Valorization of waste shrimp shell as a versatile biosorbent using hydrothermal carbonization for water purification

VIETNAM NATIONAL UNIVERSITY, HANOI VIETNAM JAPAN UNIVERSITY NGUYEN QUANG HUNG VALORIZATION OF WASTE SHRIMP SHELL AS VERSATILE BIOSORBENT USING HYDROTHERMAL CARBONIZATION FOR WATER PURIFICATION MASTER'S THESIS VIETNAM NATIONAL UNIVERSITY, HANOI VIETNAM JAPAN UNIVERSITY NGUYEN QUANG HUNG VALORIZATION OF WASTE SHRIMP SHELL AS VERSATILE BIOSORBENT USING HYDROTHERMAL CARBONIZATION FOR WATER PURIFICATION MAJOR: ENVIRONMENTAL ENGINEERING CODE: 8520320.01 RESEARCH SUPERVISOR: Dr NGUYEN THI AN HANG Hanoi, 2023 COMMITMENT It is critical that I demonstrate my comprehension and commitment to respecting ethical norms and avoiding plagiarism over the course of this project I strictly follow the criteria given in Decision Rector of Vietnam Japan University number 700/Q-HVN dated September 30, 2021, which details the regulations for combating plagiarism in academic and scientific activity I recognize the value of academic honesty and commit to properly attribute and reference any sources utilized in my study, ensuring that any ideas or information gained from outside sources are correctly attributed By assuring the truth, originality, and authenticity of my research results, I am promoting a culture of academic integrity and intellectual rigor Nguyen Quang Hung ACKNOWLEDGEMENTS Dr Nguyen Thi An Hang has given me excellent advices, steadfast support, and encouragement during the preparation of my Master's Thesis Her passion, experience, and invaluable commitment to academic success were invaluable in shaping my thoughts, developing my abilities, and enhancing my research I'd like to thank VJU for providing me with a studentship that allowed me to pursue a Master's degree and complete this study Academic rigor, intellectual variety, and a global perspective at VJU have presented me with a life-changing, illuminating, and powerful educational experience that I will remember for the rest of my life I would also like to thank all member of MEE6 for sharing the knowledge, experiences during my student’s career This research has been done under the research project QG.22.26 “Application of the innovative hydrothermal carbonization technology (HTC) in agro-wastes and sludge treatment and recycling in Vietnam for producing high-performance bio-fuels, biofertilizers, and advanced environmental materials” of Vietnam Nation University, Hanoi Finally, my deep gratitude to my parents for the opportunity to study and their support on my education path They are crucial to the accomplishment of my research since without them, I would not have enough information to draw any conclusions My appreciations go to everyone who helped me during the research process, notwithstanding how they did it June 2023 Nguyen Quang Hung TABLE OF CONTENTS LIST OF ABBREVIATIONS i LIST OF TABLES ii LIST OF FIGURES iii CHAPTER I: INTRODUCTION 1.1 Research background 1.2 Research significance 1.3 Research objectives 1.4 Thesis outline CHAPTER II: LITERATURE REVIEW 2.1 Introduction of dyes 2.1.1 Classification of dyes and introduction of Direct Blue 71 (DB71) 2.1.2 Environmental concerns of dyes 2.1.3 Dye treatment technologies 2.2 Hydrothermal carbonization (HTC) for production of environmental materials applied in wastewater treatment 11 2.2.1 Overview of HTC process 11 2.2.2 Application of hydrochar in dye rich wastewater treatment 13 2.2.3 Modification of hydrochars for enhancing adsorptive removal of dyes from wastewater 14 2.3 Waste shrimp shell (WSS) application for wastewater treatment 20 2.3.1 Pollution sources 20 2.3.2 Application of WSS in wastewater treatment 23 CHAPTER III: MATERIALS AND METHODS 25 3.1 Chemicals and apparatus 25 3.1.1 Chemicals 25 3.1.2 Apparatus 25 3.2 Material synthesis 