Green biosynthesis of Fe3O4 nanoparticles using Chlorella vulgaris extract for enhancing degradation of 2,4 dinitrophenol

Tahani Saad AlGarni; Mohamed H.H. Ali; Amal M. Al-Mohaimeed

doi:10.1016/j.jksus.2022.102426

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Original article

01 2022

:35;

102426

doi:

10.1016/j.jksus.2022.102426

Green biosynthesis of Fe₃O₄ nanoparticles using Chlorella vulgaris extract for enhancing degradation of 2,4 dinitrophenol

Tahani Saad AlGarni^{^a}, Mohamed H.H. Ali^{^b}, Amal M. Al-Mohaimeed^{^a}

a Department of Chemistry, College of Science, King Saud University, Saudi Arabia

b National Institute of Oceanography & Fisheries, Cairo, Egypt

Received: 2022-6-1, Accepted: 2022-10-30,

Disclaimer:
This article was originally published by Elsevier and was migrated to Scientific Scholar after the change of Publisher.

Peer review under responsibility of King Saud University.

Abstract

Objectives

This study aimed to provide the excellent role of Chlorella vulgaris extract as a green, reducing agent for improving and enhancing the effectiveness and performance of as-prepared NPs, which is higher than bare Fe₃O₄.

Methods

The extract of the algal cell of Chlorella vulgaris is used as a green, reducing agent was used to prepare green Fe₃O₄ NPs to improve and enhance the degradation effectiveness of 2,4 dinitrophenol (2,4 DNP) in their aqueous solution using UV irradiation. The as-synthesized bare Fe₃O₄ and green Fe₃O₄ NPs were characterized using UV–VIS spectroscopy, TEM, SEM, EDX, XRD, and FT-IR spectroscopy to determine bandgap energy, particle size, structural morphology, crystallite nature, phase structure, elemental compositions, and existed functional group.

Results

SEM and TEM images indicated that the as-synthesized NPs have a regular spherical shape with a mean size ranging between 13.68 and 31.71 nm. The energy bandgap (E_g) indicated the green Fe₃O₄ NPs have low values (2.73 and 2.3 eV) than bare Fe₃O₄ (2.89 eV). The maximum degradation of 2,4 DNP was achieved at pH = 8, 90 min contact time, 0.35 g/L catalyst dose, and 100 mg/L 2,4 DNP concentration.

Conclusion

The degradation results proved that green Fe₃O₄ NPs have more effectiveness than bare Fe₃O₄ NPs.

Keywords

Magnetite

Fe3O4

Photodegradation

2, 4 Dinitrophenol

Chlorella vulgaris

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1 Introduction

Phenols and most of their derivatives are regarded as toxic pollutants to the surrounding environment (Mirza Hedayat et al., 2018). These compounds in the surrounding environment, especially in the foodstuff, cause possible hazardous effects on human life because of their high toxicity and carcinogenicity (Ali et al. 2019a). 2,4-DNP used pesticides, petrochemicals industries, dyes, and explosives (Zhang et al. 2016). Exposure to the high concentration of 2,4-DNP causes several health problems such as cell metabolism raising, cardiac disorder, and allergy.

Many researchers have been widely used advanced nanotechnology techniques to eliminate and remove different types of organic and inorganic pollutants, especially dyes and phenolic compounds; Congo red degradation (Ali et al. 2022; Karaman et al. 2022), methylene blue degradation (Li et al. 2022; Ali et al. 2019b), 2,4-dichlorophenol oxidation (Alturiqi et al., 2021), degradation of rhodamine B dye (Ali et al. 2018), and phenol degradation (Shaari et al. 2012).

Recently, the green synthesis of NPs has attracted the attention of numerous researchers due to their high advantages, and there are successful researches in the preparation of Fe₃O₄-NPs by using plant extract. For instance, green tea (Ananthi et al. 2022), Chamomile extract (Veisi et al. 2021), Chlorella vulgaris (Govarthanan et al. 2020), the leaf extract of Zanthoxylum armatum (Ramesh et al. 2018), Ulva flexuosa (Mashjoor et al., 2018), extract of Artemisia annua and leaf extract of Perilla frutescens (Basavegowda et al. 2014), Caricaya papaya (Latha and Gowri 2014), Tridax procumbens (Senthil and Ramesh 2012).

