Fabrication and performance on environmental applications of a novel 3d superhydrophobic material based on a loofah sponge from the natural plant

VIETNAM NATIONAL UNIVERSITY, HANOI VIETNAM JAPAN UNIVERSITY DO DANH QUANG FABRICATION AND PERFORMANCE ON ENVIRONMENTAL APPLICATIONS OF A NOVEL 3D SUPERHYDROPHOBIC MATERIAL BASED ON A LOOFAH SPONGE FROM THE NATURAL PLANT MASTER’S THESIS VIETNAM NATIONAL UNIVERSITY, HANOI VIETNAM JAPAN UNIVERSITY DO DANH QUANG FABRICATION AND PERFORMANCE ON ENVIRONMENTAL APPLICATIONS OF A NOVEL 3D SUPERHYDROPHOBIC MATERIAL BASED ON A LOOFAH SPONGE FROM THE NATURAL PLANT MAJOR: ENVIRONMENTAL ENGINEERING CODE: 8520320.01 RESEARCH SUPERVISOR: Dr: TRAN THI VIET HA Hanoi, 2023 COMMITMENT I have read and understood the plagiarism violations I pledge with personal honor that this research result is my own and does not violate the Regulation on Prevention of plagiarism in academic and scientific research activities at VNU Vietnam Japan University (Issued together with Decision No 700/QD-ĐHVN dated 30/9/2021 by the Rector of Vietnam Japan University) Author of the thesis Do Danh Quang ACKNOWLEDGEMENTS I would like to express my deepest gratitude to Dr Tran Thi Viet Ha, who enthusiastically guided, guided, and helped me so that I could complete and complete the thesis fully and in the best way I would like to thank the teachers and assistants in the master's program in environmental engineering for enthusiastically teaching and helping me during my study at the school The project with the code number VJU.JICA.21.03, from VNU Vietnam Japan University, fully funds the project as part of the Research Grant Program of the Japan International Cooperation Agency Especially, I would like to thank my family’s great love, Mr Do Danh Ha, Mrs Nguyen Thi Dien, Ms Huyen Trang, and Ms Nhu Quynh, who eased and supported me during my master's degree Finally, I would like to thank my MEE batch students and friends who have always encouraged and helped me in the past time to complete my thesis TABLE OF CONTENTS LIST OF TABLES i LIST OF FIGURES ii LIST OF ABBREVIATIONS iv CHAPTER 1: INTRODUCTION 1.1 Research background 1.2 Research significance 1.3 Research objectives 1.4 Thesis outline .3 CHAPTER 2: LITERATURE REVIEW .4 2.1 Theoretical basic 2.1.1 Water wettability and water contact angle 2.1.2 Solid surface wetting states 2.1.3 Model explaining the mechanism 2.2 Methods to fabricate the superhydrophobic surface 2.2.1 Dip coating 2.2.2 Spray coating 2.2.3 Polymerization techniques 10 2.2.4 In situ nanorod/particle growth 11 2.3 Oil pollution and treatment methods previous 12 CHAPTER 3: MATERIALS AND METHODOLOGIES 16 3.1 Materials .16 3.2 Methodologies 17 3.2.1 Fabrication procedure PW-PW@LS 17 3.2.2 Optimization of fabrication parameters PW-PW@LS 18 3.3 Material characterization method .18 3.3.1 Scanning electron microscopy (SEM) 18 3.3.2 Energy-dispersive X-ray (EDX) 20 3.3.3 X-ray Diffraction (XRD) .21 3.3.4 Fourier-transform infrared spectroscopy (FTIR) 22 3.3.5 Water contact angle (WCA) 23 3.4 Evaluate the application of PW-PW@LS for environmental treatment 23 3.4.1 Separation of floating oil .23 3.4.2 Oil/solvent adsorption capacity 24 3.5 Evaluate the reusability of PW-PW@LS 25 3.6 Evaluate the durability of PW-PW@LS 25 3.6.1 Mechanical durability test 25 3.6.2 Chemical durability test .25 CHAPTER 4: RESULTS AND DISCUSSION 26 4.1 Optimization of the PW-PW@LS sample fabrication parameters 26 4.1.1 Optimization of ratio ethanol: xylene in step 3: spray-coating 26 4.1.2 Optimization of wax concentration in step 3: spray-coating 27 4.2 Characterization of fabricated materials 28 4.2.1 SEM image 28 4.2.2 EDX analysis 28 4.2.3 XRD analysis 31 4.2.4 FTIR analysis 32 4.2.5 WCA measurement results 33 4.3 Evaluate the ability to remove oils and organic solvents from water 34 4.3.1 Floating oil removal experiment 34 4.3.2 Oil adsorption: Effect of contact time 35 4.3.3 Effect of temperature 37 4.3.4 Calculation of oil adsorption capacity of PW-PW@LS 39 4.3.5 Mechanism of oil-water separation 41 4.4 Reusability and durability test of PW-PW@LS 41 4.4.1 Reusability test 41 4.4.2 Mechanical durability 42 4.4.3 Chemical durability .44 CHAPTER 5: CONCLUSION AND RECOMMENDATIONS 46 5.1 Conclusion 46 5.2 Recommendations 46 REFERENCES 48 APPENDIX 54 LIST OF TABLES Table 2.1 Advantages and disadvantages of oil pollution treatment methods 13 Table 2.2 Summary of some studies using superhydrophobic materials for oil-water separation .15 Table 3.1 The chemical formula of the material 16 Table 3.2 Conditions