Comparative Study of Ceramic Membranes Developed on Different Algerian Natural Clays for Industrial Effluent Filtration

Citation Hamoudi L Akretche DE Hadadi A Amrane A Mouni L Comparative Study of Ceramic Membranes Developed on Different Algerian Natural Clays for IndustrialEffluent Filtration Minerals 2023 13 273 https doiorg103390min13020273 Academic Editors Nevenka Rajic and Jelena Pavlovic Received 16 January 2023 Revised 10 February 2023 Accepted 14 February 2023 Published 15 February 2023 Copyright 2023 by the authors Licensee MDPI Basel Switzerland This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution CC BY license https creativecommonsorglicensesby 40 minerals Article Comparative Study of Ceramic Membranes Developed on Different Algerian Natural Clays for IndustrialEffluent Filtration Leyla Hamoudi 1 Djamel Eddine Akretche 1 Amina Hadadi 2 Abdeltif Amrane 3 and Lotfi Mouni 2 1 Laboratory of Hydrometallurgy and Inorganic Molecular Chemistry Faculty of Chemistry University of Science and Technology Houari Boumediene BP 32 El Alia Bab Ezzouar 16111 Algeria 2 Laboratoire de Gestion et Valorisation des Ressources Naturelles et Assurance Qualité Faculté SNVST Université de Bouira Bouira 10000 Algeria 3 Ecole Nationale Supérieure de Chimie de Rennes CNRS ISCRUMR6226 Université de Rennes F35000 Rennes France Correspondence abdeltifamraneunivrennes1fr AA lmouniunivbouiradz LM Abstract This research is based on the deposition of ceramic membranes made from Algerian clays within tubular supports The major objective is to compare the mechanical strength and water permeability of the developed supports The membranes made from the same clays are then examined in terms of their application areas and efficacy in treating a localcheese effluent The study of these clays demonstrates that the tubular supports made from Aomar clay are more robust than those obtained from kaolin and bentonite This was due to the higher calcination temperature which was 1000 C for Aomar and kaolin clays and 800 C for bentonite However the tubular support based on kaolin has the maximum water permeability 146009 Lm2hbar In addition the permeability tests performed on the membranes deposited on these clays indicate that those of bentonite and Aomar clay are ultrafiltration membranes whereas the membrane obtained from kaolin is a microfiltration membrane We demonstrated that the three membranes show high efficiency for the clarification and retention of multiplepollutant loads of a localcheese effluent Keywords Algerian clays ceramic membranes microfiltration and ultrafiltration membranes industrialeffluent treatment 1 Introduction Water is a vital resource for human existence and progress in a variety of industries such as agriculture and manufacturing Therefore it must be maintained clean and func tional Nonetheless the most technologically advanced human activities have led to its contamination and unfortunately it is discharged into the environment as effluents without any prior treatment 12 According to their composition these effluents are poisonous and their use is hazardous to ordinary living While certain effluents pickling bath surface treatment etc pose major pollution concerns others such as those from the agrifood industry are highly polluting yet readily biodegradable and profitable dairies sugar facto ries starch processing fruit and vegetable conversion etc 3 The color of other effluents such as those from the paper andor textile industries has a considerable aesthetic influ ence on the aquatic environment Consequently it is essential to treat them prior to their release into the natural environment In the dairy industry rejected waters are contaminated by cleaning washing and disinfecting chemicals sterilizers and other dairy products 45 all of this pollution demonstrates that dairy effluents are substantially polluted with both mineral and organic pollutants posing a significant threat to the environment when discharged untreated into aquatic receiving media 46 The purification of wastewaters entails enhancing their physicochemical and biological properties so that the treated water fulfills the needed criteria 78 In this regard a number Minerals 2023 13 273 httpsdoiorg103390min13020273 httpswwwmdpicomjournalminerals Minerals 2023 13 273 2 of 19 of procedures have been used for the treatment of wastewater including physicochemical processes such as adsorption 912 coagulationflocculation 1316 and advanced oxi dation processes 17 microorganismbased biological treatment was also used to reduce carbon nitrogen and phosphate contamination notably in dairy effluents 18 methods of membrane separation using the osmosis phenomena 19 and membranefiltration processes such as nanofiltration ultrafiltration and microfiltration membranes 20 Membrane filtration is an increasingly popular technology for treating wastewater due to its high efficiency and versatility in removing various contaminants This technology involves the use of semipermeable membranes to separate solids and dissolved substances from wastewater Over the past few decades significant progress has been made in the development and application of membranefiltration systems making it a viable alterna tive to traditional treatment methods such as sedimentation and chemical precipitation According to recent studies 2122 membrane filtration has shown promising results in terms of waterquality improvement and cost effectiveness The separation mechanism in membrane filtration is based on the sizeexclusion prin ciple where the pores in the membrane act as a physical barrier to separate contaminants from the wastewater The pore size of the membrane can be adjusted to target specific contaminants such as bacteria viruses and organic matter The separation mechanism can be further enhanced by combining membrane filtration with other