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Facile synthesis of Fe2O3 nanoparticles from Egyptian insecticide cans for efficient photocatalytic degradation of methylene blue and crystal violet dyes
Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 222 (2019) 117195
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Facile synthesis of Fe2O3 nanoparticles from Egyptian insecticide cans for efficient photocatalytic degradation of methylene blue and crystal violet dyes Ehab A. Abdelrahman a,⁎, R.M. Hegazey b, Yousra H. Kotp c, Ahmed Alharbi d a
Chemistry Department, Faculty of Science, Benha University, Benha 13518, Egypt Egyptian Petroleum Research Institute, Ahmed El Zumer Street, Nasr City, Hai Al-Zehour, Cairo 11727, Egypt. c Hydrogeochemistry Dept., Desert Research Center, El Mataryia Cairo 11753, Egypt d Department of Chemistry, Faculty of Applied Science, Umm Al-Qura University, Makkah, Saudi Arabia b
a r t i c l e
i n f o
Article history: Received 8 February 2019 Received in revised form 11 May 2019 Accepted 26 May 2019 Available online 31 May 2019 Keywords: Fe2O3 nanoparticles Insecticide cans Photocatalytic degradation Methylene blue dye Crystal violet dye
a b s t r a c t In this study, Fe2O3 (hematite) nanoparticles with different crystallite sizes (40–59 nm) were synthesized from Egyptian insecticide cans using the combustion method. The organic fuels were urea, glycine, L-alanine, and Lvaline. Fe2O3 nanoparticles were characterized utilizing different devices such as BET, PL, FT-IR, XRD, HR-TEM, FE-SEM, UV–Vis, and DTG. Crystal violet (CV) and methylene blue (MB) dyes were efficiently removed from aqueous solution by photocatalytic degradation under UV irradiation in the presence of Fe2O3 and H2O2. The % degradation of 50 mL crystal violet or methylene blue dye (20 mg/L) using 0.1 g Fe2O3 in the presence of H2O2 was 100% after 30 or 40 min, respectively. Also, the degradation processes are fitted well with the first order model. Besides, the photocatalytic activity of Fe2O3 unaltered even after it was reused three times. Hence, the synthesized Fe2O3 nanoparticles can be considered a promising and efficient photocatalyst for the degradation of crystal violet and methylene blue dyes. © 2019 Elsevier B.V. All rights reserved.
1. Introduction Synthetic dyes are utilized in numerous industries, for example, paper, textiles, and leather. The production of these dyes is 700,000 tons per year and results from 100,000 kinds of commercial dyes [1–5]. After the achievement of industrial purposes of these dyes, most of them are disposed in the environmental water bodies without treatment [6–8]. The dye effluent of textiles, paper and pulp, dyeing, tannery and paint, and dye industries are 54, 10, 21, 8, and 7%, respectively [9]. These dye effluents are considered toxic substances and harm humans, animals, and aquatic organisms [10,11]. Such contaminants must be removed from water resources because humans use water in daily activities such as washing, bathing, drinking, and cooking [12]. Also, among the reasons for getting rid of those contaminants is that they cause the destruction of the fish wealth. These dyes form a layer above the surface of the water. This layer blocks the sunlight and disrupts the respiration and photosynthesis of aquatic organisms [13]. In addition, these pollutants destroy the agricultural wealth because they fill the pores of the soil if they leaked into the fields [14]. Besides, these pollutants cause health problems such as skin irritation, difficulty in breathing, extreme sweating, confusion, nausea, vomiting, and cancer ⁎ Corresponding author. E-mail address: [email protected] (E.A. Abdelrahman).
https://doi.org/10.1016/j.saa.2019.117195 1386-1425/© 2019 Elsevier B.V. All rights reserved.
[15]. There are many ways for getting rid of these contaminants such as equalization/sedimentation, biological, advanced oxidation, electrochemical destruction, ozonation, adsorption, coagulation, membrane filtration, reverse osmosis, and photocatalytic degradation [16–25]. It is known that the photocatalytic degradation method is very effective in the removal of synthetic dyes. In this way, the sunlight or UV makes some electrons in the valence band transfer into the conduction band. Hence, holes and electrons were formed on the surface of the catalyst. Then, the holes and electrons produce hydroxide free radicals which known for its ability for the degradation of dyes into non-toxic gases such as carbon dioxide and water [26–30]. Many catalysts were used such as SnO2, SrTiO3, g-C3N4/TiO2/bentonite, Pd/CeO2, ZnO/ZnSe, ZnS, ZnO, Ag3PO4/g-C3N4, BiOBr/graphene oxide, TiO2, AgI/BiYO3, AgBr/ Ag3PO4, LaNdZr2O7/SnSe, ZnO/activated carbon, CoWO4, CdO, CdO/ CdS, and Fe2O3 [26–53]. Hematite (Fe2O3) is one of the most important catalysts due to its non-toxicity, high efficiency, and resistance to corrosion [44,54]. Many routes were used for the synthesis of Fe2O3 such as hydrothermal, microwave/ultrasound, thermal decomposition, electrospinning, combustion, and co-precipitation [54–64]. But, these methods require expensive chemicals such as iron sources. Therefore, iron wastes were considered by scientists [65]. There are many iron wastes in the Egyptian market such as insecticide cans. To the best of our knowledge, these wastes weren't used in the synthesis of Fe2O3. Combustion method was used for the synthesis of different
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Table 1 Characteristics and structure of crystal violet and methylene blue dyes.
Table 2 EDS of Egyptian insecticide cans, FU, FG, FA, and FV samples.
