The design and synthesis of graphene oxide at iron oxide (GOFexOy) for catalytic application

THAI NGUYEN UNIVERSITY UNIVERSITY OF AGRICULTURE AND FORESTRY XAYALACK LASY THE DESIGN AND SYNTHESIS OF GRAPHENE OXIDE AT IRON OXIDE (GO@FEXOY) FOR CATALYTIC APPLICATION BACHELOR THESIS Study Mode: Full-time Major: Environmental science and management Faculty: International Training and Developing center Batch: 43 Advance Education Program Thai Nguyen, October 2015 DOCUMENTATION PAGE WITH ABSTRACT Thai Nguyen University of Agriculture and Forestry Degree Program Bachelor of Environment science and Management Student name Xayalack Lasy Student ID DTN1153110275 Thesis title The design and synthesis of graphene oxide at iron oxide (GO@FexOy) for catalytic application Assoc Prof DR Tran Van Dien Supervisors Assoc Prof Yu-Fen Huang PhD Student He Yue PhD Student Celeste Abstract: The thesis describes the oxidation of methylene blue, a basic dye of thiazine series using a Fenton reaction at normal laboratory temperature and at atmospheric pressure and the advantages in use of magnetic nanoparticles (MNPs), graphene oxide @iron oxide nanoparticles(GO@FexOy) in the reaction Oxidation by Fenton reactions is proven and economically feasible process for destruction of a variety of hazardous pollutants in wastewater MNPs were synthesis via a thermal decomposition method and (GO@FexOy) via electrooxidation procedure The synthesis of MNPs and (GO@FexOy) was characterized by several techniques, Ultraviolet–visible spectroscopy (UV-Vis), and Transmission Electron Microscopy (TEM) The concentrations of dye degradation were determined ectrophotometrically using Plate Readers at 665 nm, the absorption maximum of the dye Keywords: Fenton reaction, nanocomposite, magnetic nanocomposites, Graphene oxide @ iron oxide nanoparticles, absorption, methylene blue, H2O2 Number of pages: 40 pages Date of submission: Supervisor’s signature September 30, 2015 ACKNOWLEDGEMENT First of all, we know that knowledge is just only can be proved by our works, and internship is one of the best opportunity for student whose can their first project before they find their jobs to enroll in the future Besides that, we are not only improving ourselves by knowledge in company environment, institute or laboratory but also making more friends whose are having many experiences in environment, and it will help us in the near future From my perspective, this internship is absolutely needed, helpful and important Because of that, and be assigned by the International Training Center and also the allowed of Department of Biomedical Engineering and Environmental Science (National Tsing Hua University, Taiwan) To well done this thesis, I want to express profound gratitude to Advanced Education Program, the school administrators, the staffs in Department of Biomedical Engineering and Environmental Science, the staffs of YF laboratory, and particularly my supervisor, Associate Prof DR Tran Van Dien and Associate Professor Huang Yu Fen whose is always support me every single time I got troubles I would like to send both of supervisor a warmly thanks for the supporting me, and for their sacrifice for education, as same as environmental issues in Taiwan and Vietnam as all countries in the world Finally, I would like to say that I have tried my best to finish this thesis in the best way, I guess However, to be honest, I partly believe that my thesis still have some problems because of the limitation of knowledge and reality experiences, especially in our environmental circumstances these days It is totally happy if I can get feedbacks and comments from you, my teachers, Professor, and Supervisor, to finish my thesis in a fantastic way, to get