treatment processes such as coagulation and flocculation 23 The efficiency of the separation process is also influenced by various factors including the pressure difference across the membrane the temperature and pH of the wastewater and the type of membrane material used 24 Studies have shown that the use of membrane filtration in wastewater treatment can result in high removal rates for various contaminants including pathogens eg Escherichia coli and coliphages 22 nutrients eg nitrogen and phosphorus 25 and emerging contaminants eg pharmaceuticals and personalcare products 26 The separation mechanism in membrane filtration provides a sustainable and costeffective solution for addressing the growing challenges in wastewater treatment The increasing demand for clean water and the stringent regulations for water quality have driven the need for further research and development in the field of membrane filtration Microfiltration MF and ultrafiltration UF are two commonly used membrane filtration processes for wastewater treatment MF is a lowpressure filtration process that uses membranes with pore sizes ranging from 01 to 10 µm The main goal of MF is to remove suspended solids and colloidal particles from the wastewater resulting in the improvement of water clarity and turbidity 27 UF on the other hand uses membranes with pore sizes ranging from 001 to 01 µm and operates at higher pressures than MF The objective of UF is to remove dissolved substances including proteins organic molecules and pathogens from the wastewater 28 Both MF and UF have been widely applied in various wastewatertreatment appli cations such as municipalwastewater treatment industrialwastewater treatment and desalination MF and UF are also compatible with other treatment processes such as adsorption and oxidation which can further improve the removal efficiency of contami nants 29 The use of MF and UF in wastewater treatment has been shown to result in high removal rates for various contaminants such as bacteria organic matter and nutrients The combination of MF and UF provides a flexible and costeffective solution for addressing the complex challenges in wastewater treatment Ceramic membranes are a type of membranefiltration technology that is gaining increasing attention for its potential in wastewater treatment Ceramic membranes are made from inorganic materials such as alumina zirconia and titania and are known for their high mechanical strength and chemical stability 30 Compared to polymeric membranes ceramic membranes offer several advantages such as higher temperature and pH tolerance better resistance to fouling and longer membrane life 31 However ceramic membranes also have some disadvantages such as high cost low flexibility and limited availability of pore sizes 32 Furthermore ceramic membranes have a relatively high Minerals 2023 13 273 3 of 19 permeation resistance which can result in lower permeate flux compared to polymeric membranes 33 Despite these limitations ceramic membranes have shown promising results in wastewatertreatment applications particularly in the removal of challenging contaminants such as heavy metals organics and pathogens 30 In comparison to polymeric membranes ceramic membranes have been shown to provide higher removal efficiency and longterm stability in various wastewatertreatment processes Overall ceramic membranes are a promising technology for wastewater treatment offering high performance and durability while also addressing some of the challenges associated with polymeric membranes Recently the use of clay as a raw material for synthesizing ceramic membranes has gained attention as a sustainable and lowcost alternative to traditional ceramic materials Clay is abundant and widely available making it an attractive option for largescale pro duction of ceramic membranes Additionally clay has good plasticity and can be molded into various shapes and sizes providing flexibility in the design of ceramic membranes 34 Studies have shown that claybased ceramic membranes can provide high performance in various wastewatertreatment applications including the removal of pathogens organic pollutants and heavy metals 35 Furthermore claybased ceramic membranes have demonstrated good mechanical strength and chemical stability making them a promising alternative to traditional ceramic membranes The use of clay as a raw material for syn thesizing ceramic membranes has the potential to make this technology more accessible and costeffective while also providing high performance and durability in wastewater treatment applications Further research is needed to optimize the synthesis process and enhance the performance of claybased ceramic membranes making them a viable option for wider implementation in wastewater treatment The aim of this work is to evaluate the effectiveness of three synthetized claybased ceramic membranes in purifying cheese effluent based on their performance compared to the standards set by the World Health Organization WHO as referenced in the official journal of the Algerian Republic For this purpose three Algerian clays namely bentonite from northwestern Algeria kaolin from northeastern Algeria and clay from Aomar in the central north of the country were selected for the study to our knowledge such work has never been undertaken before 2 Materials and Methods 21 Raw Materials Local clays Algerian from various regions are used to develop tubular supports including bentonite from Maghnia located in northwestern Algeria kaolin from Tamazert located in northeastern Algeria and clay from Aomar in the central north of the country which is used in the production of red brick An Xrayfluorescencespectroscopy study using a spectrometer S8 TIGER Bruker Germany was undertaken to identify the chemical composition of each kind of clay 22 Preparation of Ceramic Paste