Methylene blue dye
Crystal Violet dye
Sample
Fe%
Sn%
O%
N%
Chemical formula: C16H18ClN3S Molar mass: 319.85 g/mol Melting point: 100 °C λmax: 663 nm
Chemical formula: C25H30ClN3 Molar mass:407.99 g/mol Melting point: 205 °C λmax: 590 nm
Waste FU FG FA FV
47.13 72.36 71.09 72.50 71.86
50.41 1.86 0.74 1.24 0.84
– 25.78 28.17 26.26 27.30
2.46 – – – –
nanoparticles because of its simplicity, low heat consumption, and low cost. In this paper, Fe2O3 nanoparticles were synthesized from Egyptian insecticide cans utilizing the combustion method. Organic fuels such as urea, glycine, L-alanine, and L-valine were used. In addition, the synthesized products were used as a catalyst for the photocatalytic degradation of crystal violet and methylene blue dyes under UV irradiation. 2. Experimental 2.1. Chemicals The utilized chemicals are nitric acid (HNO3), urea (CH4N2O), glycine (C2H5NO2), L-alanine (C3H7NO2), and L-valine (C5H11NO2). All of the aforementioned chemicals were purchased from Sigma-Aldrich Company. Egyptian insecticide cans were obtained from the local Egyptian market.
0.10 g of Fe2O3 catalyst was mixed with 50 mL crystal violet or methylene blue dye solution (20 mg/L) using a Pyrex beaker. Then, the mixture was stirred for 12 h in a dark place at 450 rpm for creating an adsorption/desorption equilibrium and distributing the catalyst well. After that, the beaker was placed for a specified time in a box containing five xenon arc UV lamps (365 nm, 250 W, Toshiba SHLS-002). In addition, the Fe2O3 catalyst was separated from crystal violet or methylene blue dye solution utilizing centrifugation at 2000 rpm. Then, the concentrations of crystal violet and methylene blue dyes were measured at 590 and 663 nm utilizing a UV–Vis spectrophotometer, respectively. The previous steps were repeated for more specified times. The % removal of crystal violet or methylene blue dyes after stirring in the dark was measured using Eq. (1). Also, the % degradation of crystal violet or methylene blue dyes at time t was measured utilizing Eq. (2). %removal ¼ ðCi −Cd Þ 100=Ci
2.2. Synthesis of hematite (Fe2O3) nanoparticles 4.290 g of Egyptian insecticide cans was dissolved in 30 mL nitric acid then the solution was diluted up to 100 mL using distilled water. The resulting solution was named solution M. 5.579 g of urea (92.890 mmoles), 4.649 g of glycine (61.929 mmoles), 3.311 g of L-alanine (37.165 mmoles), or 2.418 g of L-valine (20.640 mmoles) was dissolved in 40 mL distilled water. The resulting solution was named solution F. Then, solution F was added to solution M drop by drop with constant stirring at 250 °C till the whole solution evaporates. The remained powder was collected and calcined at 500 °C for 3 h. The samples which were synthesized using urea, glycine, L-alanine, and L-valine were labeled FU, FG, FA, and FV, respectively. 2.3. Photocatalytic degradation of dyes The photocatalytic degradation of crystal violet or methylene blue dyes at 365 nm under the action of UV irradiation was examined utilizing a Fe2O3 catalyst which was fabricated using glycine. Table 1 contains the characteristics and structure of crystal violet or methylene blue dye.
Fig. 2. XRD patterns of the FU (A), FG (B), FA (C), and FV (D) samples.
Fig. 1. EDS analysis of Egyptian insecticide cans.
ð1Þ
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Scheme 1. Proposed mechanism for the synthesis of Fe2O3 nanoparticles.
%degradation ¼ ðCd −Ct Þ 100=Cd
ð2Þ
where, Ci (mg/L) is the initial concentration of crystal violet dye or methylene blue, Cd (mg/L) is the concentration of crystal violet or methylene blue dye solution after adsorption/desorption equilibrium, and Ct (mg/L) is the concentration of crystal violet or methylene blue dye at irradiation time t.
3
Å. The elemental analysis and HR-TEM images of the Fe2O3 samples were obtained utilizing a transmission electron microscope (JEOL 2100; 200 kV). FT-IR spectra were obtained by measuring the Fe2O3 samples on an FT-IR spectrophotometer (Nicolet Avatar 230) from 4000 to 400 cm−1. After coating the Fe2O3 samples with gold on K550X sputter coater, the morphology of the Fe2O3 samples was obtained with an ultra-high resolution FE-SEM microscope (JSM5410JEOL). The EDS analysis of Egyptian insecticide cans was obtained using FE-SEM microscope (JSM5410JEOL) equipped with an energy-dispersive X-ray spectrometer SEM-EDX as clarified in Fig. 1 [66]. The optical energy gap of Fe2O3 samples and absorption spectra of crystal violet or methylene blue dyes were carried out utilizing a UV–Vis spectrophotometer (Jasco; Model v530). Thermal stabilities of the Fe2O3 samples were verified using a thermal analyzer (Shimadzu; DT-60H). The samples were measured in a nitrogen gas atmosphere from room temperature up to 1000 °C with a heating speed of 15 °C/ min. The room temperature photoluminescence (PL) spectra were obtained utilizing a thermo scientific fluorescence spectrophotometer (Model Lumina; He/Cd laser). The surface texturing properties such as BET surface area, mean pore radius, and total pore volume were measured from N2 adsorption isotherms at 77 K utilizing a Quantachrome apparatus after sample out-gassing at 473 K for 12 h. 3. Results and discussion
2.4. Physicochemical measurements 3.1. XRD and EDS XRD patterns were obtained by measuring the Fe2O3 samples on an X-ray diffraction apparatus (18 kW; Model D8 Advance; Bruker) outfitted with monochromated Cu Kα radiation with wavelength equals 1.54
Fig. 1 represents the EDS analysis of Egyptian insecticide cans. The results showed that this waste is composed of approximately equal
Fig. 3. FE-SEM images of the FU (A), FG (B), FA (C), and FV (D) samples.