27 3.2.1 Raw waste shrimp shell (WSS) 27 3.2.2 Acid activated waste shrimp shell derived hydrochar (A_WSH) 28 3.3 Material characterization methods 29 3.3.1 Fourier transform infrared spectroscopy (FTIR) 29 3.3.2 Scanning electron microscope (SEM) 30 3.3.3 Brunauer–emmett–teller (BET) 30 3.3.4 pH point of zero charge determination 31 3.4 Batch adsorption experiments setup 31 3.4.1 Factors influencing DB71 adsorption by A_WSH 31 3.4.2 DB71 adsorption behaviors by A_WSH 34 CHAPTER IV: RESULTS AND DISCUSSION 40 4.1 DB71 calibration 40 4.1.1 Color-metric method 40 4.1.2 Calibration curve 40 4.2 Material characterization 42 4.2.1 FTIR analysis result 42 4.2.2 SEM analysis result 43 4.2.3 BET analysis result 44 4.2.4 pH point of zero charge 45 4.3 Adsorptive removal of DB71 from synthetic wastewater using A_WSH 45 4.3.1 Process parameters governing DB71 adsorption by A_WSH 45 4.3.2 Elucidation of DB71 adsorption behaviors and mechanisms by A_WSH 51 CHAPTER V: CONCLUSION AND RECOMMENDATIONS 60 5.1 Conclusion 60 5.2 Recommendations 60 AOPs : A-WSH : BET : BOD : COD : DB71 : LIST OF ABBREVIATIONS Advanced oxidation processes Acid activated waste shrimp hydrochar Brunauer–emmett–teller Biological oxygen demand Chemical oxygen demand Direct blue 71 FTIR : Fourier-transform infrared spectroscopy HTC : MO : PFO : pHzpc : PSO : SEM : WSH : WSS : Hydrothermal carbonization Methyl orange Pseudo - first - order pH zero point charge Pseudo - second - order Scanning electron microscope Waste shrimp hydrochar Waste shrimp shell i LIST OF TABLES Table 2.1: Dye treatment technologies Table 2.2: Products of HTC process 13 Table 2.3: Summary of studies on dye adsorption 17 Table 3.1: The nature of adsorption process in relation with RL value 36 Table 3.2: The nature of adsorption process in relation with n value 37 Table 3.3: The nature of adsorption process in relation with bT value 38 Table 3.4: The nature of adsorption process in relation with ΔH, ΔS, ΔG values 39 Table 4.1: BET analysis results of WS, WSH, and A-WSH 44 Table 4.2: Variation of surface charge of A-WSH over the pH value 45 Table 4.3: Linear PFO and PSO kinetic parameters for DB71 adsorption by A-WSH 52 Table 4.4: Intra-particle diffusion kinetic parameters for DB71 adsorption by A-WSH 53 Table 4.5: Langmuir and Freundlich isotherm parameters for DB71 adsorption by AWSH 54 Table 4.6: Calculated RL values at different DB71 concentrations 55 Table 4.7: Temkin isotherm parameters for DB71 adsorption by A-WSH 56 Table 4.8: Thermodynamic parameters for DB71 adsorption by A-WSH 57 Table 4.9: Comparison of the maximum adsorption capacity (qmax) of A-WSH in this work and those of other adsorbents in previous studies 58 ii LIST OF FIGURES Figure 2.1: Chemical structure of an orange colored azo dye Figure 2.2: Classes of azo dye Figure 2.3: Structure of Direct Blue 71 (DB71) Figure 2.4: Overview of HTC process and potential applications of hydrochar 11 Figure 2.5: Hydrochar produced from organic waste 13 Figure 2.6: Shrimp head as the waste in Philippine 21 Figure 2.7: The dumping site of waste shrimp shell next to Suoi Dau industrial park 22 Figure 2.8: Chitosan for wastewater treatment purpose 24 Figure 3.1: Raw waste shrimp shell 27 Figure 3.2: Procedure for fabrication of A-WSH 28 Figure 4.1: UV-VIS S2150UV spectrophotometer, Unico 40 Figure 4.2: Calibration curve of DB71 41 Figure 4.3: FTIR spectra of WS, WSH and A-WSH 42 Figure 4.4: SEM images of (a) raw waste shrimp shell (WS), (b) waste shrimp shell derived hydrochar (WSH), (c) acid activated waste shrimp shell derived hydrochar (A-WSH) 43 Figure 4.5: pHzpc of A-WSH 45 Figure 4.6: Influence of initial dye solution pH on DB71 adsorption by A-WSH (adsorbent dose 0.5 g/L, temperature = 27oC, time = 24 h, Ci = 50 mg/L) 46 Figure 4.7: Influence of adsorbent dose on