The optimal formulation of ceramic pastes using various types of clay has been developed to possess the requisite rheological characteristics including homogeneity cohe sion porosity and extrusiondeformation capacity ensuring their suitability for intended applications 36 Each type of clay is sieved through a 75 µm sieve mixed with water and organic additives starch with the chemical formula C6H10O5nfrom FlukaBiochemika methocel which is a cellulosic derivative with the chemical name hydroxypropyl methylcellulose and from The Dow Chemical Company amijel which is a derivative product consisting of pregelled starch Cplus12072 cerestar These organic additives play a vital role in tubularsupport shaping and providing acceptable physical and mechanical qualities after sintering 37 Minerals 2023 13 273 4 of 19 23 Extrusion of Ceramic Paste Extrusion of the previously produced ceramic paste is used to construct tubular supports It is based on the idea of compressing the paste in a cylinder which is put on another cylindrical molded component to produce singlechannel tubular supports with welldefined diameters 3839 Following extrusion the supports are air dried for 6 days before being heat treated in a furnace Nabertherm GmbH Lilienthal Germany using a twostage thermal program Figure 1ac show the experimental procedures for this preparation including all of the tubular supports produced for each kind of clay the thermal program used for sintering them and a schematic depiction of the thermal program used for sintering the tubular supports Minerals 2022 12 x FOR PEER REVIEW 4 of 17 Each type of clay is sieved through a 75 µm sieve mixed with water and organic additives starch with the chemical formula C6H10O5nfrom FlukaBiochemika methocel which is a cellulosic derivative with the chemical name hydroxypropyl methylcellulose and from The Dow Chemical Company amijel which is a derivative product consisting of pregelled starch Cplus12072 cerestar These organic additives play a vital role in tub ularsupport shaping and providing acceptable physical and mechanical qualities after sintering 37 23 Extrusion of Ceramic Paste Extrusion of the previously produced ceramic paste is used to construct tubular sup ports It is based on the idea of compressing the paste in a cylinder which is put on another cylindrical molded component to produce singlechannel tubular supports with wellde fined diameters 3839 Following extrusion the supports are air dried for 6 days before being heat treated in a furnace Nabertherm GmbH Lilienthal Germany using a two stage thermal program Figure 1ac show the experimental procedures for this prepara tion including all of the tubular supports produced for each kind of clay the thermal program used for sintering them and a schematic depiction of the thermal program used for sintering the tubular supports drying in the air dry and high temperature sintering tubular ceramic supports extrusion after restingand obtaining tubular supports let the ceramic paste rest for 24 hours Obtaining a ceramic paste mixing the mixture with water mix of 84 of clay 4 of Amijel 4 of Méthocel 8 of Amidon a b For tubular supports of bentonite 345 385 115 565 525 3 hours 0 800C 2Cminutes Time min Temperature C 1000C 5Cminutes 250 C 2 hours 3 hours 235 For tubular supports of Kaolin and Aomar clays 20 C Compressor Feed tank Valve Manometer Membrane support Water pump Filtration module Permeate c d Figure 1 Representative figures of the a flowchart of the main procedures followed for the elabora tion of tubular ceramic supports b tubular supports obtained for each type of clay c schematic representation of the thermal program followed for the sintering of the tubular supports and d schematic representation of used filtration pilot Minerals 2023 13 273 5 of 19 24 Mechanical and Physical Properties of Tubular Supports before and after Sintering The outer and inner diameters lengths and thicknesses of the elaborated tubular supports were measured with a caliper before during and after drying and sintering to determine their physical properties To regulate the resistance of the tubular supports the mechanical properties of the supports produced after sintering were determined by measuring their mechanical resis tance using the threepoint bending technique with a TLSTechlabsystem instrument Lezo Spain The objective of this measurement is to position a sample of a solid material on two simple supports and apply a force to the samples center until it fractures and then read the breakingstrength data 25 Test of Water Permeability for Tubular Supports Following sintering the tubular supports were cut to 15 cm and tested for permeability using a closedcircuit filtering pilot see Figure 1d This pilot consists of a feed tank a water pump a filter module including the support two pressure regulators and a compressor used to apply varying pressures 26 Membrane Preparation and Deposition Our membranes were manufactured by preparing a slip consisting of a mass percent age W combination of 30 W polyvinyl alcohol gel 12 W PVA in water 65 W water and 5 W clay powder sieved through 40 µm 39 Slipcasting is the technique used for the deposition of membranes of each type of clay It consists of placing the tubular supports which are blocked at one end in a vertical position and then filling them with the slip during a specific time of engobing then allowing them to air dry for 24 h to allow the excess slip to drip off The membranes placed on the inner surface of the tubular supports are consolidated using heat treatment at the optimal sintering temperature for each membrane 750 C for the bentonitebased membrane and 900 C for the kaolin and Aomarclaybased membranes It is essential to note that the optimal sintering temperature for each membrane was determined based on their homogeneity and adhesion to the inner