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amounts of tin and iron as clarified in Table 2 [66]. Also, FU, FG, FA, and FV samples are composed of iron, oxygen, and a small percent of tin as clarified in Table 2. Fig. 2A–D represents XRD patterns of the FU, FG, FA, and FV samples, respectively. The results proved that all the synthesized samples are composed of hematite Fe2O3 (Rhombohedral; ICDD No. 01-076-4579; Space group: R-3c) [44]. The characteristic peaks of Fe2O3 at 2ɵ = 24.22, 33.26, 35.76, 40.97, 49.57, 54.17, 57.75, 62.53, 64.08, 72.06, and 75.56 can be attributed to lattice plans of (012), (104), (110), (113), (024), (116), (018), (214), (300), (1010), and (220), respectively. The crystallite size (Z, nm) of the Fe2O3 samples was measured utilizing Scherrer equation Eq. (3): Z ¼ 0:9λ=β cos θB
ð3Þ
where, λ, θB, and β are the wavelength of X-ray radiation, diffraction angle, and full width at half maximum, respectively [66–105]. The results confirmed that the crystallite sizes of the FU, FG, FA, and FV samples were 49, 40, 50, and 59 nm, respectively. The mechanism of the synthesis was illustrated in Scheme 1. Tin reacts with nitric acid forming nitrogen dioxide and tin oxide clouds. Also, iron reacts with nitric acid forming ferric nitrate. Besides, ferric nitrate reacts with different organic fuels (urea, glycine, L-alanine, and L-valine) forming Fe2O3 nanoparticles.
3.2. FE-SEM and HR-TEM Fig. 3A–D represents FE-SEM images of the FU, FG, FA, and FV samples, respectively. Spherical shapes have an average size of ca. 109, 103, and 165 nm were observed in the FU, FG, and FV samples, respectively. Also, spongy shapes have an average size of ca. 162 nm were observed in the FA sample. Fig. 4A–D represents HR-TEM images of the FU, FG, FA, and FV samples, respectively. Spherical, hexagonal, and irregular shapes have an average diameter of ca. 45, 43, 56, and 53 nm were observed in the FU, FG, and FV samples, respectively. The previous diameters were compatible with the XRD data. 3.3. FT-IR, optical energy gap, and thermal analysis Fig. 5A–D represents FT-IR spectra of the FU, FG, FA, and FV samples, respectively. The peaks which were observed at 429 and 517 cm−1 are due to Fe\\O bond vibrations [58,60,62]. The optical energy gap (Eg) of the FU, FG, FA, and FV samples was determined according to Eq. (4) utilizing the UV–Vis absorption spectra of the previous samples in nujoll mull [15,22–24]. Z
ðαhυÞ ¼ K hυ−Eg
ð4Þ
where, Z, K, and α are an integer depending on the type of transition, a
Fig. 4. HR-TEM images of the FU (A), FG (B), FA (C), and FV (D) samples.
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5
Fig. 5. FT-IR spectra of the FU (A), FG (B), FA (C), and FV (D) samples.
constant, and absorption coefficient, respectively. If Z = 2, directly allowed transitions were obtained. If Z = 0.5, indirectly allowed transitions were obtained. The plot of (αhυ) 2 versus hυ for the FU, FG, FA, and FV samples was clarified in Fig. 6A–D, respectively. Consequently, the directly allowed transitions were prevalent in all Fe2O3 samples. The optical energy gap (Eg) was determined by extrapolating the graph so that (αhυ)2 equals zero. The optical energy gaps of the FU, FG, FA, and FV samples were 1.52, 1.64, 2.50, and 2.45 eV, respectively. Fig. 7A–D represents the thermal analysis of the FU, FG, FA, and FV samples, respectively. The total weight loss percentages of the FU, FG, FA, and FV samples are 0.832, 1.034, 2.936, and 0.444%, respectively. Hence, this confirms the stability of the Fe2O3 samples. 3.4. Surface textures and photoluminescence The BET nitrogen adsorption-desorption isotherms of FU, FG, FA, and FV samples are given in Fig. 8A–D, respectively. The pertinent textural information is exhibited in Table 3. The obtained isotherms belong to type IV. The FG sample gives the highest surface area value and hence possesses the higher photocatalytic activity because it has the highest active sites. The PL emission spectra of FU, FG, FA, and FV samples are given in Fig. 9A–D, respectively. The FG sample gives the lowest emission
intensity value among peaks which centered at around 467 nm. Hence, this sample possesses the higher photocatalytic activity because it has the lowest recombination rate for the e−/h photogenerated carriers. 4. Photocatalytic degradation of crystal violet and methylene blue dyes The degradation of crystal violet or methylene blue dye utilizing UV irradiation and FG sample was studied. This Fe2O3 sample was chosen because it has the lowest crystallite size and emission intensity. The % removal of crystal violet and methylene blue dyes in the dark are 23.23 and 11.29%, respectively. Fig. 10A–B represents the visible spectra of methylene blue dye under the action of (FG UV) and (FG H2O2 UV), respectively. Also, Fig. 11A–B represents the visible spectra of crystal violet dye under the action of (FG UV) and (FG H2O2 UV), respectively. The results showed that the absorbance of the characteristic peaks at λmax was decreased when UV irradiation time was increased. In addition, Fig. 12A represents the relation between % degradation of dyes and irradiation time under the action of (FG UV) and (FG H2O2 UV). In the case of methylene blue (MB), the % degradation was 65.67% at 180 min and 100% at 40 min under the action of (FG UV)
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Fig. 6. The plot of (αhυ)2 versus hυ of the FU (A), FG (B), FA (C), and FV (D) samples.
Fig. 7. Thermal analysis of the FU (A), FG (B), FA (C), and FV (D) samples.