for optimizing the ratio of ethanol and xylene to fabricate PWPW@LS 18 Table 3.3 Optimization of wax concentration variation for fabrication PW-PW@LS18 Table 4.1 Change the ratio of ethanol: xylene in step 26 Table 4.2 Change the concentration of wax in step 27 Table 4.3 Elemental composition of raw LS 30 Table 4.4 Elemental composition of PW-PW@LS .30 Table 4.5 R2 and constant value for different adsorption kinetic models 36 Table 4.6 Results of adsorption capacity of PW-PW@LS 40 i LIST OF FIGURES Figure 2.1 Solid surface wetting states and WCA values (Zhang & Xu, 2021) Figure 2.2 Wenzel and Cassie-Baxter's analysis of the wettability of a rough surface (Teisala et al., 2014) Figure 3.1 Spray gun (Wider 1, ANEST IWATA, Japan) 18 Figure 3.2 SEM TM4000Plus (Hitachi Corp., Japan) 19 Figure 3.3 EDX MisF+ instrument (Oxford Instruments plc., UK) 20 Figure 3.4 XRD MiniFlex 600 (Rigaku Corp., Japan) 21 Figure 3.5 FTIR-4600 (Jasco Corp., Japan) 22 Figure 3.6 SmartDrop WCA (Femtofab Co Ltd., Korea) 23 Figure 3.7 Experimental diagram for separating floating oil from water 23 Figure 3.8 The schematic of the abrasion test of PW-PW@LS with sandpaper 25 Figure 4.1 SEM image of LS sample a) raw, b) after pretreatment, c) PW@LS, and d) PW-PW@LS 28 Figure 4.2 EDX spectra of LS sample a) raw, b) after pretreatment, c) PW@LS, and d) PW-PW@LS .29 Figure 4.3 Element mapping on PW-PW@LS surface .30 Figure 4.4 XRD patterns of sample a) palm wax, b) raw LS, c) LS after pretreatment, d) PW@LS, and e) PW-PW@LS 31 Figure 4.5 FTIR spectra of sample a) palm wax, b) raw LS, c) LS after pretreatment, d) PW@LS, and e) PW-PW@LS 33 Figure 4.6 Digital photo of water droplets and oil (kerosene) added on the surface a) raw LS, b) PW@LS, c) PW-PW@LS Small sections stand for OCA and WCA measurements, respectively The water is stained blue 34 Figure 4.7 Experimental diagram of removing floating oil from water Diesel oil is used as floating oil on seawater, and the water is dyed brilliant green for easy distinction 34 Figure 4.8 Pseudo-first-order kinetic model 35 Figure 4.9 Pseudo-second-order kinetic model 36 Figure 4.10 Effect of temperature on oil adsorption capacity .38 Figure 4.11 The density of oil and solvent at different temperatures (GmbH, 2023a, 2023b; Paleu & Nelias, 2007; Rusanov et al., 1966; ToolBox, 2018a, 2018b) 38 Figure 4.12 The adsorption capacity of PW-PW@LS for various oils and solvents 39 Figure 4.13 Effect of density on oil adsorption capacity 40 Figure 4.14 Schematic diagram of oil adsorption in PW-PW@LS a) for light oil, b) through capillary force, light oil is transported along cellulose fibers, and c) magnified photo 41 Figure 4.15 The adsorption capacity of PW-PW@LS after 10 cycles 42 Figure 4.16 Appearance shapes before and after compression of (a) raw LS, (b) PW@LS, and c) PW-PW@LS 43 ii Figure 4.17 The kerosene adsorption capacity of PW-PW@LS after 20 abrasion cycles 44 Figure 4.18 The kerosene adsorption capacity of PW-PW@LS at pH=2, pH=7, 0.5 M NaCl 45 iii LIST OF ABBREVIATIONS CA: Contact angle CVD: Chemical vapor deposition DI: Deionized EDX: Energy-dispersive X-ray FTIR: Fourier-transform infrared spectroscopy KLAMG Key Laboratory of Advanced Materials for Green Growth LS: Loofah sponge PW: Palm wax SA: Sliding angle SEM: Scanning electron microscope WCA: Water contact angle XRD: X-ray Diffraction iv 4.3.5 Mechanism of oil-water separation Based on the results, the oil-water separation mechanism is Van Der Van's weak force, hydrophobic interaction, and capillary force The main motive force for oil and water separation of PW-PW@LS is hydrophobic interaction and capillary force When PW-PW@LS was brought to the oil surface, the hydrophobic surface on PW-PW@LS made water impermeable to the sponge Because the PW-PW@LS has a 3D skeleton structure, the oil was guided into the sponge along the capillary fibers and was adsorbed onto the sponge Adsorption is so simple that desorption or reuse will be accessible by techniques such as centrifugation and press Figure 4.14 Schematic diagram of oil adsorption in PW-PW@LS a) for light oil, b) through capillary force, light oil is transported along cellulose fibers, and c) magnified photo 4.4 Reusability and durability test of PW-PW@LS 4.4.1 Reusability test This test used fabricated LS to adsorb oil/solvent in water The LS, after performing adsorption experiments, was desorbed by centrifuge, then dried and evaluated for reuse for 10 cycles As Figure 4.15 shows the high reusability with 10 cycles of PW-PW@LS Furthermore, the recycled wax solution can