the best results Sincerely, Thai Nguyen, October, 2015 Student Xayalack Lasy STATEMENT BY THE AUTHOR I hereby declare that this submission is my own work from doing my experimental research and to the best of my knowledge, it contains no material previously published, nor material which to a substantial extent has been accepted for the award of any other degree or diploma at any educational institution, except where due acknowledgement is made in the thesis TABLE OF CONTENTS CHAPTER I INTRODUCTION .1 1.1 Rationale 1.2 Objectives .2 CHAPTER II LITERATURE REVIEW 2.1 Nanotechnologies and Nanomaterial .3 2.1.1 Nanotechnologies 2.1.2 Nanomaterial .4 2.1.3 Methods synthesis of nanomaterial 2.1.4 Overview of research and application of nanomaterial and nanocomposite 2.1.5 Magnetic NPs and application of magnetic NPs in wastewater treatment 11 2.2 Fenton reaction in the degradation of methylene blue 13 2.3 The use of magnetic nanocomposites in catalytic degradation of methylene blue 14 2.4 The equipment used to determine the properties of gold nanoparticles and methylene blue degradation 15 2.4.1 Ultraviolet–visible spectroscopy (UV-Vis) 15 2.4.2 Transmission Electron Microscopy (TEM) 15 CHAPTER III METHODOLOGY 18 3.1 Preparation of magnetic nanoparticles and Graphene oxide@iron oxide 18 3.1.1 Method synthesis Fe3O4 NPs 18 3.1.2 Method synthesis FeOx, GO@FexOy andGO-Au,FeOx 19 3.2 Fenton reaction and the use of Magnetic NPs and Graphene oxide@ iron oxide NPs in in Fenton reaction for catalytic degradation of dye 21 3.2.1 Chemicals and equipment 21 3.2.2 Method preparation stock solution: 22 3.2.3 Procedure 25 CHAPTER IV RESULTS AND DISCUSSIONS 26 4.1 Characterizations 26 4.1.1 Magnetic nanoparticles 26 4.2 Magnetic NPs and Graphene@iron oxide NPs apply in Fenton reaction degradation of methylene blue 27 4.2.1 Standard Fenton-like reaction for degradation of methylene blue 27 4.2.2 Application of magnetic nanoparticles,graphene oxide @iron-oxide on degradation of MB 31 4.2.3 The use of MNC, GO-FeOx in degradation of dye 34 CHAPTER V CONCLUSIONS AND RECOMMENDATION 36 5.1 Conclusions 36 5.2 Recommendation 36 REFERENCE 37 LIST OF FIGURES Figure 1.1 Diagram of principle synthesis of nanomaterial Figure 1.2 Ultraviolet–visible spectroscopy (UV-Vis) 15 Figure 1.3 Schematic diagram of a TEM Generally, TEM is divided into two main parts: illumination and imaging 17 Figure 1.4 Setup for synthesis MNC 18 Figure 1.5 Setup usingsonicators method 19 Figure 1.6 Setup for extract Fe3O4 NPs by centrifuging 19 Figure 1.7 Scheme for synthesis iron oxide, Graphen at iron oxide and Graphen at gold,iron oxide nanoparticles 20 Figure 1.8 Using plastic tubes to containing the solutions of MB degradation on the magnetic stirrer 25 Figure 1.9 TEM images of Fe3O4 NPs in different scale bar: (a) 50 nm; (b) 100 nm 26 Figure 2.0 dynamic light-scattering (DLS) 27 Figure 2.1 UV–Vis spectra of 3.13×10-5 M methylene blue solution at (control) with absorption maximum at 665 nm 27 Figure 2.2 Temporal UV–Vis spectra absorption showing changes the concentration of methyleneblue during Fenton reaction: a) at 0min; b) at 60min 28 Figure 2.3 Degradation of methylene blue by Fe (II) (pH 2-3) 28 Figure 2.4 Effect of [Fe2+] on degradation of MB at 60 minutes 29 Figure 2.5 Effect of [H2O2] on degradation of MB at 30 minutes 30 Figure 2.6 Effect of pH on degradation of MB 30 Figure 2.7 Degradation of methylene blue by Fe (II); Fe (II) + Fe (III) and Fe (III) at pH 2-3 31 Figure 2.8 the degradation of MB by GO-FeOx 3h 32 Figure 2.9 the degradation of MB by GO-Au,FeOx 5V 32 Figure 3.0 Detection of Concentration of GO-FeOx 3h and GO-Au, FeOx 5V 34 Figure 3.1 UV-vis absorption spectra of GO and GO-FeOx 35 Figure 3.2 recycle the