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Fig. 8. Nitrogen gas adsorption–desorption data for the FU (A), FG (B), FA (C), and FV (D) samples.
and (FG H2O2 UV), respectively. In the case of crystal violet (CV), the % degradation was 65.70% at 180 min and 100% at 30 min under the action of (FG UV) and (FG H2O2 UV), respectively. The photocatalytic degradation processes were described by the first order kinetic model using Eq. (5) [15,22–24]. ln ðCd =Ct Þ ¼ ðKobs Þ t
ð5Þ
where, Kobs (1/min) is the rate constant of the first order model. Fig. 12B represents the plot of time versus ln(Cd/Ct) of dyes under the action of (FG UV) and (FG H2O2 UV). The results showed that the photocatalytic degradation processes fitted well with the first order. The constants of the first order were clarified in Table 4. FG catalyst was calcined at 300 °C for the successful regeneration of it. After the regeneration process, it was used as photocatalyst for three cycles toward crystal violet or methylene blue dyes as previously described in the experimental part. The results proved that the photocatalytic activity of the FG sample unaltered even after it was reused three times. Scheme 2 represents the mechanism of the photocatalytic
degradation of crystal violet or methylene blue dyes. UV irradiation makes some electrons in the valence band transfer into the conduction band. Hence, holes (h ) and electrons (e−) were formed at the surface of Fe2O3 catalyst. Then, the holes react with hydroxide ion while electrons react with dissolved oxygen for the production of hydroxide free radicals which degrade methylene blue or crystal violet dyes into nontoxic gases such as carbon dioxide and water. Also, hydrogen peroxide reacts with electrons for the production of more hydroxide free radicals for enhancing the degradation of dyes [15,22–24].
Table 3 Texture properties of the FU, FG, FA, and FV samples. Sample
BET surface area (m2/g)
Total pore volume (cm3/g)
Mean pore radius (Ao)
FU FG FA FV
14.11 26.01 9.06 7.36
3.023E-02 4.438E-02 4.121E-02 3.491E-02
42.85 14.79 90.93 94.86
Fig. 9. Photoluminescence (PL) spectra of the FU (A), FG (B), FA (C), and FV (D) samples.
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Fig. 10. Visible spectra of methylene blue dye under the action of (FG UV) (A) and (FG H2O2 UV) (B).
Table 5 represents a comparative study between the synthesized Fe2O3 photocatalyst and other photocatalysts in the literature [106–111]. The comparison proved that the synthesized Fe2O3 efficiently degrades the methylene blue and crystal violet dyes.
5. Conclusions Hematite (Fe2O3) nanoparticles were synthesized from iron wastes utilizing the combustion method. Organic fuels such as urea, glycine,
Fig. 11. Visible spectra of crystal violet dye under the action of (FG UV) (A) and (FG H2O2 UV) (B).
Fig. 12. The relation between time and both of % degradation (A) and ln(Cd/Ct) (B).
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Acknowledgments
Table 4 First order constants of the degradation processes. Factors
MB MB CV CV
Parameters
FG UV FG H2O2 UV FG UV FG H2O2 UV
9
R2
Kobs (1/min)
0.893 0.977 0.986 0.899
0.00627 0.09795 0.00600 0.11120
L-alanine, and L-valine were used. In addition, the synthesized products were used as a catalyst for the photocatalytic degradation of crystal violet and methylene blue dyes under UV irradiation. In the case of crystal violet (CV), the % degradation was 65.70% at 180 min and 100% after 30 min under the action of (FG UV) and (FG H2O2 UV), respectively. In the case of methylene blue (MB), the % degradation was 65.67% at 180 min and 100% at 40 min under the action of (FG UV) and (FG H2O2 UV), respectively.
The corresponding author “Ehab A. Abdelrahman” gratefully thanks his wife “Asmaa Elsayed Fetoh” for her continuous encouragement. References [1] J. Abdi, M. Vossoughi, N. Mohammad, Synthesis of metal-organic framework hybrid nanocomposites based on GO and CNT with high adsorption capacity for dye removal, Chem. Eng. J. 326 (2017) 1145–1158. [2] M. Rafatullah, O. Sulaiman, R. Hashim, A. Ahmad, Adsorption of methylene blue on low-cost adsorbents: a review, J. Hazard. Mater. 177 (2010) 70–80. [3] C.R. Holkar, A.J. Jadhav, D.V. Pinjari, N.M. Mahamuni, A.B. Pandit, A critical review on textile wastewater treatments: possible approaches, J. Environ. Manag. 182 (2016) 351–366. [4] R. Paper, Non-conventional low-cost adsorbents for dye removal: a review, Bioresour. Technol. 97 (2006) 1061–1085. [5] V.K. Gupta, Application of low-cost adsorbents for dye removal – a review, J. Environ. Manag. 90 (2009) 2313–2342. [6] S. De Gisi, G. Lofrano, M. Grassi, M. Notarnicola, Characteristics and adsorption capacities of low-cost sorbents for wastewater treatment: a review, SUSMAT 9 (2016) 10–40.
Scheme 2. Proposed mechanism for the degradation of methylene blue and crystal violet dyes.
Table 5 Comparative study between the synthesized Fe2O3 photocatalyst and other photocatalysts in the literature. Photocatalyst
Dye
E
Name
W (g)
Name
C(mg/L)
V(mL)
Fe/FeS Co alloyed CdZnS Iron oxide Degussa P25 Titania Degussa P25 Titania CuO Fe2O3 Fe3O4/SnO2 ZnO HgO Fe2O3
0.5 0.03 0.1 0.2 0.2 0.1 0.1 0.5 0.1 0.1 0.1
MB MB MB MB MB MB MB CV CV CV CV
5 25 10 11.5 11.5 10 20 8.16 8.16 20 20
40 25 100 100 100 50 50 500 40 50 50
E = Excitation source, V = Volume, C = Concentration, and W = Weight.