be reused The wax coating can be easily regenerated with hot xylene 41 Figure 4.15 The adsorption capacity of PW-PW@LS after 10 cycles 4.4.2 Mechanical durability The stability and durability of the PW-PW@LS are essential for practical applications Therefore, the material mechanical durability was also evaluated according to Figures 4.16 and 4.17 with a weight of 500g As shown in Figure 4.16, after the compression test, the surface of the LS samples did not change in shape and size Thus, the LS material shows good resilience after being affected by gravity 42 Figure 4.16 Appearance shapes before and after compression of (a) raw LS, (b) PW@LS, and c) PW-PW@LS According to the results shown in Figure 4.17, the kerosene adsorption capacity of PW-PW@LS was reduced by 12% after 20 abrasion cycles This is also inevitable because when performing the abrasive process, the wax-hydrophobic surface on the 43 PW-PW@LS surface loses a small part through each cycle resulting in reduced water resistance It also means that the oil-in-water separation efficiency of PW-PW@LS after 20 abrasion cycles is lower than that of the original PW-PW@LS sample Figure 4.17 The kerosene adsorption capacity of PW-PW@LS after 20 abrasion cycles 4.4.3 Chemical durability The oil adsorption capacity of PW-PW@LS in harsh environments such as acidic, alkaline, and high salinity environments was also investigated The result is shown in the graph of Figure 4.18 The adsorption capacity of PW-PW@LS had good stability in neutral pH, pH = 12, and 0.5M NaCl However, there was a decrease in pH = In a strongly acidic environment, electrostatic interaction occurs on the surface of PW-PW@LS, reducing the hydrophobicity of the surface This results in an affected oil-water separation and reduced oil-adsorption capacity of PW-PW@LS 44 Figure 4.18 The kerosene adsorption capacity of PW-PW@LS at pH=2, pH=7, 0.5 M NaCl 45 CHAPTER 5: CONCLUSION AND RECOMMENDATIONS 5.1 Conclusion The naturally derived hydrophobic material PW-PW@LS was successfully fabricated through a 2-step dipping and spraying process Two best conditions were found to improve the quality of PW-PW@LS: the ratio of ethanol and xylene was 2:8, and the concentration of wax was 0.01 g/mL The structural properties and chemical composition of materials were studied in detail by modern methods SEM, EDX, XRD, FTIR, and WCA The water contact angle of the PW-PW@LS was determined to be 142.3° ± 1° Experiments on oil-in-water adsorption were performed The results show that PWPW@LS can adsorb oil with efficiency up to 2.1 - 6.4 times the weight of the adsorbent In addition, PW-PW@LS was also a potential "green" material that is biodegradable The results show that this material can have practical applications in cleaning up oil spills and removing organic pollutants on the water’s surface, towards environmental protection and sustainable development 5.2 Recommendations Study on oil removal from natural wastewater: A detailed inquiry is advised on oil removal from actual wastewater This study examines various oil removal technologies and techniques, such as physical separation, chemical processing, and biological processes The study shall examine the efficiency of several techniques for removing oil contaminants from wastewater samples Economic feasibility study: Conduct a thorough economic feasibility study to determine whether producing PW-PW@LS is commercially viable In this analysis, it is essential to look at all manufacturing expenses, including personnel, raw materials, machinery, and energy use PW-PW@LS's prospective profitability, as well as the market's demand, should be considered Deciding the viability and benefits of manufacturing PW-PW@LS will be possible by looking at the economic variables 46 Environmental impact assessment: To find any potential effects of producing PWPW@LS, perform an environmental impact study Every product's life cycle phase should be considered, including gathering raw materials, 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Fabrics for Oil/Water Separation ACS Applied Materials & Interfaces, 5(15), 7208-7214 53 APPENDIX Map showing the relationships and frequency of phrases used in studies on oil pollution Bubble sizes denote the occurrence intensity, and colors show the cluster number related to the dataset, and intersecting bubbles indicate phrases co-occurring more frequently Scopus-based data was analyzed by VOS viewer (van Eck & Waltman, 2010) 54 Relationship and occurrence graph of words used in research related to a loofah sponge 55