DB71 adsorption by A-WSH (pH = 6.78, temperature = 27oC, time = 24 h, Ci = 50 mg/L) 48 Figure 4.8: Influence of contact time on DB71 adsorption by A-WSH (adsorbent dose = g/L, pH = 6.78, temperature = 27oC, Ci = 50 mg/L) 48 Figure 4.9: Influence of initial dye concentration on DB71 adsorption by A-WSH (adsorbent dose = g/L, pH = 6.78, temperature = 27oC, contact time = h) 49 Figure 4.10: Isortherm curves obtained at 303, 313, 323, and 333 K for DB71 adsorption onto A-WSH (adsorbent dose = g/L, pH = 6.78, time = h, Ci = 25 – 500 mg/L) 50 Figure 4.11: Effect of the temperature in the removal efficiency of DB71 onto A-WSH (adsorbent dose = g/L, pH = 6.78, time = h, Ci = 25 – 500 mg/L) 51 Figure 4.12: Kinetic models for DB71 adsorption by A-WSH (adsorbent dose = 1g/L, pH = 6.78, temperature = 27oC, Ci = 50 mg/L) 51 Figure 4.13: Intra-particle diffusion kinetic model for adsorption of DB71 onto A-WSH (adsorbent dose = g/L, pH = 6.78, temperature = 27oC, Ci = 50 mg/L) 52 Figure 4.14: Langmuir isotherm model (a) and Freundlich isotherm model (b) for adsorption of DB71 onto A-WSH (adsorbent dose = g/L, pH = 6.78, temperature = 27oC, time = h, Ci = 25 - 500 mg/L) 54 Figure 4.15: Temkin isotherm model for adsorption of DB71 onto A-WSH (adsorbent dose = 1g/L, pH = 6.78; temperature = 27oC, time = h, Ci = 25 - 500 mg/L) 56 iii Figure 4.16: Plot ln(KL) vs 1/T for estimation of thermodynamic parameters for DB71 adsorption onto A-WSH (adsorbent dose = g/L; pH = 6.78, time = 4h) 57 iv PFO and PSO model are calculated follow the equation (6) and (7) respectively Apparently, correlation coefficients (R2) values for PSO were higher than those PFO model On the other hand, when compared to the findings obtained using the pseudo-first-order model, the calculated equilibrium adsorption capacity (qe, cal) computed using the pseudosecond-order model exhibited a significantly closer agreement with the experimental adsorption capacity (qe, exp) in Table 4.3 This shows that the pseudo-second-order model is more adapted to represent the adsorption of DB71 molecules onto A-WSH, showing that the adsorption is chemical in nature Table 4.3: Linear PFO and PSO kinetic parameters for DB71 adsorption by A-WSH Parameters Pseudo-firstorder (PFO) Pseudo-secondorder (PSO) qe(mg/g) 50.235 56.687 K 0.0088 0.00038 R2 0.947 0.957 Intra-particle diffusion model Linear Intraparticle diffusion 50.00 Phase II qt (mg/g) 40.00 30.00 y = 0.0741x + 48.108 R² = 0.939 Phase I y = 1.8566x + 9.8474 R² = 0.9506 20.00 10.00 0.00 10 √𝒕 15 X 20 25 30 Figure 4.13: Intra-particle diffusion kinetic model for adsorption of DB71 onto AWSH (adsorbent dose = g/L, pH = 6.78, temperature = 27oC, Ci = 50 mg/L) 52 A plot of qt against t1/2 in Figure 4.13 demonstrates the existence of two linear segments, indicating the participation of intra-particle diffusion during the adsorption process The appearance of two linear sections with different slopes implies that two independent phases in the adsorption processes occurred At phase I: the first stage of the adsorption process comprises instant adsorption or diffusion on the exterior surface, particularly within macro-pores, until saturation on the outer surface is reached At phase II: diffusion rate decreased (Table 4.4) which means the solute moved from a larger pores size to a smaller one, indicating that the adsorption rate became slower, and gradually become saturation of the adsorbent surface The findings showed that in the early period, macro-pore diffusion was dominating, but in the latter period, intra-particle diffusion became the rate-controlling step Table 4.4: Intra-particle diffusion kinetic parameters for DB71 adsorption by AWSH KP1 (mg/(g min1/2)) R2 KP2 (mg/(g min1/2)) R2 1.856 0.9506 0.074 0.939 The comparison of Kp of this thesis with others has been mentioned