Visible light UV light Visible light Visible light Laser, 150 mJ pulse energy UV light UV light UV light Visible light UV light UV light
% Degradation
Ref
Value
Time (min)
96 83 100 40 34 96.18 100 83 83 100 100
200 100 140 120 120 360 40 180 60 180 30
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Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy journal homepage: www.elsevier.com/locate/saa
Facile synthesis of Fe2O3 nanoparticles from Egyptian insecticide cans for efficient photocatalytic degradation of methylene blue and crystal violet dyes Ehab A. Abdelrahman a,⁎, R.M. Hegazey b, Yousra H. Kotp c, Ahmed Alharbi d a
Chemistry Department, Faculty of Science, Benha University, Benha 13518, Egypt Egyptian Petroleum Research Institute, Ahmed El Zumer Street, Nasr City, Hai Al-Zehour, Cairo 11727, Egypt. c Hydrogeochemistry Dept., Desert Research Center, El Mataryia Cairo 11753, Egypt d Department of Chemistry, Faculty of Applied Science, Umm Al-Qura University, Makkah, Saudi Arabia b
a r t i c l e
i n f o
Article history: Received 8 February 2019 Received in revised form 11 May 2019 Accepted 26 May 2019 Available online 31 May 2019 Keywords: Fe2O3 nanoparticles Insecticide cans Photocatalytic degradation Methylene blue dye Crystal violet dye
a b s t r a c t In this study, Fe2O3 (hematite) nanoparticles with different crystallite sizes (40–59 nm) were synthesized from Egyptian insecticide cans using the combustion method. The organic fuels were urea, glycine, L-alanine, and Lvaline. Fe2O3 nanoparticles were characterized utilizing different devices such as BET, PL, FT-IR, XRD, HR-TEM, FE-SEM, UV–Vis, and DTG. Crystal violet (CV) and methylene blue (MB) dyes were efficiently removed from aqueous solution by photocatalytic degradation under UV irradiation in the presence of Fe2O3 and H2O2. The % degradation of 50 mL crystal violet or methylene blue dye (20 mg/L) using 0.1 g Fe2O3 in the presence of H2O2 was 100% after 30 or 40 min, respectively. Also, the degradation processes are fitted well with the first order model. Besides, the photocatalytic activity of Fe2O3 unaltered even after it was reused three times. Hence, the synthesized Fe2O3 nanoparticles can be considered a promising and efficient photocatalyst for the degradation of crystal violet and methylene blue dyes. © 2019 Elsevier B.V. All rights reserved.
1. Introduction Synthetic dyes are utilized in numerous industries, for example, paper, textiles, and leather. The production of these dyes is 700,000 tons per year and results from 100,000 kinds of commercial dyes [1–5]. After the achievement of industrial purposes of these dyes, most of them are disposed in the environmental water bodies without treatment [6–8]. The dye effluent of textiles, paper and pulp, dyeing, tannery and paint, and dye industries are 54, 10, 21, 8, and 7%, respectively [9]. These dye effluents are considered toxic substances and harm humans, animals, and aquatic organisms [10,11]. Such contaminants must be removed from water resources because humans use water in daily activities such as washing, bathing, drinking, and cooking [12]. Also, among the reasons for getting rid of those contaminants is that they cause the destruction of the fish wealth. These dyes form a layer above the surface of the water. This layer blocks the sunlight and disrupts the respiration and photosynthesis of aquatic organisms [13]. In addition, these pollutants destroy the agricultural wealth because they fill the pores of the soil if they leaked into the fields [14]. Besides, these pollutants cause health problems such as skin irritation, difficulty in breathing, extreme sweating, confusion, nausea, vomiting, and cancer ⁎ Corresponding author. E-mail address: [email protected] (E.A. Abdelrahman).
https://doi.org/10.1016/j.saa.2019.117195 1386-1425/© 2019 Elsevier B.V. All rights reserved.
[15]. There are many ways for getting rid of these contaminants such as equalization/sedimentation, biological, advanced oxidation, electrochemical destruction, ozonation, adsorption, coagulation, membrane filtration, reverse osmosis, and photocatalytic degradation [16–25]. It is known that the photocatalytic degradation method is very effective in the removal of synthetic dyes. In this way, the sunlight or UV makes some electrons in the valence band transfer into the conduction band. Hence, holes and electrons were formed on the surface of the catalyst. Then, the holes and electrons produce hydroxide free radicals which known for its ability for the degradation of dyes into non-toxic gases such as carbon dioxide and water [26–30]. Many catalysts were used such as SnO2, SrTiO3, g-C3N4/TiO2/bentonite, Pd/CeO2, ZnO/ZnSe, ZnS, ZnO, Ag3PO4/g-C3N4, BiOBr/graphene oxide, TiO2, AgI/BiYO3, AgBr/ Ag3PO4, LaNdZr2O7/SnSe, ZnO/activated carbon, CoWO4, CdO, CdO/ CdS, and Fe2O3 [26–53]. Hematite (Fe2O3) is one of the most important catalysts due to its non-toxicity, high efficiency, and resistance to corrosion [44,54]. Many routes were used for the synthesis of Fe2O3 such as hydrothermal, microwave/ultrasound, thermal decomposition, electrospinning, combustion, and co-precipitation [54–64]. But, these methods require expensive chemicals such as iron sources. Therefore, iron wastes were considered by scientists [65]. There are many iron wastes in the Egyptian market such as insecticide cans. To the best of our knowledge, these wastes weren't used in the synthesis of Fe2O3. Combustion method was used for the synthesis of different
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E.A. Abdelrahman et al. / Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 222 (2019) 117195
Table 1 Characteristics and structure of crystal violet and methylene blue dyes.
Table 2 EDS of Egyptian insecticide cans, FU, FG, FA, and FV samples.
