. This type of wastewater is saturated with removal attained 100% during the frontal microfiltration period. The
organic matter, suspended solid particles, and chemical components larger particle size of the RWW3 is the main reason for the removal of
coming from the leaching products of the used clothes. Some of the suspended matter by our ceramic membrane [61]. The removal of TDS
detergents can produce allergies and can be hazardous to human health. and the suspended matter is caused by the accumulation of rejected
Therefore, this water must be treated to protect the environment [28]. particles forming a deposit on the membrane’s surface, which partially
Fig. 8a plots the variation of permeate flux with time for the sintered reduces pore size. This phenomenon is generally observed in the
membrane at 1050 ◦ C under 0.2 bar pressure for 180 min. The permeate microfiltration process [2,62,63]. Concerning electrical conductivity,
flux decreases with time from 4.13 L/h.m2 to 2.58 L/h.m2, then stabi the rejection rate is significant as a function of time, it goes from 11.5%
lizes after 120 min. These results can be explained by the clogging of the to 66.2% after 3 hours of filtration. This evolution is mainly linked to the
ceramic membrane by particles finer than the pores [6,59,60]. The deposition and adsorption of dissolved salts on the cake that was created
reduction in permeate flux is caused by the adsorption of solid and by the accumulation of large solid particles on the filtering surface of our
colloidal particles or micro-organisms on the filtering surface of the ceramic membrane [24].
membrane and the subsequent formation of a deposit in the form of a Fig. 9a illustrates the complete removal of suspended matter
10
S. Lagdali et al. Case Studies in Chemical and Environmental Engineering 8 (2023) 100388
11
S. Lagdali et al. Case Studies in Chemical and Environmental Engineering 8 (2023) 100388
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