Dyes are one of the most dangerous chemical compounds in industrial wastewater, including textile wastewater. Reactive dyes have many applications in the textile industry. Nevertheless, due to the high solubility and stability of these dyes in water, the discharge of wastewater containing these dyes to receiving waters prevents the transmission of sunlight to aquatic environments and disrupts biological processes. The aim of this study was to synthesize N_doped FeNi3/TiO2 nano-photocatalyst and to investigate the removal efficiency of reactive red 195 dye from aqueous medium. In this study, the effect of important variables was investigated including initial concentration including pH (3-11), contact time (5 - 200 minutes), dye concentration (5 - 40 mg l-1), and nanocomposite dose (1 - 6 g l-1), in removal of reactive red 195 dye. The characteristics of the synthesized nanocomposites were also studied using BET, FTIR, FESEM, and VSM techniques. The results of this study revealed that increasing the contact time and decreasing the dye concentration enhanced the adsorption efficiency. The highest percentage of RR 195 dye adsorption was 82% after 90 minutes at the adsorbent concentration of 4 g l-1, pH=3 and the initial concentration of RR 195 of 5 mg l-1. Detection techniques also confirmed the synthesis of good quality synthesized nanocomposites. According to the results, the advanced oxidation process of N-doped FeNi3/Tio2 nano-photocatalyst had a high efficiency removal of reactive red 195 dye adsorption from aqueous medium. As a result, this method can be used effectively in the treatment of colored wastewater.
Research Article
Synthesis and application of N_doped FeNi3/TiO2 nano-photocatalyst in advanced oxidation process to remove reactive red 195 dye from aqueous medium
https://doi.org/10.21203/rs.3.rs-1453184/v1
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N-dopedFeNi3/Tio2 nanocomposite
photocatalytic degradation
advanced oxidation
RR195 pollutant
Many dyes are produced due to the waste and residuals of textile, dyeing, printing, rubber, paper, plastic, and related industries. Most dyes have aromatic rings in their structure making them highly toxic, non-biodegradable, carcinogenic, and mutagenic to the human body and aquatic animals (Yaman & Gündüz 2015). Meanwhile, in terms of dye production, the most important industries are usually the textile and dyeing industries (Somayajula et al. 2012).The textile industry is an important part of the industries of developing countries (Aksakal & Ucun 2010). About one-fifth of the total dye production in the textile industry is transferred to the environment through wastewater (Chládková et al. 2015). Dyes are classified into three main categories: anionic (direct, acidic and reactive), cationic (all primary colors), and non-ionic (dispersed colors) (Mahmoud et al. 2016). Azoic dyes are the largest group of dyes used for textile dyeing and other industrial applications (Mate & Pathade 2012). Dyes are chemical compounds that are important for a variety of reasons, including reduced light permeability and disrupted photosynthesis in water sources. Aesthetically, these compounds also negatively affect water quality and cause allergies, dermatitis, skin irritation, cancer, and genetic mutations in humans (Mahmoud et al. 2013). Reactive red 195 contains an active group consisting of an aromatic heterocyclic ring containing fluoride or chloride ions (Tahir et al. 2016). This dye is commonly used for dyeing cellulose fabrics and printing on fabric textures (Birmole et al. 2019).
Many aromatic color rings can affect the residues of various substances that are mutagenic, non-biodegradable, carcinogenic, and toxic to humans. Traditional methods cannot easily eliminate colors (Clavijo & Osma 2019). Thus, the removal of dye from industrial wastewater for environmental safety is challenging (Rani et al. 2017). Azo RR 195 dye is one of the dyes that includes the reaction group and is used in industries (Raval, Shah, Ladha, et al. 2016). There are various methods introduced as water treatment, such as Fenton, flocculation and adsorption processes, biological treatment, electrochemical techniques, ion exchange, advanced oxidation processes, and photocatalytic degradation under ultraviolet light (Rahimi et al. 2011). Advanced oxidation process or AOPs can be used in the decomposition of most organic and inorganic compounds without producing waste and problems with temperature and atmospheric pressure (Raval, Shah, & Shah 2016).
An important mediator produced in this process is reactive hydroxyl radicals (OH−) which can support primary oxidants such as TiO2, H2O2, UV, etc. In recent years, the use of magnetic nanoparticles as adsorbents to remove various contaminants has increased for RR 195 due to their important properties such as easy separation by an external magnetic field, easy synthesis, high surface area, and easy surface modification (Badruddoza et al. 2011). On the other hand, magnetic nanoparticles have challenges that prevent applications such as rapid aggregation, oxidation, etc. (Solisio & Aliakbarian 2017).