Methylene blue dye
Crystal Violet dye
Sample
Fe%
Sn%
O%
N%
Chemical formula: C16H18ClN3S Molar mass: 319.85 g/mol Melting point: 100 °C λmax: 663 nm
Chemical formula: C25H30ClN3 Molar mass:407.99 g/mol Melting point: 205 °C λmax: 590 nm
Waste FU FG FA FV
47.13 72.36 71.09 72.50 71.86
50.41 1.86 0.74 1.24 0.84
– 25.78 28.17 26.26 27.30
2.46 – – – –
nanoparticles because of its simplicity, low heat consumption, and low cost. In this paper, Fe2O3 nanoparticles were synthesized from Egyptian insecticide cans utilizing the combustion method. Organic fuels such as urea, glycine, L-alanine, and L-valine were used. In addition, the synthesized products were used as a catalyst for the photocatalytic degradation of crystal violet and methylene blue dyes under UV irradiation. 2. Experimental 2.1. Chemicals The utilized chemicals are nitric acid (HNO3), urea (CH4N2O), glycine (C2H5NO2), L-alanine (C3H7NO2), and L-valine (C5H11NO2). All of the aforementioned chemicals were purchased from Sigma-Aldrich Company. Egyptian insecticide cans were obtained from the local Egyptian market.
0.10 g of Fe2O3 catalyst was mixed with 50 mL crystal violet or methylene blue dye solution (20 mg/L) using a Pyrex beaker. Then, the mixture was stirred for 12 h in a dark place at 450 rpm for creating an adsorption/desorption equilibrium and distributing the catalyst well. After that, the beaker was placed for a specified time in a box containing five xenon arc UV lamps (365 nm, 250 W, Toshiba SHLS-002). In addition, the Fe2O3 catalyst was separated from crystal violet or methylene blue dye solution utilizing centrifugation at 2000 rpm. Then, the concentrations of crystal violet and methylene blue dyes were measured at 590 and 663 nm utilizing a UV–Vis spectrophotometer, respectively. The previous steps were repeated for more specified times. The % removal of crystal violet or methylene blue dyes after stirring in the dark was measured using Eq. (1). Also, the % degradation of crystal violet or methylene blue dyes at time t was measured utilizing Eq. (2). %removal ¼ ðCi −Cd Þ 100=Ci
2.2. Synthesis of hematite (Fe2O3) nanoparticles 4.290 g of Egyptian insecticide cans was dissolved in 30 mL nitric acid then the solution was diluted up to 100 mL using distilled water. The resulting solution was named solution M. 5.579 g of urea (92.890 mmoles), 4.649 g of glycine (61.929 mmoles), 3.311 g of L-alanine (37.165 mmoles), or 2.418 g of L-valine (20.640 mmoles) was dissolved in 40 mL distilled water. The resulting solution was named solution F. Then, solution F was added to solution M drop by drop with constant stirring at 250 °C till the whole solution evaporates. The remained powder was collected and calcined at 500 °C for 3 h. The samples which were synthesized using urea, glycine, L-alanine, and L-valine were labeled FU, FG, FA, and FV, respectively. 2.3. Photocatalytic degradation of dyes The photocatalytic degradation of crystal violet or methylene blue dyes at 365 nm under the action of UV irradiation was examined utilizing a Fe2O3 catalyst which was fabricated using glycine. Table 1 contains the characteristics and structure of crystal violet or methylene blue dye.
Fig. 2. XRD patterns of the FU (A), FG (B), FA (C), and FV (D) samples.
Fig. 1. EDS analysis of Egyptian insecticide cans.
ð1Þ
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Scheme 1. Proposed mechanism for the synthesis of Fe2O3 nanoparticles.
%degradation ¼ ðCd −Ct Þ 100=Cd
ð2Þ
where, Ci (mg/L) is the initial concentration of crystal violet dye or methylene blue, Cd (mg/L) is the concentration of crystal violet or methylene blue dye solution after adsorption/desorption equilibrium, and Ct (mg/L) is the concentration of crystal violet or methylene blue dye at irradiation time t.
3
Å. The elemental analysis and HR-TEM images of the Fe2O3 samples were obtained utilizing a transmission electron microscope (JEOL 2100; 200 kV). FT-IR spectra were obtained by measuring the Fe2O3 samples on an FT-IR spectrophotometer (Nicolet Avatar 230) from 4000 to 400 cm−1. After coating the Fe2O3 samples with gold on K550X sputter coater, the morphology of the Fe2O3 samples was obtained with an ultra-high resolution FE-SEM microscope (JSM5410JEOL). The EDS analysis of Egyptian insecticide cans was obtained using FE-SEM microscope (JSM5410JEOL) equipped with an energy-dispersive X-ray spectrometer SEM-EDX as clarified in Fig. 1 [66]. The optical energy gap of Fe2O3 samples and absorption spectra of crystal violet or methylene blue dyes were carried out utilizing a UV–Vis spectrophotometer (Jasco; Model v530). Thermal stabilities of the Fe2O3 samples were verified using a thermal analyzer (Shimadzu; DT-60H). The samples were measured in a nitrogen gas atmosphere from room temperature up to 1000 °C with a heating speed of 15 °C/ min. The room temperature photoluminescence (PL) spectra were obtained utilizing a thermo scientific fluorescence spectrophotometer (Model Lumina; He/Cd laser). The surface texturing properties such as BET surface area, mean pore radius, and total pore volume were measured from N2 adsorption isotherms at 77 K utilizing a Quantachrome apparatus after sample out-gassing at 473 K for 12 h. 3. Results and discussion
2.4. Physicochemical measurements 3.1. XRD and EDS XRD patterns were obtained by measuring the Fe2O3 samples on an X-ray diffraction apparatus (18 kW; Model D8 Advance; Bruker) outfitted with monochromated Cu Kα radiation with wavelength equals 1.54
Fig. 1 represents the EDS analysis of Egyptian insecticide cans. The results showed that this waste is composed of approximately equal
Fig. 3. FE-SEM images of the FU (A), FG (B), FA (C), and FV (D) samples.