degradation of GO-FeOx on MB 35 LIST OF TABLES Table 1.1 Chemicals used in the experiment 21 Table 1.2 Preparation of Methylene blue stock solution 22 Table 1.3 Preparation of H2SO4 stock solution 22 Table 1.4 Preparation of Fe2+ within H2SO4(0.1M)stock solution 23 Table 1.5 Preparation of Fe2+ without H2SO4stock solution 23 Table 1.6 Preparation stock solution of Fe2+ 24 Table 1.7 Preparation stock solution of H2O2 25 Table 1.8 detection concentration of GO-FeOx 3h and GO-Au,FeOx 5V 33 LIST OF ABBREVIATIONS AOP oxidation processes AFM The atomic force microscope Conc Concentration (GO@FeOx) Graphene oxide@iron oxide MNC Magnetic nanoclusters MNPs magnetic nanoparticles Concentration MB Methylene Blue OH• Radical Ppb Part per billion Ppm Part per million RO reverse osmosis SAM the scanning acoustic microscope STM Scanning Tunneling Microscope TEM Transmission Electron Microscopy UV-Vis Ultraviolet–visible spectroscopy CHAPTER IV RESULTS AND DISCUSSIONS 4.1 Characterizations 4.1.1 Magnetic nanoparticles Fe3O4 NPs were successfully synthesized via the thermal decomposition of Fe(acac)3 in benzyl ether and oleylamine By varying the volume ratio of benzyl ether and oleylamine, we can tune the NP sizes from 10 to 13 nm, a range that showed reasonably large magnetization and is suitable for a CVD catalytic study a) b) Figure 1.9 TEM images of Fe3O4 NPs in different scale bar: (a) 50 nm; (b) 100 nm The morphology of GO-FeOx was characterized by transmission electron microscopy (TEM) Typically, GO-FeOx hybrids exhibit a wrinkled sheet like structure Besides, FeOx nanoparticles were uniformly deposited on the surface of GO sheets in the GO-FeOx sample In addition, dynamic light-scattering (DLS) measurements showed that the size of GO-FeOx was 460 nm 26 40 35 30 25 Record 16: GO-Fe b2 20 Record 17: GO-Fe b2 15 Record 18: GO-Fe b2 10 -5 5000 10000 15000 Figure 2.0 dynamic light-scattering (DLS) 4.2 Magnetic NPs and Graphene@iron oxide NPs apply in Fenton reaction degradation of methylene blue 4.2.1 Standard Fenton-like reaction for degradation of methylene blue 4.2.1.1 Mechanism of Fenton reaction Fe2+ + H2O2 = Fe3+ + HO− + HO• (1) H2O2 + HO• = HO2• + H2O (2) 2+ 3+ Fe + HO• = Fe + HO − (3) The HO• radical is the main reactant in the process capable of detoxifying a number of organic substrates via oxidation The kinetic activity of this radical is also tremendous It reacts almost in a diffusion-controlled manner with second-order rate constant in the range 109–1010 dm3 mol−1 s−1 ( Ross, 1988) with a variety of reductants including attack to double bonds 4.2.1.2 Degradation of methylene blue 0min 0.8 0.6 0.4 0min 0.2 0 200 400 600 800 1000 Figure 2.1 UV–Vis spectra of 3.13×10-5 M methylene blue solution at (control) with absorption maximum at 665 nm 27 To verify the adsorption and the oxidation effect of the synthesized samples, methylene blue (MB) was used as a model molecule This compound was to monitor by simple UV-visible spectroscopy at its maximum absorption wavelength, 665 nm The absorption spetra was showed in figure 2.1 In a typical experiment, 5.73 ×10-4 M Fe2+ and 8×10−4 M H2O2 were added in 3.13×10-5 M methylene blue solution The reaction was adjusted pH at 2.5-3 by adding µL H2SO4 0.97% and took place at room temperature The UV-vis spectra showed the absorption of MB steadily decrease during reaction (Figure 2.2) The color of b to discoloration d after e60 Within first c solution changed from blue at reaction, degradation of MB occurred rapidly and almost 30% of MB was decayed The conversion efficiency of reaction was showed in Figure 2.3 0.4 a) 0.35 b) 0.3 3mins 0.25 5mins 0.2 15mins 0.15 30mins 0.1 60mins 0.05 0 200 400 600 800 1000 Figure 2.2 Temporal UV–Vis spectra absorption