walls of the tubular supports 27 Determination of the Field of Application of Each Membrane Determining the area of application for ceramic membranes is a crucial stage in the membranefiltration process in order to determine the type of the effluent that will be filtered on each membrane 37 Figure 1d depicts a filtration pilot used to test the permeability to pure water of our newly designed membranes We were able to identify the area of application for our membranes based on the findings obtained by comparing the volumeflowdensity order with that of different membrane techniques described in the literature 37 28 The Efficiency of Membranes for Filtration of a Cheese Effluent Filtration of a cheese effluent from the TARTINO cheese situated in the Rouiba indus trial zone was used to evaluate the performance of our newly designed membranes central north of Algeria The effluent was injected into the feed tank while the support containing the ceramic membrane was installed within the module Figure 1d and exposed to varying pressures of effluent circulation Following filtration various physicochemical pollution characteristics were analyzed for each permeate collected in Erlenmeyer flasks for each applied pressure as well as the unfiltered effluent returned to the feed tank Table 1 depicts the pollutant metrics evaluated and their limit levels regarding Algerian industrial discharges Minerals 2023 13 273 6 of 19 Table 1 Limit values of some physicochemical parameters of pollution in industrial rejection in Algeria Parameters Temperature T C pH SP mgL Conductiviy µSCm Turbidity NTU Phosphates mgL Nitrates mgL Nitrite mgL Ammonium mgL BOD5 mgL COD mgL Limit values 30C 6585 35 2500 80 10 30 3 5 35 120 SP Suspended particles BOD5 Biologicaloxygen demand COD Chemicaloxygen demand Minerals 2023 13 273 7 of 19 3 Results and Discussions 31 Characterization of the Raw Materials The findings produced by the Xrayfluorescence analysis are stated in the oxide equivalent for each atom present in each clay see Table 2 The Xrayfluorescence analysis of the three clays showed that they are composed of several metal oxides with different proportions The silicates and alumina form the main composition of each clay studied This outcome aligns with the findings in the study of natural zeolitebased clay ceramic membranes 40 32 Physical and Mechanical Characteristics of Tubular Supports Table 3 shows the physical and mechanical properties of tubular supports produced without membrane from each kind of clay The table demonstrates that the fabricated tubular supports underwent volume shrink age during air drying represented by VSd and volume shrinkage during sintering rep resented by VSs The tubular supports prepared on the basis of bentonite have a higher volume shrinkage compared to those based on the kaolin and Aomar clays These two phenomena linked to VSd and VSs have been explained in the literature by the disappear ance of the water used for the production of ceramic pastes during drying in addition to the removal of organic additives included in the paste during sintering 41 Furthermore mechanical resistance to ceramic while drying as well as the disappearance of bending reveal that tubular supports made of Aomar clay are more robust than those made of kaolin and bentonite 2102 Mpa 186 Mpa and 1384 Mpa respectively This finding is explained by the difference in the rate of lime CaO in the three clays which is larger in Aomar clay 1318 compared to Kaolin 615 and bentonite 237 Indeed recent studies have demonstrated that increasing the quantity of lime in clays enhances thermal stability and mechanical strength 4243 33 Determination of the Water Permeability of Tubular Supports The permeability of the supports based on each clay was measured by applying the wellknown relationship 1 44 to investigate the fluctuation of the permeation flux with distilled water through the support until it reaches stability Figure 2 shows the Studys findings for each kind of clay Jw V S t 1 where Jw is the water permeate flux V the volume collected after each 10 min S represents the support surface S 2πrL and t is the time required to collect the same volume of water after every 10 min The data in Figure 2 clearly illustrate the fact that the permeate flow diminishes with time in all examined tubular supports and stabilizes after 40 min for each applied pressure This fluxstability finding is consistent with previous research which reveals that the permeation flux often stabilizes within 30 or 40 min 373945 Using the relation 2 46 we were able to calculate the water permeability Lp for the tubular supports that corresponded to each kind of clay via the graphical depiction of the flux fluctuation as a function of applied pressure Jw fP Lp Jw P 2 were P is the effective transmembranepressure difference and Jw the steady flow of the applied pressure The findings reveal that the flux variation as a function of pressure is linear for all of the supports investigated Furthermore the permeability computed for each support see Figure 3a shows that kaolin has a larger permeability than the Aomar and bentonite clays 146009 Lm2 bar 57073 Lm2 h bar and 8311 Lm2 bar respectively Minerals 2023 13 273 8 of 19 Table 2 Chemical composition of the clays in mass percentageW Designation SiO2 Al2O3 CaO Fe2O3 MgO TiO2 Na2O P2O5 K2O Mn2O3 SO3 Bentonite 6329 1990 237 197 292 015 238 004 191 005 001 Aomar clay 5183 1685 1318 869 196 099 135 019 202 016 017 Kaolin 5785 2425 615 349 042 038 016 012 346 004 011 Table 3 Physicalmechanical characteristics of the tubular supports obtained from each type of clay Tubular Support Length L Outside Diameter Dout and Inside Dins Just after Extrusion Length L Outside Diameter Dout and Inside Dins after Drying Better Sintering Temperature Length L Outside Diameter Dout and Inside Dins after Sintering