According to Huang et al (2011) , the elimination of anionic eosin Y by using modified chitosan had rate constant K and diffusion rate Kp were 1.9 x 10-4 g/mg∙min and 9.427 mg/(g min1/2) respectively The rate constant K of this thesis is 3.8 x 10-4 g/mg∙min, which is higher than the previous study indicating that the rate of DB71 adsorption is faster Whereas, the diffusion rate has only 1.856 mg/(g∙min1/2), which is lower than the diffusion rate of anionic eosin Y onto modified chitosan b) Adsorption isotherm study Langmuir and Freundlich isotherm model 53 The Freundlich and Langmuir models were used to analyze the adsorption data Two graphs encompassing a variety of concentrations were constructed to compare both isotherms The results of this comparison are shown in Figure 4.14: (a) (b) Langmuir isotherm for DB71 adsorption onto A-WSH 3.00 2.0 2.00 y = 0.0064x + 0.12 R² = 0.9623 1.0 0.0 100 200 300 400 Ce (mg/g) 500 logqe Ce/qe (g/L) 3.0 Freundlich isotherm for DB71 adsorption onto A-WSH y = 4.3515x - 7.0803 R² = 0.8796 1.00 0.00 0.00 -1.00 0.50 1.00 1.50 2.00 2.50 logCe Figure 4.14: Langmuir isotherm model (a) and Freundlich isotherm model (b) for adsorption of DB71 onto A-WSH (adsorbent dose = g/L, pH = 6.78, temperature = 27oC, time = h, Ci = 25 - 500 mg/L) Table 4.5 shows the estimated values of the DB71 adsorption parameters generated from various models Table 4.5: Langmuir and Freundlich isotherm parameters for DB71 adsorption by A-WSH Langmuir isotherm model qmax (mg/g) 156.25 RL R2 0.3 0.962 Freundlich isotherm model KF ((mg/g)∙(L/mg) -8 8.3x10 1/n n R2 0.23 0.879 The calculated data fitted quite well with the Langmuir and Freundlich isotherm model Nevertheless, the correlation coefficients of Langmuir (R2 = 0.962) were higher than the Freundlich model indicating that the data fitted better with the Langmuir isotherm model Hence, the adsorption type could be considered as monolayer adsorption Furthermore, the parameter n is not comparable The constant n refers to the interaction between exchange sites in the adsorbent and DB71 ions Value of n < shows that the adsorption process followed physical adsorption, which is conflicted with 54 chemisorption of PSO model Additionally, the calculated KL in Langmuir isotherm model measures the affinity between adsorbent and adsorbate Therefore, a greater KL value equates to greater quantities of adsorption at small solution amounts Table 4.6: Calculated RL values at different DB71 concentrations Adsorption process Ci (mg/L) RL 25 0.429 Favorable adsorption 50 0.273 Favorable adsorption 100 0.158 Favorable adsorption 200 0.086 Irreversible adsorption 300 0.059 Irreversible adsorption 400 0.045 Irreversible adsorption 500 0.036 Irreversible adsorption nature The findings indicate that the adsorption process was extremely favorable throughout the concentration range once more It's also worth noticing that all of the values are very near zero, suggesting that things are on the verge of irreversibility Temkin isotherm model 180.00 160.00 140.00 y = 15.761x + 51.357 R² = 0.8869 qe (mg/g) 120.00 100.00 80.00 60.00 40.00 20.00 -2.00 -1.00 0.00 0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 lnCe 55 Figure 4.15: Temkin isotherm model for adsorption of DB71 onto A-WSH (adsorbent dose = 1g/L, pH = 6.78; temperature = 27oC, time = h, Ci = 25 - 500 mg/L) Table 4.8 shows the estimated values of the DB71 adsorption parameters generated from Temkin models Table 4.7: Temkin isotherm parameters for DB71 adsorption by A-WSH B bT (kJ/mol) 15.761 157.20 From the Table 4.7 showed that the bT value was much more than kJ/mol indicating that the adsorption process was chemisorption This mechanism process is compatible with the mechanism of the Langmuir isotherm model and PSO model In addition, it is assumed that the adsorption