showing changes the concentration of methyleneblue during Fenton reaction: a) at 0min; b) at 60min Convesion efficiency (%) Fe II 0.8 0.6 0.4 0.2 Fe II 0.1 0.2 0.3 0.4 0.5 0.6 Concentration (mM) Figure 2.3 Degradation of methylene blue by Fe (II) (pH 2-3) 28 * Optimize [Fe2+] on degradation of MB With 3.13×10−5 M of MB solution, the rate of degradation showed remarkable dependence on the initial Fe2+ concentration used whereas no degradation was observed in the solution without H2O2 Experiments were performed at different Fe2+ concentrations 0.5×10−3 M; 1×10−3 M; 1.5×10−3 M; 2×10−3; 2.5×10−3 for fixed initial concentration of 4×10−4M, H2O2 and 3.13×10−5 M,MB, respectively By comparing the results of the MB after 1h, it was found that the conversion increased as the Fe2+concentration was increased from 0.5×10−3to 2.5×10−3M, and becomes practically constant when it exceeds 2.5×10−3M Fe2+ with different diluted Conversion effiviency (%) 100 80 60 Fe2+ with different diluted fold(X) 40 20 0 20 40 60 80 Time (min) Figure 2.4 Effect of [Fe2+] on degradation of MB at 60 minutes Thus, from the extent of degradation of the MB after 1h, we found that there was an optimum Fe2+ concentration for the most effective degradation of 3.13 × 10−5 M MB solutions Keeping the MB and H2O2 fixed at above concentrations, we studied the effect of variation of Fe2+ concentration for complete destruction of the MB * Optimize [H2O2] on degradation of MB In order to optimize of H2O2 concentration on the degradation kinetics, experiments were conducted at different H2O2 concentrations with 3.13×10−5 M MB and 0.01M Fe2+ solutions In the experiments, we observed that the concentration of the MB dropped instantaneously as H2O2 was added The H2O2 concentration was varied from 0.0003M to 0.0005 M At a fixed Fe2+ concentration of 0.01 M, the0.0005 29 M H2O2 concentration was thought to be the optimized concentration which caused more than 0.1 % conversion efficiency of MB within 30 minutes 0.7 Conversion efficiency (%) 0.6 0.5 0.4 0.3 0.2 0.1 -0.1 0.0001 0.0002 0.0003 0.0004 0.0005 0.0006 H2O2 with different dilute fold (x) Figure 2.5 Effect of [H2O2] on degradation of MB at 30 minutes * Effect of pH value on conversion efficiency of MB Reactions were carried out at a seriers of pH environment from 2.5 -7 pH value was adjusted by adding H2SO4 or NaOH owning to find the optimum pH for MB conversion The effect of pH on the conversion of the MB is shown in Fig 2.4 It showed that best effective conversion of MB was achieved about 43% within 1h when the solution pH was around 2.5 Conversion efficiency (%) 45 30 p H -3 p H -5 p H -7 15 0 30 60 T im e (m in ) Figure 2.6 Effect of pH on degradation of MB 30 4.2.2 Application of magnetic nanoparticles,graphene oxide @iron-oxide on degradation of MB 4.2.2.1 Standard Fenton reaction Both Fe3O4 magnetic nanoclusters and GO@FexOy nanocomposites have good catalytic potential on the degradation of methylene blue (André et al., 2014) In theory, the ratio between Fe (II) and Fe (III) reactants of Fe3O4 magnetic NPswas 0.5) As a result, Fe (II); Fe (III); Fe (II) + Fe (III) solution was considered to be our positive control which compared with ourmagnetic nanoclusters and GO@FexOy According to Figure 2.7, the decomposition of H2O2reaction was rapid at the beginning when inthe Fe (II) solution whereas decomposition of H2O2was slightly slower Interestingly, the changed profile of the mixed Fe (II) and Fe (III) solution was similar approach to Fe (II).So, according to above observation, we assume that while the decomposition of MB start with Fe (III), other reaction may be involved during the decomposition reaction, which was shown below: Fe3+ + HO2• = Fe2+ + O2 + H+ (4) Fe2+ + HO2• + H+ = Fe3+ + H2O2 (5) 2HO2• = H2O2 + O2 (6) Although, the reaction was prior to Fe (II) for the degradation, still all the three groups achieve to 90 % The reaction was almost complete 100 Conversion efficiency (%) 80 60 F e ( II) F e ( II) + F e ( III) F e ( III) 40 20 0 50 100 150 200 250 300 T im e (m in ) Figure 2.7 Degradation of methylene blue by Fe (II); Fe (II) + Fe (III) and Fe (III) at pH 2-3 31 4.2.2.2 Comparing GO-FeOx and GO-Au,FeOx on degradation of MB Figure 2.8 show that the degradation of Methalene blue by GO- FeOx 3h (50ul) with 3.13×10−5 M of MB (20ul), 4×10−4 M of H2O2 (8ul), 5×10−4 M of H2SO4 (1ul) and ddH2O (121ul) are the best and new one to degrade Methalene blue which spending time for hour as well as successful degradation in 0.1% 0.7 0.6 0.5 0.4 GO-FeOx 3h 0.3 Control 0.2 0.1 0 200 400 600 800 1000 Figure 2.8 the degradation of MB by GO-FeOx 3h Figure 2.9 Shows that the degradation of Methalene Blue by GO-Au,FeOx 5V(50ul) with 3.13×10−5 M of MB (20ul), 4×10−4 M of H2O2 (8ul), 5×10−4 M of H2SO4 (1ul) and ddH2O (121ul) are slowly degradation by spending time around hour as well as degradation of Methalene Blue in 0.2% 0.7 0.6 0.5 0.4 GO-Au,FeOx 5V 0.3 Control 0.2 0.1 0 200 400 600 800 1000 Figure 2.9 the degradation of MB by GO-Au,FeOx 5V 32 Therefore, this experimental research could compare that Figure 2.8 and Figure 2.9 are clearly different level of the degradation with comparing by control time and percent in degradation that GO-FeOx is the best in degradation of MB, which presented in a picture below 4.2.2.3 Detection Concentration ofGO-FeOx and GO-Au,FeOx Based on the detection concentration of GO-FeOx and GO-Au,FeOx, the researcher need to prepare a sample solution that made the control by using Fe3+ which different Concentration (mM) of each sample from sample to sample Then last sample adding sample7 (GO-FeOx3h) and sample ( GO-Au,FeOx 5V) with doing detection by adding all sample into plate reader and using UV- visible absorption spectra (Computer program) for detection automatically obtained data, by looking in the table below Concentration (mM) Abs (a u.) Sample Sample Sample Sample Sample Sample Sample Fe3+2 Fe3+1.6 Fe3+1.2 Fe3+0.8 Fe3+0.4 Fe3+0.2 GO-FeOx3h 1.720199943 1.417500019 1.235700011 0.995700002 0.614400029 0.298900008 Sample GO-Au,FeOx 5V 0.676299989 0.48089999 Table 1.8 detection concentration of GO-FeOx 3h and GO-Au,FeOx 5V 33 Then calculating by take the abs of GO-FeOx 3h and abs of GO-Au,FeOx 5V minus 0.282 and divide by 0.7404 is will be equals the Concentration of GO-FeOx 3h and GO-Au,FeOx Conc of GO-FeOx: 0.27 mM Conc of GO-Au, FeOx: 0.53 mM 3.5 2mM 2.5 1.6mM 1.2mM 1.5 0.8mM 0.4mM 0.5 0.2mM 0 1.8 1.6 1.4 1.2 0.8 0.6 0.4 0.2 10 15 20 y = 0.7404x + 0.282 R² = 0.9697 Series1 Linear (Series1) 0.5 1.5 2.5 Figure 3.0 detection of Concentration of GO-FeOx 3h and GO-Au,FeOx 5V 4.2.3 The use of MNC, GO-FeOx in degradation of dye Based on the conditions from the Fe (II); Fe (II) + Fe (III) and Fe (III) as above, MNC and GO@FeOxwas further investigated for MB degradation afterwards The conversion efficiency was conducted, with the Iron (II), Iron (III), Iron (II) + Iron (III), MNC, GO@FeOxbefore annealing andGO@FexOy after annealing The concentrations of H2O2 were kept at xx M Figure 3.1 shows UV-vis absorption spectra of GO and GO-FeOx, respectively The optical absorption spectrum of the GO suspension shows an absorption peak at 34 230 nm and a shoulder at 290 nm, corresponding to П–П* transitions for aromatic C=C and n–П* transitions for C=O bonds After the electro-deposition of FeOx on GO, the main absorption peak was broadened These changes can be assigned to the formation of a composite between the FeOx and the graphene