Volumetric Shrinkage after Drying VSd and after Sintering VSs Mechanical Resistance to Bending MPa Bentonitebased support L 190 mm Dout 14 mm Dins 9 mm L 182 mm Dout 11 mm Dins 65 mm 800 C L 172 mm Dext 10 mm Dins 6 mm VSd 247 VSs 141 1384 AomarClayBased support L 190 mm Dout 14 mm Dins 9 mm L 188 mm Dout 13 mm Dins 8 mm 1000 C L 187 mm Dout 125 mm Dins 75 mm VSd 812 VSs 436 2102 KaolinBased support L 190 mm Dout 14 mm Dins 9mm L 185 mm Dout 12 mm Dins 7 mm 1000 C L 183 mm Dout 11 mm Dins 6 mm VSd 1654 VSs 932 186 Minerals 2023 13 273 9 of 19 1 2 Minerals 2022 12 x FOR PEER REVIEW 8 of 17 10 20 30 40 50 60 800 1200 1600 2000 2400 2800 3200 3600 4000 Jw Lhm2 time minute for 05 bar for 1 bar for 15 bar for 2 bar c Figure 2 Variation in the permeation flux with distilled water as a function of time for the a sup port based on bentonite b support based on Aomar clay and c support based on kaolin Using the relation 2 46 we were able to calculate the water permeability Lp for the tubular supports that corresponded to each kind of clay via the graphical depiction of the flux fluctuation as a function of applied pressure Jw fP Lp Jw ΔP 2 were P is the effective transmembranepressure difference and Jw the steady flow of the applied pressure The findings reveal that the flux variation as a function of pressure is linear for all of the supports investigated Furthermore the permeability computed for each support see Figure 3a shows that kaolin has a larger permeability than the Aomar and bentonite clays 146009 Lm2 bar 57073 Lm2 h bar and 8311 Lm2 bar respectively Figure 2 Variation in the permeation flux with distilled water as a function of time for the a support based on bentonite b support based on Aomar clay and c support based on kaolin Minerals 2023 13 273 10 of 19 Minerals 2022 12 x FOR PEER REVIEW 9 of 17 05 10 15 20 0 500 1000 1500 2000 2500 3000 Pressures bars 3 2 a Lp 8311 Lm2hbar b Lp 57073 Lm2hbar c Lp 146009 Lm2hbar Jw Lh m2 1 a 00 05 10 15 20 25 30 35 40 0 200 400 600 800 1000 1200 1400 1600 1800 6 5 4 a Lp 7169 Lm2hbar b Lp 1512 Lm2hbar c Lp 54737 Lm2hbar Jw Lh m2 Pressures bars b Figure 3 a Variation of the flux as a function of the applied pressure for the support based on 1 bentonite 2 Aomar clay 3 kaolin and for the membranes developed based on b 4 bentonite 5 Aomar clay and 6 kaolin 34 The Water Permeability of Membranes Developed The permeability of membranes produced from the investigated clays was calculated using the same approach as the permeability of the previously indicated supports The acquired findings are shown in Figure 3b The various domains of application of membranes ultrafiltration microfiltration and nanofiltration have been characterized in the literature based on permeability to dis tilled water and appliedpressurevalue intervals 3747 In this regard the values obtained for the Lp permeability of different membranes in Figure 3b indicate that the membranes based on bentonite and Aomar clays are ultrafil tration membranes with values of Lp 7169 and 1512 Lm2hbar respectively and the membrane based on kaolin is a microfiltration membrane with a value of Lp 54737 Lm2hbarThe comparison of our findings with prior studies on natural zeolitebased ce ramic membranes highlights the application of these membranes for ultrafiltration and nanofiltration 354448 These studies have demonstrated their efficacy in filtering saline water and retaining monovalent and bivalent metals 35 The Study of the Efficiency of Our Membranes in the Filtration of a Local Effluent Our filtering membranes are specifically aimed at filtration of a localcheese effluent This is because the effluent needs to undergo special treatment to reduce its organic and inorganic contaminant levels prior to being released into the environment 4749 Figure 4 shows the difference in appearance of the effluent before and after filtration with varying transmembrane pressures on the developed membranes as well as the liq uid in the feed tank The images reveal that before filtration the effluent has a white tint with high turbidity However after filtration through the microfiltration and ultrafiltra tion membranes at various pressures the resulting permeate is clear and transparent in dicating the effectiveness of the membraned in clarifying the effluent The dark color and high turbidity of the liquid in the feed tank also supports this result 1 Figure 3 a Variation of the flux as a function of the applied pressure for the support based on 1 bentonite 2 Aomar clay 3 kaolin and for the membranes developed based on b 4 bentonite 5 Aomar clay and 6 kaolin 34 The Water Permeability of Membranes Developed The permeability of membranes produced from the investigated clays was calculated using the same approach as the permeability of the previously indicated supports The acquired findings are shown in Figure 3b The various domains of application of membranes ultrafiltration microfiltration and nanofiltration have been characterized in the literature based on permeability to distilled water and appliedpressurevalue intervals 3747 In this regard the values obtained for the Lp permeability of different membranes in Figure 3b indicate that the membranes based on bentonite and Aomar clays are ultrafiltra tion membranes with values of Lp 7169 and 1512 Lm2hbar respectively and the mem Minerals 2023 13 273 11 of 19 brane based on kaolin is a microfiltration membrane with a value of Lp 54737 Lm2hbar The comparison of our findings with prior studies on natural zeolitebased ceramic mem branes highlights the application of these membranes for ultrafiltration and nanofiltra tion 354448 These studies have demonstrated their efficacy in filtering saline water and retaining monovalent and bivalent metals 35 The Study of the Efficiency of Our Membranes in the Filtration of a Local Effluent Our filtering membranes are