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amounts of tin and iron as clarified in Table 2 [66]. Also, FU, FG, FA, and FV samples are composed of iron, oxygen, and a small percent of tin as clarified in Table 2. Fig. 2A–D represents XRD patterns of the FU, FG, FA, and FV samples, respectively. The results proved that all the synthesized samples are composed of hematite Fe2O3 (Rhombohedral; ICDD No. 01-076-4579; Space group: R-3c) [44]. The characteristic peaks of Fe2O3 at 2ɵ = 24.22, 33.26, 35.76, 40.97, 49.57, 54.17, 57.75, 62.53, 64.08, 72.06, and 75.56 can be attributed to lattice plans of (012), (104), (110), (113), (024), (116), (018), (214), (300), (1010), and (220), respectively. The crystallite size (Z, nm) of the Fe2O3 samples was measured utilizing Scherrer equation Eq. (3): Z ¼ 0:9λ=β cos θB
ð3Þ
where, λ, θB, and β are the wavelength of X-ray radiation, diffraction angle, and full width at half maximum, respectively [66–105]. The results confirmed that the crystallite sizes of the FU, FG, FA, and FV samples were 49, 40, 50, and 59 nm, respectively. The mechanism of the synthesis was illustrated in Scheme 1. Tin reacts with nitric acid forming nitrogen dioxide and tin oxide clouds. Also, iron reacts with nitric acid forming ferric nitrate. Besides, ferric nitrate reacts with different organic fuels (urea, glycine, L-alanine, and L-valine) forming Fe2O3 nanoparticles.
3.2. FE-SEM and HR-TEM Fig. 3A–D represents FE-SEM images of the FU, FG, FA, and FV samples, respectively. Spherical shapes have an average size of ca. 109, 103, and 165 nm were observed in the FU, FG, and FV samples, respectively. Also, spongy shapes have an average size of ca. 162 nm were observed in the FA sample. Fig. 4A–D represents HR-TEM images of the FU, FG, FA, and FV samples, respectively. Spherical, hexagonal, and irregular shapes have an average diameter of ca. 45, 43, 56, and 53 nm were observed in the FU, FG, and FV samples, respectively. The previous diameters were compatible with the XRD data. 3.3. FT-IR, optical energy gap, and thermal analysis Fig. 5A–D represents FT-IR spectra of the FU, FG, FA, and FV samples, respectively. The peaks which were observed at 429 and 517 cm−1 are due to Fe\\O bond vibrations [58,60,62]. The optical energy gap (Eg) of the FU, FG, FA, and FV samples was determined according to Eq. (4) utilizing the UV–Vis absorption spectra of the previous samples in nujoll mull [15,22–24]. Z
ðαhυÞ ¼ K hυ−Eg
ð4Þ
where, Z, K, and α are an integer depending on the type of transition, a
Fig. 4. HR-TEM images of the FU (A), FG (B), FA (C), and FV (D) samples.
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5
Fig. 5. FT-IR spectra of the FU (A), FG (B), FA (C), and FV (D) samples.
constant, and absorption coefficient, respectively. If Z = 2, directly allowed transitions were obtained. If Z = 0.5, indirectly allowed transitions were obtained. The plot of (αhυ) 2 versus hυ for the FU, FG, FA, and FV samples was clarified in Fig. 6A–D, respectively. Consequently, the directly allowed transitions were prevalent in all Fe2O3 samples. The optical energy gap (Eg) was determined by extrapolating the graph so that (αhυ)2 equals zero. The optical energy gaps of the FU, FG, FA, and FV samples were 1.52, 1.64, 2.50, and 2.45 eV, respectively. Fig. 7A–D represents the thermal analysis of the FU, FG, FA, and FV samples, respectively. The total weight loss percentages of the FU, FG, FA, and FV samples are 0.832, 1.034, 2.936, and 0.444%, respectively. Hence, this confirms the stability of the Fe2O3 samples. 3.4. Surface textures and photoluminescence The BET nitrogen adsorption-desorption isotherms of FU, FG, FA, and FV samples are given in Fig. 8A–D, respectively. The pertinent textural information is exhibited in Table 3. The obtained isotherms belong to type IV. The FG sample gives the highest surface area value and hence possesses the higher photocatalytic activity because it has the highest active sites. The PL emission spectra of FU, FG, FA, and FV samples are given in Fig. 9A–D, respectively. The FG sample gives the lowest emission
intensity value among peaks which centered at around 467 nm. Hence, this sample possesses the higher photocatalytic activity because it has the lowest recombination rate for the e−/h photogenerated carriers. 4. Photocatalytic degradation of crystal violet and methylene blue dyes The degradation of crystal violet or methylene blue dye utilizing UV irradiation and FG sample was studied. This Fe2O3 sample was chosen because it has the lowest crystallite size and emission intensity. The % removal of crystal violet and methylene blue dyes in the dark are 23.23 and 11.29%, respectively. Fig. 10A–B represents the visible spectra of methylene blue dye under the action of (FG UV) and (FG H2O2 UV), respectively. Also, Fig. 11A–B represents the visible spectra of crystal violet dye under the action of (FG UV) and (FG H2O2 UV), respectively. The results showed that the absorbance of the characteristic peaks at λmax was decreased when UV irradiation time was increased. In addition, Fig. 12A represents the relation between % degradation of dyes and irradiation time under the action of (FG UV) and (FG H2O2 UV). In the case of methylene blue (MB), the % degradation was 65.67% at 180 min and 100% at 40 min under the action of (FG UV)
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Fig. 6. The plot of (αhυ)2 versus hυ of the FU (A), FG (B), FA (C), and FV (D) samples.
Fig. 7. Thermal analysis of the FU (A), FG (B), FA (C), and FV (D) samples.