Naturally, iron oxides are found in different chemical forms; iron oxide (FeO), maghemite (γ-Fe₂O₃), and hematite (α-Fe₂O₃). Magnetite (Fe₃O₄) is the most common existing form. The magnetite crystal structure shows an inverse spinel pattern (Blaney 2007). Nonetheless, as points of nano-biocompatibility, the green synthesis of magnetic iron oxide (Fe₃O₄ NPs) is considered one of the advanced techniques by the green route. The green as-synthesized Fe₃O₄ NPs has characterized by low-cost, non-toxic, high availability, high surface area, sustainable, cleaner, biocompatible, and eco-environmentally more than the conventional chemo-physical technologies (Mashjoor et al. 2018).

As a result, the study's primary goals are: (i) green preparation of Fe₃O₄ NPs using Chlorella vulgaris and (ii) characterize the fabricate Fe₃O₄@C. vul. NPS uses different characterization methods. In addition, enhancing 2,4 DNP photodegradation under specific conditions such as pH of the solution, irradiation time, and catalyst dose.

2 Materials and methods

2.1

2.1 Chemicals and materials

All used chemicals in this study, including; ferrous sulfate heptahydrate (FeSO₄·7H₂O), ferric chloride hexahydrate (FeCl₃·6H₂O), ammonia solution (NH₄OH), and 2,4 dinitrophenol were purchased from Sigma-Aldrich and Merck chemical companies in analytical grade. Chlorella vulgaris was obtained from National Research Center (NRC), Cairo, Egypt.

2.2

2.2 Culturing and sampling of Chlorella vulgaris

C. vulgaris was isolated from Manzala Lake, north of Egypt. The isolate species were purified by dilution and planting according to Sen et al. (2005) method (more details in Supplementary section).

2.3

2.3 Preparation of green iron oxide (Fe3O4.NPs)

Liu et al. (2008) methods was used to prepare iron oxide (Fe₃O₄) NPs using the co-precipitation (more details in Supplementary section).

2.4

2.4 Physical characterizations

UV–vis spectroscopy was carried out using (Shimadzu −2450, Tokyo, Japan) spectrometer. XRD examination was carried out using Philips X-ray diffractometer (Model PW-3710). SEM, TEM and EDX were carried out using a Zeiss-EVO emission scanning electron microscope (model Carl Zeiss, USA). FTIR was done using a spectrometer (6700FTIR, Nicolet, America).

2.5

2.5 Batch adsorption experiment

The degradation process of 2,4 DNP was investigated using as-synthesized Fe₃O₄, Fe₃O₄@C.vul (2:1), and Fe₃O₄@C.vul (1:1) in a photoreactor unit using UV irradiation. Different conditions that affect the 24 DNP degradation were investigated at different pH of the 2,4 DNP solution, several irradiation time intervals, different catalytic doses, and initial concentration of 2,4 DNP as important factors that affect the adsorption process (more details in Supplementary section).

The efficiency of the photocatalytic process (q_e) was calculated according to the following equation Eqs. (1) and (2);

(1)

q_{e} = \frac{(C_{i} - C_{f}) x V}{M}

(2)

R % = \frac{(C_{i} - C_{f}) x 100}{C_{j}}

Where; V is the solution volume used, C_i initial 2,4 DNP concentration, C_r final 2,4 DNP concentration, and M is the mass of the catalyst (g).

3 Results and discussion

3.1

3.1 Characterization

The spectral absorption of UV–Vis showed that two strong bands appeared at 230 and 260 nm, indicating the presence of terpenoids, tannins, phenolic acid, alkaloids, carbohydrates, and flavonoids in green Fe₃O₄ NPs (Fig. 1a). These findings agree with the results obtained by Ramesh et al. (2018) for green Fe₃O₄ using Zanthoxylum armatum extract. Another weak band appeared at 360 nm, indicating Fe₃O₄ NPs formation (Ahmad et al. 2009).

(a) UV–VIS spectra of diffuse reflectance and (b-d) plot of Tauc relation for estimation Eg of bare and green Fe3O4 NPs.

The energy band gap has been calculated using Tauc’s equation (Eq 3).

(αhu)² = A (hu-E_g) Eq 3.

Figure (1b-d), indicates the energy bandgap of the bare Fe₃O₄ NPs and as-synthesized green Fe₃O₄ NPs. The calculated E_g are 2.89, 2.73, and 2.3 eV for as-synthesized Fe₃O₄ NPs. These values are considered suitable for using these nanoparticles as photocatalysts to degrade most organic compounds (Govarthanan et al. 2020). Moreover, the obtained E_g values are very close to those obtained by Ananthi et al. (2022), who reported E_g of 2.78 eV and 2.24 eV for as-prepared Fe₃O₄ NPs.