specifically aimed at filtration of a localcheese effluent This is because the effluent needs to undergo special treatment to reduce its organic and inorganic contaminant levels prior to being released into the environment 4749 Figure 4 shows the difference in appearance of the effluent before and after filtration with varying transmembrane pressures on the developed membranes as well as the liquid in the feed tank The images reveal that before filtration the effluent has a white tint with high turbidity However after filtration through the microfiltration and ultrafiltration membranes at various pressures the resulting permeate is clear and transparent indicating the effectiveness of the membraned in clarifying the effluent The dark color and high turbidity of the liquid in the feed tank also supports this result Minerals 2022 12 x FOR PEER REVIEW 10 of 17 Figure 4 Representative image of the visual appearance of the effluent a before filtration on the developed membranes b after filtration on the developed membrane based on bentonite c after filtration on the developed membrane based on Aomar clay and d after filtration on the developed membrane based on kaolin Tables 46 shows the results of physicochemicalpollutantparameter analyses per formed on our samples before and after membrane filtration Table 4 Results of the physicochemical pollution parameters measured on the studied effluent using membrane based on bentonite UF Membrane Parameter of Pollution Measured Effluent before Filtration Permeate Collected at 1 bars Permeate Collected at 2 bars Permeate Collected at 3 bars Permeate Collected at 4 bars Effluent Re tained in the Feed Tank Membrane based on Bentonite UF Turbidity NTU 2400 108 105 102 122 2812 Conductivity µS 2170 773 762 753 758 632 Ammonium NH4 mgL 592 305 191 138 232 4724 Nitrites NO2 mgL 288 084 056 048 116 2212 Nitrates NO3 mgL 768 975 78 549 105 4815 Phosphates PO43 mgL 297 1002 460 233 082 27423 pH 680 690 705 708 712 638 Figure 4 Representative image of the visual appearance of the effluent a before filtration on the developed membranes b after filtration on the developed membrane based on bentonite c after filtration on the developed membrane based on Aomar clay and d after filtration on the developed membrane based on kaolin Tables 46 shows the results of physicochemicalpollutantparameter analyses per formed on our samples before and after membrane filtration Minerals 2023 13 273 12 of 19 Table 4 Results of the physicochemical pollution parameters measured on the studied effluent using membrane based on bentonite UF Membrane Parameter of Pollution Measured Effluent before Filtration Permeate Collected at 1 bars Permeate Collected at 2 bars Permeate Collected at 3 bars Permeate Collected at 4 bars Effluent Retained in the Feed Tank Membrane based on Bentonite UF Turbidity NTU 2400 108 105 102 122 2812 Conductivity µS 2170 773 762 753 758 632 Ammonium NH4 mgL 592 305 191 138 232 4724 Nitrites NO2 mgL 288 084 056 048 116 2212 Nitrates NO3 mgL 768 975 78 549 105 4815 Phosphates PO43 mgL 297 1002 460 233 082 27423 pH 680 690 705 708 712 638 Temperature C 217 208 215 217 235 234 COD mgL 5920 66551 64012 54032 4768 167665 BOD5 mgL 2400 81228 75723 67145 57578 83035 RATIO CODBOD 5 247 082 085 080 083 202 Table 5 Results of the physicochemicalpollution parameters measured on the studied effluent using membrane based on Aomar clay UF Membrane Parameter of Pollution Measured Effluent before Filtration Permeate Collected at 1 bars Permeate Collected at 2 bars Permeate Collected at 3 bars Permeate Collected at 4 bars Effluent Retained in the Feed Tank Membrane based on Aomar clay UF Turbidity NTU 2400 106 874 24 260 2700 Conductivity µS 2170 1668 1628 1613 1618 1347 Ammonium NH4 mgL 592 52 402 281 458 3985 Nitrites NO2 mgL 288 195 12 095 24 176 Nitrates NO3 mgL 768 217 152 12 22 238 Phosphates PO43 mgL 297 144 1007 492 157 25888 pH 680 692 703 705 707 635 Temperature C 217 215 223 229 237 239 COD mgL 5920 1520 1476 1254 1123 359523 BOD5 mgL 2400 1740 1650 1440 1254 176642 RATIO CODBOD 5 396 087 089 087 089 204 Minerals 2023 13 273 13 of 19 Table 6 Results of the physicochemical pollution parameters measured on the studied effluent using membrane based on kaolin MF Membrane Parameter of Pollution Measured Effluent before Filtration Permeate Collected at 1 bars Permeate Collected at 2 bars Permeate Collected at 3 bars Permeate Collected at 4 bars Effluent Retained in the Feed Tank Membrane based on Kaolin MF Turbidity NTU 2400 28 19 14 16 2650 Conductivity µS 2170 2023 2003 1985 1993 1499 Ammonium NH4 mgL 592 188 1285 965 1095 546 Nitrites NO2 mgL 288 112 16 144 277 1554 Nitrates NO3 mgL 768 2672 184 1432 85 64 Phosphates PO43 mgL 297 1176 79 432 325 2153 pH 680 690 695 700 73 632 Temperature C 214 217 215 216 225 21 COD mgL 5920 1320 1020 950 798 352054 BOD5 mgL 2400 1400 1379 1136 936 1550 RATIO CODBOD 5 246 094 078 084 084 227 Minerals 2023 13 273 14 of 19 The turbidity level of the examined effluent before filtering was 2400 NTU which is substantially higher than the recommended limit in Algeria 80 NTU The rise in turbidity might be attributed to the mobilization of organic and inorganic particles in suspension 50 The turbidity in the permeate collected at different pressures was reduced to values well below the required standard after filtration in contrast to the highest turbidity ob served in the liquid retained in the feed tank this result indicates that the suspended matter was retained by the three membranes studied These findings are consistent with previous studies on the measuring of turbidity before and after membrane filtration 374551 A reduction in turbidity has been observed with the rise of transmembrane pressure up to 3 bars after which they progressively increase as indicated in Tables 46 which may be explained by a partial fouling of