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7
Fig. 8. Nitrogen gas adsorption–desorption data for the FU (A), FG (B), FA (C), and FV (D) samples.
and (FG H2O2 UV), respectively. In the case of crystal violet (CV), the % degradation was 65.70% at 180 min and 100% at 30 min under the action of (FG UV) and (FG H2O2 UV), respectively. The photocatalytic degradation processes were described by the first order kinetic model using Eq. (5) [15,22–24]. ln ðCd =Ct Þ ¼ ðKobs Þ t
ð5Þ
where, Kobs (1/min) is the rate constant of the first order model. Fig. 12B represents the plot of time versus ln(Cd/Ct) of dyes under the action of (FG UV) and (FG H2O2 UV). The results showed that the photocatalytic degradation processes fitted well with the first order. The constants of the first order were clarified in Table 4. FG catalyst was calcined at 300 °C for the successful regeneration of it. After the regeneration process, it was used as photocatalyst for three cycles toward crystal violet or methylene blue dyes as previously described in the experimental part. The results proved that the photocatalytic activity of the FG sample unaltered even after it was reused three times. Scheme 2 represents the mechanism of the photocatalytic
degradation of crystal violet or methylene blue dyes. UV irradiation makes some electrons in the valence band transfer into the conduction band. Hence, holes (h ) and electrons (e−) were formed at the surface of Fe2O3 catalyst. Then, the holes react with hydroxide ion while electrons react with dissolved oxygen for the production of hydroxide free radicals which degrade methylene blue or crystal violet dyes into nontoxic gases such as carbon dioxide and water. Also, hydrogen peroxide reacts with electrons for the production of more hydroxide free radicals for enhancing the degradation of dyes [15,22–24].
Table 3 Texture properties of the FU, FG, FA, and FV samples. Sample
BET surface area (m2/g)
Total pore volume (cm3/g)
Mean pore radius (Ao)
FU FG FA FV
14.11 26.01 9.06 7.36
3.023E-02 4.438E-02 4.121E-02 3.491E-02
42.85 14.79 90.93 94.86
Fig. 9. Photoluminescence (PL) spectra of the FU (A), FG (B), FA (C), and FV (D) samples.
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Fig. 10. Visible spectra of methylene blue dye under the action of (FG UV) (A) and (FG H2O2 UV) (B).
Table 5 represents a comparative study between the synthesized Fe2O3 photocatalyst and other photocatalysts in the literature [106–111]. The comparison proved that the synthesized Fe2O3 efficiently degrades the methylene blue and crystal violet dyes.
5. Conclusions Hematite (Fe2O3) nanoparticles were synthesized from iron wastes utilizing the combustion method. Organic fuels such as urea, glycine,
Fig. 11. Visible spectra of crystal violet dye under the action of (FG UV) (A) and (FG H2O2 UV) (B).
Fig. 12. The relation between time and both of % degradation (A) and ln(Cd/Ct) (B).
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Acknowledgments
Table 4 First order constants of the degradation processes. Factors
MB MB CV CV
Parameters
FG UV FG H2O2 UV FG UV FG H2O2 UV
9
R2
Kobs (1/min)
0.893 0.977 0.986 0.899
0.00627 0.09795 0.00600 0.11120
L-alanine, and L-valine were used. In addition, the synthesized products were used as a catalyst for the photocatalytic degradation of crystal violet and methylene blue dyes under UV irradiation. In the case of crystal violet (CV), the % degradation was 65.70% at 180 min and 100% after 30 min under the action of (FG UV) and (FG H2O2 UV), respectively. In the case of methylene blue (MB), the % degradation was 65.67% at 180 min and 100% at 40 min under the action of (FG UV) and (FG H2O2 UV), respectively.
The corresponding author “Ehab A. Abdelrahman” gratefully thanks his wife “Asmaa Elsayed Fetoh” for her continuous encouragement. References [1] J. Abdi, M. Vossoughi, N. Mohammad, Synthesis of metal-organic framework hybrid nanocomposites based on GO and CNT with high adsorption capacity for dye removal, Chem. Eng. J. 326 (2017) 1145–1158. [2] M. Rafatullah, O. Sulaiman, R. Hashim, A. Ahmad, Adsorption of methylene blue on low-cost adsorbents: a review, J. Hazard. Mater. 177 (2010) 70–80. [3] C.R. Holkar, A.J. Jadhav, D.V. Pinjari, N.M. Mahamuni, A.B. Pandit, A critical review on textile wastewater treatments: possible approaches, J. Environ. Manag. 182 (2016) 351–366. [4] R. Paper, Non-conventional low-cost adsorbents for dye removal: a review, Bioresour. Technol. 97 (2006) 1061–1085. [5] V.K. Gupta, Application of low-cost adsorbents for dye removal – a review, J. Environ. Manag. 90 (2009) 2313–2342. [6] S. De Gisi, G. Lofrano, M. Grassi, M. Notarnicola, Characteristics and adsorption capacities of low-cost sorbents for wastewater treatment: a review, SUSMAT 9 (2016) 10–40.
Scheme 2. Proposed mechanism for the degradation of methylene blue and crystal violet dyes.
Table 5 Comparative study between the synthesized Fe2O3 photocatalyst and other photocatalysts in the literature. Photocatalyst
Dye
E
Name
W (g)
Name
C(mg/L)
V(mL)
Fe/FeS Co alloyed CdZnS Iron oxide Degussa P25 Titania Degussa P25 Titania CuO Fe2O3 Fe3O4/SnO2 ZnO HgO Fe2O3
0.5 0.03 0.1 0.2 0.2 0.1 0.1 0.5 0.1 0.1 0.1
MB MB MB MB MB MB MB CV CV CV CV
5 25 10 11.5 11.5 10 20 8.16 8.16 20 20
40 25 100 100 100 50 50 500 40 50 50
E = Excitation source, V = Volume, C = Concentration, and W = Weight.
Visible light UV light Visible light Visible light Laser, 150 mJ pulse energy UV light UV light UV light Visible light UV light UV light
% Degradation
Ref
Value
Time (min)
96 83 100 40 34 96.18 100 83 83 100 100
200 100 140 120 120 360 40 180 60 180 30
[106] [107] [108] [109] [109] [22] This study [110] [111] [15] This study
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