sheets during the electro-deposition reaction Besides, the optical absorbance of GO–FeOx in the visible and NIR regions was significantly enhanced relative to pristine GO, likely owing to the partial reduction of GO during the formation of FeOx on GO sheets 0.5 0.4 0.3 0409 3h 1000rcf sub 0.1x 0.2 GO-FeOx sub 0.1x 0.1 0 200 400 600 800 1000 Figure 3.1UV-vis absorption spectra of GO and GO-FeOx Overall the degradation of Methalene Blue by GO-FeOx is not only one time degradation but it’s could be degraded several times of waste water or degraded of Methalene Blue So, based on the research experiment that GO-FeOx could reduce waste water possibility which mentioned in the figure 3.2 as well as it’s also process furthermore that it can recycle for the degradation of Methalene Blue again 12000 10000 8000 6000 0409 3h 1000rcf sub 0.1x GO-FeOx 4000 rGO-FeOx 2000 0 500 1000 1500 2000 2500 Figure 3.2recycle the degradation of GO-FeOx on MB 35 CHAPTER V CONCLUSIONS AND RECOMMENDATION 5.1 Conclusions The whole purpose of this experiment researching is comparing between Fe2+, Fe3+ whether which one will be the best on degradation of Methylene blue and powerful in reducing waste water, however Fe2+ and Fe3+ is not good enough to degraded MB, because both of this materials (Fe2+ and Fe3+) cannot be the best to a recycling degradation in several time Therefore replacing GO-FeOx 3h was necessary and important to progressing in this experiment that successfully degradation MB as specially this material (GO-FeOx) available to recycling degradation MB by several times So Graphene oxide @Iron oxide nanoparticles and magnectic nanoparticles were successfully synthesized by a simple and inexpensive synthetic procedure with controlled size and shell thickness The magnetic nanocomposites showed good catalytic performance for MB organic dye oxidation by H2O2after 1hours of reaction The reaction was able to proceed at pH neutral in room temperature 5.2 Recommendation We continue survey the synthesis of magnetic nanoparticles with different conditions to uniform the size of nanoparticles and optimum the synthetic procedure and continue lerning how to catalytic application of all nonmaterial for powerful and useful processing in recycle degradation of MB or waste water as well The research experimental is very important to explore new scientific ideas for improve and develop the previous ideas as very necessary as possible to optimize the concentration of H2O2, Fe (II), Fe (III) and magnetic nanocomposites using on degradation of MB 36 REFERENCES Akhavan, O., Azimirad, R (2009) Photocatalytic property of Fe2O3 nanograin chains coated by TiO2 nanolayer in visible light irradiation Appl Catal A Gen 369(1–2):77–82 Anh, D (2007) Synthesis and study of SERS and antimicrobial activity of Ag nanomaterials on silica carriers Chemical Master's thesis, University of Hanoi Education Bandara, J., Klehm, U., Kiwi, J (2007) Raschig rings–Fe2O3, composite photocatalyst activate in the degradation of 4-chlorophenol and Orange II under daylight irradiation Appl Catal B Environ 2007; 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Fenton reaction to demonstrate the degradation in water pollutants, a study: THE DESIGN AND SYNTHESIS OF GRAPHENE OXIDE AT IRON OXIDE (GO@ FexOy) FOR CATALYTIC APPLICATION" was conducted 1.2 Objectives... DTN1153110275 Thesis title The design and synthesis of graphene oxide at iron oxide (GO@FexOy) for catalytic application Assoc Prof DR Tran Van Dien Supervisors Assoc Prof Yu-Fen Huang PhD Student... concentration of Iron ion and Graphene oxide at Iron oxide * Design and synthesis to use Physical materials and Chemical materials on degradation of methylene blue * Determine optimum of H2O2