X-ray diffraction analysis was used to determine the crystallographic and phase structure of the green synthesized Fe₃O₄ NPs (Fig. 2). An observable peak appeared at d = 7.662 Å, corresponding to 2θ = 11.54 (JCPDS 85–1436), indicating the cubic phase of Fe₃O₄ (Ananthi et al. 2022). Several typical peaks belonging to Fe₃O₄ are appeared at 2θ = 30.21, 35.71, 44.61, 53.54, 57.0, and 62.64° corresponding to (2 2 0), (3 1 1), (4 0 0), (4 2 2), (5 1 1) and (4 4 0) respectively (JCPDS 65–3107) (Wang et al. 2022).

XRD pattern of bare Fe3O4, Fe3O4@C vul. 2:1 and Fe3O4@C vul. 1:1 nanoparticle.

The external morphological structure of the surface of as-synthesized green Fe₃O₄ NPs was detected by SEM images. Fig. (3a&b) shows the SEM photos of prepared green Fe₃O₄ NPs, with regular aggregated spherical shapes with a highly porous surface (Ting and Chin 2020). The porosity of green Fe₃O₄ NPs plays an important role in increasing the degradation process of organic particles throughout the high adsorption efficiency of dye molecules (Ali et al. 2019a).

SEM images of a) bare Fe3O4 and b) green Fe3O4 with C. vulgaris NPs. and EDX images of c) bare Fe3O4 and d) green Fe3O4 with C. vulgaris NPs.

Fig. 3 (c&d) shows the EDX spectrograms, bare Fe₃O₄ showed only two peaks, Fe (69.7 %) and O (30.3 %), indicating the formation of pure Fe₃O₄ only. Some minor peaks appeared in bio-Fe₃O₄ NPs (Fig. 3c) belonging to N (4.3), Si (3.1 %), and S (1.02 %). These findings are similar to those conducted by Wang et al (2022), who reported three peaks attributed to Fe (63.7 %), O (28.8 %), and C (7.5 %) in the formation of Fe₃O₄/pectin NPs.

TEM photos of bare Fe₃O₄ and green Fe₃O₄ NPs indicated that most formed NPs crystallites have a cubic-spherical shape with an average size ranging between 55.8 and 172.9 nm for bare Fe₃O₄ (Fig. 4a), and these diameters were diminished in the green Fe₃O₄ NPs and ranged between 13.68 and 31.71 nm (Fig. 4b).

Transmission electron microscope (TEM) images of as-synthesized a) bare Fe3O4; b) Fe3O4@ C. vul (2:1), c) Fe3O4@ C. vul (1:1) NPs.

Three distinct peaks were appeared at 3675, 3386, and 2372 cm⁻¹ in bio-Fe₃O₄ NPs while they don't appear in the bare Fe₃O₄ NPs (Fig. 5); the first peak at 3675 cm⁻¹ due to stretching O—H vibration reveal existence of polyphenolic group, while the second peak at 3386 cm⁻¹ attributed to the bending stretching N—H of amine group. The band at 2372 cm⁻¹, belonged to stretching vibrations of CH₂ (Mashjoor et al. 2018). Some intensive peaks appeared in all synthesized Fe₃O₄ NPs at 1715, 1616, and 1471 cm⁻¹, corresponding to pectin-carbohydrate, and amide I groups. The peaks recorded at 1288, 1187, and 1152 cm⁻¹ are characterized by asymmetric and symmetric stretching vibrations of the carboxyl group (–COOH) group, proving that green-Fe₃O₄ NPs due to the effect of algal extract (Senthil and Ramesh, 2012).

FTIR Spectrum of bare Fe3O4; Fe3O4@C. vul (2:1) and Fe3O4@C. vul (2:1) NPs.

3.2

3.2 Batch experiments

3.2.1

3.2.1 Effect of pH

the pH of the altering the reaction conditions leading to affecting the absorption and degradation of the 2,4 DNP molecules (Rani et al. 2020). Thus, the decomposition of 2,4 DNP under the impact of various pH values (2–9) was carried out to investigate the photocatalytic activities of bio-Fe₃O₄ NPs (Fig. 6). The degradation reaction shows low degradation in acidic conditions (pH < 6) followed by gradual increase with increasing pH values till reaches maximum degradation at pH 8 with q_e = 84.30, 85.8, and 86.4 mg/g for bare Fe₃O₄, Fe₃O₄@C. vul (2:1) and Fe₃O₄@C vul. (1:1) respectively. The increasing degradation in neutral and basic conditions owing to lowering of H⁺ ion and elevation of OH^– at these conditions creates a negative charge on the catalyst NPs surfaces; therefore, favor adsorption of 2,4 DNP on the surface of catalysts occurred (Ramesh et al. 2018). Many studies by Chen et al. (2017), Rani and Shanker (2019), and Lu et al. (2013) indicated that the neutral and slight basic conditions were more suitable conditions for maximum photodegradation of phenolic derivatives (Table 1).