One way to mitigate such challenges is to use a composite shell structure to preserve the core and magnetic properties of FeNi3 as well as other iron alloys. When an insulating shell is used, nanocomposites in RR red 195uce the performance, stability and aggregation of nanoparticles and RR red 195 their toxicity (Zhu et al. 2018). On the other hand, the special properties of TiO2 as a cost-effective, non-toxic, and stable nanoparticle for a long time can be used as a catalyst to purify water and eliminate air pollution (Farooghi et al. 2018). Studies have shown that doping non-metals such as nitrogen (N), carbon (C), sulfur (S), and fluorine (F) with Tio2 would lower the recombination property and improve the photocatalytic activity of this particle under visible light with a wavelength greater than 400 nm (Ho et al. 2006). Among these non-metals, nitrogen is important due to its low ionization energy, similar size to oxygen, and high stability (Asahi et al. 2001). In the created structure, nitrogen ions replace oxygen ions in the Tio2 lattice and create a new energy level in the Tio2 bond gap, reducing the electron-hole recombination property (Huang et al. 2007). The process of TiO2 oxidation begins with the exchange of adsorption and diffusion (Lu et al. 2011). The photocatalytic limitations of TiO2 are due to the small surface area and low adsorption properties. Formation of different composites and hybrids can cover these limitations thus enhancing their efficiency and reverse degradation (Liu et al. 2005). In general, TiO2 interacts with metal ions in oxidation radicals to reduce oxidation and improve the light absorption spectrum. In addition, metal ions help reduce electron hole recombination by trapping electrons (Nasseh, Taghavi, et al. 2019). In addition, as shown in our previous studies (Khodadadi et al. 2019), the significant degradation efficiencies of organic pollutants using Fe-Ni3/TiO2 indicate the good potential of this technique as a real wastewater treatment system of an oil refinery. The results revealed that the combination of iron with Ni3 can turn it into a photocatalyst (Nasseh et al. 2018). In the present paper, FeNi3 magnetic nanoparticles have been fabricated using nickel and iron salts (Eslami et al. 2016; Nasseri & Sadeghzadeh 2013) and N-dopped in the Fe-Ni3/TiO2 synthesized structure. Its photocatalytic activity to remove RR 195 from aqueous solution in the presence of visible light has been examined (Kamranifar et al. 2018; Nasseh, Barikbin, et al. 2019).
2.1 Chemicals
The dye used in this study was a dye (RR195) solution with a molecular weight of 1136.32 and molecular formula of C31H19ClN7Na5O19S6 (Tan et al. 2012). A spectrophotometric device with a wavelength of 540 nm was used to measure the residual dye concentration (Birmole et al. 2019).
Other materials used included hydrazinium hydrate with formula N2H4.H2O with 80% purity, ethanol (C2H5OH), titanium butoxide (TBOT) with formula C12H28O4Ti, iron chloride with formula FeCl2 (4H2O), hydrogen peroxide 1 gr, 6% w Nickel NiCL2 (6H2O), HCl, and NaOH all produced by Merck. Dionysian water was used to prepare the solutions. The method described in Standard Method Book No. 5220 was employed for measurement (Clesceri et al. 2012).
The devices used included spectrophotometer (model (UV/Vis T80 +, FTIR (model AVATAR 370 made in USA with spectrometer in the range of (400–4000 cm), FESEM (model SLGMA Vp-500 Zeiss made in Germany) and VSM (model LAKE shore 7404 made in USA). BET analysis was performed by using model device (BElSORP Mini, Microtrac Bel Corp).
2.2 N_doped FeNi3/TiO2 composite synthesis method
2.2.1 Synthesis of Fe-Ni3
Initially, 1 gram of polyethylene glycol 6000 was dissolved in 180 ml of ion-free water. Then 0.713 g of nickel chloride and 0.198 g of iron chloride were dissolved separately in two containers containing 30 ml of ion-free water and added to the first solution. After complete mixing, using sodium hydroxide, the pH of the solution was adjusted between 12 and 13, then 9.1 ml of hydrazine hydrate (N2H4.H2O) with a concentration of 80% was added to the obtained suspension. The reaction was carried out for 24 hours at room temperature and the pH was constantly monitored during this time to maintain the desired range. Finally, the obtained FeNi3 nanocomposite was rinsed with water and ethanol in several steps. This nanocomposite was dried in a vacuum oven at 30°C after separation by an external magnetic field (Khodadadi et al. 2019; Nasseh et al. 2018; Nasseh, Taghavi, et al. 2019).
2.2.2 Synthesis of Fe-Ni3/TiO2 nanocomposite
Here, 0.2 g of the synthesized FeNi3 magnetic nanoparticles was mixed in a mixture containing 10 ml of 1-propanol and 50 ml of deionized water. Then, 2 ml of titanium butoxide (TBOT) was added dropwise to the previous solution and added for 24 hours while the resulting mixture was stirred at 500 rpm at 80°C. Finally, the obtained FeNi3/TiO2 nanocomposite was rinsed with water and ethanol in several steps. This nanocomposite was dried in a vacuum oven at 30°C after separation by an external magnetic field. Once dried, the samples were placed in a 400 ° C oven for 4 hours for calcination (Lian et al. 2009).