process followed the ionic bonds, which means the affinity between negative DB71 and positive A-WSH was an electrostatic force c) Adsorption thermodynamic study The thermodynamic parameters for the DB71 adsorption process onto WSS were calculated For this study, the experimental data from the four tests done at different temperatures The KL are shown in Figure 4.16 56 1.86 y = -304.73x + 2.7575 R² = 0.9656 1.84 ln(kL) 1.82 1.80 1.78 1.76 1.74 0.0030 0.0030 0.0031 0.0031 0.0032 0.0032 0.0033 0.0033 0.0034 1/T (K-1) Figure 4.16: Plot ln(KL) vs 1/T for estimation of thermodynamic parameters for DB71 adsorption onto A-WSH (adsorbent dose = g/L; pH = 6.78, time = 4h) The above chart showed has high correlation coefficient (R2) indicating that the data is reliable Therefore, from the above plot, enthalpy change ∆H0, entropy change ∆S0, Gibbs free energy ∆G0 were calculated, and shown in Table 4.8: Table 4.8: Thermodynamic parameters for DB71 adsorption by A-WSH T (K) qmax (mg/g) 303 156.25 313 204.08 323 285.71 333 400 ∆H0 (kJ/mol) ∆S0 (Jꞏmol-1ꞏK-1) ∆G0 (kJ/mol) -4398.76 2533.53 22.93 -4655.98 -4891.49 -5081.67 The occurrence of a positive value for the enthalpy change (∆H0), demonstrates that the adsorption in this research is an endothermic process Furthermore, a positive entropy change (∆S0) indicates an increase in randomness at the solid/liquid interface during DB71 adsorption onto WSS Finally, the negative value of the Gibbs free energy (∆G0) illustrates the adsorption process's viability and spontaneity 4.4 Comparison A-WSH with other adsorbents in terms of qmax 57 To assess the effectiveness of A-WSS compared to other adsorbents in terms of DB71 adsorption, a study was conducted by reviewing the literature for maximum adsorption capacity (qmax) reported in various papers The findings of this study are presented in Table 4.9, summarizing the results Table 4.9: Comparison of the maximum adsorption capacity (qmax) of A-WSH in this work and those of other adsorbents in previous studies Adsorbents Modification method qmax (mg/g) References Unmodified adsorbents Sunflower stalk - 49 [24] Amberlite IRA 458 - 48 [28] Polyacrylate anion exchanger - 42 [29] Raw Kaolin - 36.41 [23] - 3.42 [32] 338.67 [26] FeCl3 294 [22] Acetic acid 156.25 Multiwalled carbon nanotubes (MWCNTs) Modified adsorbents Spent mushroom waste Poly pyrrole polymer composite (PPC) Acid activated WSS derived hydrochar (A-WSH) Chemically Modified Sunflower stalks Cetyltrimethylammonium bromide Quaternary ammonium group THIS STUDY 148 [24] 61.35 [21] Magnetic nanocomposite of chitosan/SiO2/carbon Fe3O4 and SiO2 nanotubes 58 Adsorbents Activated carbon-Thevetia Peruviana (TPAC) Modification method qmax (mg/g) References H3PO4 50 [22] As can be seen from Table 4.10, the activated waste shrimp shell used in this thesis is still far from another adsorbent, nevertheless, it is better than most of the other activated materials, and non-activated materials The maximum adsorption capacity of A-WSH is more than 1.5 -2 times higher than activated material, and 3.5 – 50 times compare to nonactivated materials 59 CHAPTER V: CONCLUSION AND RECOMMENDATIONS 5.1 Conclusion The A-WSH has been successfully synthesized from WSS using HTC and activation method Furthermore, the optimal conditions for DB71 adsorption onto A-WSH were natural pH (6.78), adsorbent dose of g/L, contact time of 4h, shaking speed of 120 rpm, and room temperature of 25 ± 0.5oC In addition, the DB71 adsorption onto A-WSH was satisfactorily described by Langmuir isotherm model and Pseudo-second-order kinetic model, and the maximum DB71 adsorption capacity (qmax) of A-WSH was 156.25 mg/g, which was significantly higher than those of other adsorbents Since A-WSH exhibited high qmax value, 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