Effect of pH on the degradation of 2,4 DNP (C0 = 100 mg/L, T = 25 °C) using green Fe3O4 NPs.

Table 1 Degradation efficiency of some photocatalysts under the optimum conditions for some phenolic compounds.

Organic substrate	Catalyst	pH	Conc. (mg/L)	Time (min)	Dose (g/L)	Eff. %	Ref
Methylene blue	Fe₃O₄ with Zanthoxylum armatum extract	11	15	180	*	70	Ramesh et al. (2018)
Bisphenol	H₃PW₁₂O₄₀/TiO₂.	8.2	20	240	6.3 %	90	Lu et al. (2013)
Phenol	Florsil –Pd(II)	*	20	180	0.5	80	Lupa et al. (2020)
2,4 DNP	Fe₃O₄@SiO₂@TiO₂/rGO	7	30	35	0.3	90	Mirza Hedayat et al. (2018)
2,4-DNP	CdHCC with Azadirachta indica leaf extract	7	50	12 h	0.25	97	Rani et al. (2020a)
2,4 DNP	BiOI/Fe₃O₄@GO	4	50	60	1	60	Singh et al. (2019)
2,4 DNP	ZnFe₂O₄-ZrO₂	7.2	15	50	0.2	98	Chen et al. (2017)
Phenol	ZnO@FeHCF	7	2	24 h	0.25	91	Rani and Shanker (2019)
2,4 DNP	Fe₃O₄ with C. vulgaris	6	50	60	0.3	>85	Recent data

* not available.

3.2.2

3.2.2 Effect of exposure time

The photodegradation of 2,4 DNP was carried out under different UV irritation times (5 – 120 min, Fig. 7). The results clearly showed two phases of the degradation of 2,4 DNP. The first is the rapid phase observed at the beginning of the reaction till it reaches 60 min due to the large accessibility of active sites on the catalyst surface. After that, the decrease of the availability of active sites as a result of its occupying the second phase has appeared with slowed dawn of the reaction till reached equilibrium at 90 min achieving maximum degradation efficiency with q_e of 83.1, 86.6, 88.1 mg/g for used photocatalysts respectively (Fig. 7). Further increasing time, there was no further degradation of 2,4 DNP, indicating attain the reaction equilibrium (Ramesh et al. 2018). Singh et al. (2019) reported 60 min for maximum decomposition of 2,4 DNP using BiOI/Fe₃O₄@GO, while MirzaHedayat et al. (2018) reported 30 min as optimum contact time for breakdown of 2,4-DNP using Fe₃O₄@SiO₂@TiO₂/rGO (Table 1).

Effect of contact time on the degradation of 2,4 DNP (pH = 8, C0 = 100 mg/L, T = 25 °C, and dose 0.35 g/L) using green Fe3O4 NPs.

3.2.3

3.2.3 Effect of dose

The degradation process applicability depends mainly on the used catalyst amount load. Thereby, various catalyst doses (0.05 – 0.4 g/L) were investigated for 2,4 DNP degradation (Fig. 8). A remarkable increase in reaction rate was observed with increasing catalyst dose from 0.05 g/L to 0.35 mg/L. The degradation efficiency of 2,4 DNP increased from 50 %, reaching a maximum of 83.8 %. With further increase of catalyst amount, there was no more degradation the reaction became declining (Fig. 8). The maximum degradation occurs due to the great availability of numerous active sites on the catalyst surface (Rani et al. 2020). Increasing the catalyst amount may lead to particle aggregation of catalyst and solution opaqueness, so the light scattered, and the reaction was deactivated (Ali et al., 2022). Some researchers supported our results, such as Chen et al. (2017) found that 25 mg/l is an optimum catalyst amount for degradation of 2,4 DNP using ZnFe₂O₄-ZrO₂. In addition, MirzaHedayat et al. (2018) reported that 0.3 g/L of Fe₃O₄@SiO₂@TiO₂/rGO is the optimum dose for maximum degradation of 2,4 DNP.

Effect of catalyst amount on the degradation of 2,4 DNP (pH = 8, C0 = 100 mg/L, T = 25 °C, t = 90 min) using green Fe3O4 NPs.