the membranes caused by transmembrane pressures of more than 3 bars 52 351 Conductivity The recorded electricalconductivity values from both the effluent before filtration and the permeates after filtration at various transmembrane pressures between 1 and 4 bars are better than the Algerian standard cited in Table 2 These findings explain why the samples studied had substantial salt even after mem brane filtration less than 2500 µScm This salinity is caused by salts washing chemicals detergents and disinfectants 5354 It is critical to note here that the values of electrical conductivity steadily rise as the transmembrane pressure reaches 3 bars which corresponds to the turbidity values reached beyond 3 bars These conductivity findings in Tables 46 suggest that ultrafiltration membranes are more effective than microfiltration membranes for mineralsalt retention as reported in the literature 51 This result of the successful retention of mineral salts by our two ultrafiltration membranes is in line with previous research findings on the filtration of saline water using ceramic membranes based on natural zeolites 354448 352 Ammonium NH4 Ammonia nitrogen is a reliable indication of urbaneffluent contamination in water systems The findings in Tables 46 reveal that the quantity of NH4 ions in the unfiltered effluent is excessively high reaching 592 mgL After ultrafiltration and microfiltration by the membrane at various pressures a considerable drop in the quantity of these ions was noticed which was followed by an increase in the retained liquid showing that these ions were successfully retained by filtration on all three membranes Indeed better values for NH4 ions were found After ultrafiltration with the bentonite and Aomar clay membranes the result was consistent with the necessary standardlimit value 5 mgL even when the applied pressure was increased from 1 to 4 bars However the amount of NH4 produced via mem brane microfiltration based on kaolin is substantially greater than the Algerian standard This outcome is due to the excessively high permeability achieved by the kaolinbased membrane at 54737 Lm2hbar see Figure 3b which is approximately four times greater than the permeability values of the bentonite and Aomarclaybased membranes This explains why the porosity of the kaolinbased membrane is significant allowing a great amount of ammonium ions to pass through its pores even at low transmembrane pressure refer to the results in Table 6 of the revised version of the manuscript 353 Nitrates NO3 and Nitrite NO2 Nitrates and nitrites are both oxidized forms of nitrogen pollution found in wastewa ter 55 The presence of lactating proteins mineral nitrogen in milk the bacterial oxidation of ammonia andor organicmatter decomposition and the usage of nitric acid during washing all contribute to the high concentration of these ions that define nitrogen pollu tion 53 Tables 46 shows that the measured nitrate and nitrite levels in the unfiltered Minerals 2023 13 273 15 of 19 effluent are much higher than the necessary requirements 30 mgL for NO3 ions and 03 mgL for NO2 ions Even at high transmembrane pressures we detect a drop in these values after filtration on our UF and MF membranes Indeed the amounts of NO3 recovered after filtering are less than the acceptable requirements allowing us to conclude that these ions were partly retained by the two filtration procedures in all membranes tested Moreover the concentration of NO2 ions obtained after filtering using the two procedures of UF and MF is lower than the necessary standard This conclusion is explained by the fact that NO2 is an intermediate molecule that is unstable in the presence of oxygen and has a lower concentration than the two other forms namely nitrate and ammonium ions 56 354 Phosphates PO43 The amount of ions in orthophosphates obtained in Tables 46 for the unfiltered efflu ent is higher than the Algerian standard 10 mgL which is most likely due to the usage of H3PO4 for machine cleaning at the level of cheese manufacturers in general Further more phosphorus compounds such as soluble orthophosphates and organophosphorus derivatives may be found in natural waters and wastewater 55 The number of orthophosphate Ions Is lowered below the acceptable level after filtering using ultrafiltration membranes based on bentonite and Aomar clays regardless of the applied transmembrane pressure 14 bars However the quantities of these ions following filtration on kaolinbased microfiltration membranes remain too high at all pressures employed These findings suggest that a membraneultrafiltration method can achieve orthophosphate retention but not a microfiltration procedure 355 pH and Temperature pH is an effective indication of pollution it fluctuates depending on whether the effluent is basic or acidic The biological pH range is 65 to 85 57 Indeed the pH values obtained before and after filtration for the three kinds of membranes demonstrate that all of the samples studied had pH values between 68 and 73 These results are consistent with those of the rejected effluents in Algeria where the pH must be in the range 6585 Temperature changes have a significant impact on the formation of microorganism colonies 5859 Indeed increasing the temperature of industrial effluents promotes their growth and hence the consumption of huge amounts of oxygen while decreasing the amount of dissolved oxygen in these effluents 60 According to Tables 46 the observed temperatures for all ultrafiltration and microfiltration membrane samples are almost consistent and fall below the acceptable limit 30 C This result indicates that the examined samples do not constitute a thermalpollution concern to the receiving natural environment Values over 30 C on the other hand contribute to the acceleration of biological processes for the treatment of industrial