3.2.4

3.2.4 Effect of initial 2,4 DNP concentration

The results of different initial concertation of 2,4 DNP on the photodegradation process were studied as shown in (Fig. 9). It is observed a gradual decrease of removal percentage from 95 % for 10 mg/L concentration of 2,4 DNP till reaches 84.5 % at 100 mg/L of 2,4 DNP. The very low concentration of DNP doesn't express the real degraded amount of 2,4 DNP. At the same time, this low amount is consumed completely while the active sites are still empty. Calculating the maximum efficiency q_e using Eq (1) indicated low qe (9.32 mg/g) for 10 mg/L DNP. The maximum q_e (86.6 mg/g) was achieved at 100 mg/L. A further increase of 2,4 DNP concentration led to a lowering of the photodegradation ability of the catalyst (Rani and Shanker 2020). The decrease of the photodegradation process at a high concentration of 2,4 DNP is mainly attributed to the formation of intermediates in a lot of quantity which may compete with the 2,4 DNP particles and absorb UV light, leading to reducing the efficiency of the degradation process (MirzaHedayat et al. 2018).

Effect of initial concentration of 2,4 DNP on the degradation process (pH = 8, T = 25 °C, t = 90 min) using green Fe3O4 NPs.

4 Isotherms studies

Langmuir and Freundlich models, were applied to investigate the photodegradation process. The obtained results (Table S1, Figs S1 and S2) show that the correlation coefficient (R²) is almost > 0.99 for the used two isothermal models indicating that both Freundlich and Langmuir models well fit the photodegradation process of 2,4 DNP for all used Fe₃O₄ NPs (supplementary data).

5 Kinetics models

To predict the variation of the adsorbate concentration (2,4DNP) through the experimental time using the catalyst, two commonly known kinetic models were used (Table S2, Figs S3 & S4). The obtained results proved that the degradation of 2,4 DNP obeyed the pseudo-second-order reaction with q_e values ranging between 43.47 and 44.05 mg/g and the corresponding R² > 0.99 (more details in supplementary data).

6 Conclusion

In this current work, the green synthesis of Fe₃O₄ NPs using extract of algal cells of Chlorella vulgaris is regarded as a promise a novel, promise, eco-friendly effective, and cheap photocatalyst for the degradation of 2,4-DNP from the aqueous solution under UV light. SEM and TEM images indicated that the as-synthesized NPs have a regular spherical shape with a mean size ranging between 13.68 and 31.71 nm. The calculated E_g from Tauc's plot indicated the green Fe₃O₄ NPs have low values (2.73 and 2.3 eV) than bare Fe₃O₄ (2.89 eV). The photodegradation of 2,4DNP was carried out under specific conditions; pH of the solution, duration time, catalyst dose, and initial 2,4 DNP concentration to investigate the optimum condition and achieve maximum degradation process. The obtained results showed that basic condition (pH = 8), 90 min contact time, 0.35 g/L catalyst dose, and 100 mg/L 2,4 DNP concentration are the most favorable conditions for the degradation process. The degradation process has shown significant effectiveness using green Fe₃O₄ NPs more than bare Fe₃O₄ NPs. The studied isothermal models indicated that both Freundlich and Langmuir models better fit the photodegradation process. Moreover, the lowering value of q_max for bare Fe₃O₄ than green Fe₃O₄ NPs proves that Chlorella vulgaris extracted greatly improves the properties of Fe₃O₄ catalyst and enhances its degradation efficiencies. Kinetically, the results showed that the pseudo-second-order reaction better expresses the adsorption reaction type than the pseudo-first-order reaction model.

Acknowledgement

The authors extend their appreciation to the Deputyship for Research & Innovation, Ministry of Education in Saudi Arabia for funding this research work through the project no. (IFKSURG-2-120).

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

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Zhang X., Wang L., Liu C., Ding Y., Zhang S., Zeng Y., Liu Y., Luo S., . A bamboo-inspired hierarchical nanoarchitecture of Ag/CuO/TiO₂ nanotube array for highly photocatalytic degradation of 2,4-dinitrophenol. J. Hazard. Mater.. 2016;313:244-252.
[Google Scholar]

Introduction

Materials and methods

Chemicals and materials
Culturing and sampling of Chlorella vulgaris
Preparation of green iron oxide (Fe3O4.NPs)
Physical characterizations
Batch adsorption experiment

Results and discussion

Characterization
Batch experiments

Isotherms studies

Kinetics models

Conclusion

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