effluents by increasing the kinetics of organic degrading matter 61 356 The Chemical Oxygen Demand COD The COD data Tables 46 demonstrate that the unfiltered effluent is highly con taminated with organic matter with a value of 5928 mgL which is much more than the necessary limit 120 mgL The COD value reported in this unfiltered effluent is three times that found in study work on wastewaterCOD analysis 62 This conclusion may be explained by the fact that cheese effluents include residues of milk and chemical products used for machine cleaning at the cheesefactory level resulting in an increase in the quantity of organic matter responsible for the growth of aerobic bacteria 63 After filtering at pressures ranging from 1 to 4 bars the COD value drops to between 6655 and 4768 mgL approximately 90 of organic matter eliminated for the bentonite membrane between 1520 and 1123 mgL approximately 81 of organic matter eliminated for the Aomarclay membrane and between 1320 and 798 mgL approximately 90 of organic matter eliminated for the kaolin membrane These values remain high following Minerals 2023 13 273 16 of 19 filtering by the two UF and MF procedures indicating that the organic components in this cheese effluent were partly retained by all of the membranes tested The results of our investigation of the COD show improved outcomes compared to previous research on the filtration of dairy effluent conducted over a onemonth period at a sequencingbatch reactor station 6 Our results are even more favorable in comparison to the treatment of wastewater in a series of three microphytelagoon basins 63 357 BOD5 Biological Oxygen Demand for 5 days The findings in Tables 46 further demonstrate that the BOD5 value obtained for the effluent before filtering is extremely high 2400 mgL which explains why this effluent is so rich in biodegradable compounds After filtering the BOD5 in all permeates sampled at each applied pressure from 1 to 4 bars falls progressively across all membranes examined This gradual drop when pressure is increased may be explained by the partial fouling of our membranes over time It is critical to note that all BOD5 readings measured before and after filtering remain very high and exceed the necessary level of 35 mgL 358 The Ratio of CODBOD5 The CODBOD5 ratio allows us to assess the biodegradability of contaminants and determine the purification chain of a given effluent Wastewater rejected directly into receiving waters exhibits householdwastewater characteristics CODBOD5 3 64 This increasing ratio suggests an increase in nonbiodegradable organic matter 5759 The CODBOD5 ratio values obtained in Tables 46 for the permeate collected after filtering of our effluent on the three membranes investigated at varying pressures are significantly lower than 3 between 074 and 094 indicating that these are readily biodegradable effluents 61 The CODBOD5 ratios of the effluent before filtering and the liquid retained in the feed tank on the other hand are between 2 and 3 indicating that they are moderately biodegradable effluents 575961 indeed as stated by Mesrouk et al 60 and Litébé et al 65 an analysis of this ratio clearly highlights the biodegradability of wastewater These findings indicate that all of our samples both before and after membrane filtration may be purified using biological treatment 5861 4 Conclusions In the study conducted here tubular supports were fabricated using three clays sourced from various regions in Algeria with the intention of utilizing them in ultrafiltra tion and microfiltration processes Results showed that the kaolinbased support had the highest water permeability The developed membranes effectively clarified a localcheese effluent and retained suspended particles and organic compounds at transmembrane pres sures less than or equal to 3 bars The ultrafiltration membranes based on bentonite and Aomar clay retained NH4 ions but this was not the case for the microfiltration based on kaolin unlike the NO2 and NO3 ions which all three membranes tested retained The study found that when the transmembrane pressure is greater than 3 bars NH4 and NO2 ions begin to cross the membranes and their retention is facilitated by ultrafiltration membranes based on bentonite and Aomar clay The analysis showed that the permeates collected at pressures between 1 and 4 bars are readily biodegradable and require bio logical treatment The study concluded that COD and BOD5 are important for reducing organic matter and biodegradablematerial loads and that the permeates collected are fairly biodegradable and need biological treatment Author Contributions Conceptualization LH and DEA methodology LH DEA and AH validation LM and AA formal analysis LH and DEA investigation LH resources LM and AA data curation LH and DEA writingoriginal draft preparation LH writingreview and editing AH LM and AA visualization LM and AA supervision LM and AA project admin istration LM and AA All authors have read and agreed to the published version of the manuscript Funding This research received no external funding Minerals 2023 13 273 17 of 19 Institutional Review Board Statement Not applicable Informed Consent Statement Not applicable Data Availability Statement Not applicable Acknowledgments The authors wish to thank all who assisted in conducting this work Conflicts of Interest The authors declare no conflict of interest References 1 Mustapha S Shuaib DT Ndamitso MM Etsuyankpa MB Sumaila A Mohammed UM Nasirudeen MB Adsorption isotherm kinetic and thermodynamic studies for the removal of PbII CdII ZnII and CuII ions from aqueous solutions using Albizia lebbeck pods Appl Water Sci 2019 9 142 CrossRef 2 Mustapha S Dauda B Ndamitso M Mathew J Bassey U Muhammed S Biosorption of Copper from Aqueous Solutions by Raw and Activated Spines of 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