2.2.3 Synthesis of N-doped Fe-Ni3/TiO2 catalyst
Initially, 140 mg of FeNi3/TiO2 was dispersed in 70 ml of deionized water for 20 minutes under ultrasonic waves. Then with 35% ammonia, the pH was adjusted to 10 and then 2 ml of hydrazine hydrate was added and stirred. Finally, it was heated in a Teflon autoclave at 80°C for 3 hours. Then, the reduced sheets of N_doped FeNi3/TiO2 were collected and the product was washed with deionized water and dried it in a vacuum oven at 50 ° C (Wang et al. 2012; Wang et al. 2013).
2.2.4 Investigation of Fe-Ni3/TiO2 nanocomposite properties
FESEM Images were used to determine the shape, mean diameter, and surface area of the synthesized nanoparticles. The magnetic properties of the nanoparticles were measured using a VSM vibrating sample magnetometer analysis. Also, X-ray spectra, FTIR, and BET were used to identify the composition and crystalline structure characteristics of RR 195 and nanoparticle size.
3.1 Adsorption of RR 195 by N-doped Fe-Ni3/TiO2 catalyst
A stock solution (1000 mg L− 1) of RR 195 dye was made in deionized water. The effect of different adsorption parameters of RR 195 by nanoparticles was investigated. Five pH ranges (Cai et al. 2021; Kim et al. 2013) were used including (3, 5, 7, 9, 11) for reactive red 195 dye, five initial concentration ranges for the desired contaminant (5-10-20-30-40 mg L− 1), nine ranges for contact time (5, 10, 15, 30, 60, 90, 120, 180, 200 minutes), and four ranges of nanocomposite (1-2-4 and6 g l− 1) with N42 magnet employed to separate the magnetic nanoparticles. RR 195 concentration was measured before and after the adsorption process using a spectrophotometer at a wavelength of 547 nm. In all stages of the experiments, the efficiency and adsorption capacity in the adsorption stage were calculated using the following equations.
To calculate the removal efficiency, Eq. 1 was used, where %R represents the removal efficiency, Ct denotes the residual concentration of reactive red 195 dye at time t (mg L− 1), and C0 is the initial concentration of dye (mg L− 1).
$$\text{%}R= {C}_{0-{C}_{t}}/{c}_{0}\times 100$$
1
Equation 2 was used to calculate the equilibrium adsorption capacity.
$$qe=V/M \times \left({C}_{1- }{C}_{T}\right)$$
2
C1 and Ct are the initial concentration and the residual concentration at time t in mg L− 1, qe represents equilibrium capacity in mg/g, V is the volume of the solution in lit, and M indicates the dose of the adsorbent in gram (Tang et al. 2017).
To determine the pHZPC or zero-point pH for N-doped FeNi3/Tio2 magnetic nanoparticles, 100 ml of deionized water was added to the Erlenmeyer flask. The pH of the deionized water was then adjusted within the range of 2–12 with hydrochloric acid and 0.1 N sodium hydroxide. Next, 0.1 g L− 1 of magnetic nanoparticles was added to each of the desired containers and placed on a shaker at a speed of 150 rpm. After 24 hours, the final pH of the solution was measured using a pH meter. The initial pH diagram was plotted against the final pH, and the point where the two RR 195 curves used each other indicated the isoelectric point (Khaniabadi et al. 2018; Panahi et al. 2019).
3.2 Adsorption isotherms, adsorption kinetics, and thermodynamics
The adsorption isotherms for RR 195 use the adsorption capacity of various adsorbents to evaluate the feasibility of a process and are also useful for analysis as well as design (Khaniabadi et al. 2017). In a system, the content of adsorbate per unit mass of adsorbent in RR 195 decreases with ease of concentration in RR 195. However, this relationship is not linear. Adsorption isotherms show the ratio between the concentration of the adsorbate unit and the compound concentration of the residual material in the solution. Adsorption isotherms can take many forms for different systems. In this study, two isotherm models known as Langmuir and Freundlich were evaluated. The Langmuir isotherm model describes the monolayer coating of the adsorbed compound on the adsorbent surface. Freundlich isotherm is based on monolayer and heterogeneous adsorption of adsorbate on adsorbent. Indeed, in the Freundlich model, it is assumed that the adsorption is monolayer and non-uniform. The following equation represents the Freundlich isotherm model. Eq. 3 was used to calculate the Freundlich isotherm.
(3)
In the Langmuir adsorption isotherm, adsorption is monolayer and the adsorption regions on the surface of the adsorbent are uniform, and all have the same adsorption power. Adsorption bonds are also reversible. The following equation represents the Langmuir isotherm model (Wanyonyi et al. 2014). Equation 4 was used to calculate the Langmuir isotherm.
$${c}_{e}/{q}_{e}= 1/{q}_{max}{k}_{l}+ {c}_{e}/{q}_{max}$$
4
4.1 Characteristics of synthesized N-doped Fe-Ni3/TiO2 nanocomposite
4.1.1 FTIR analysis
FTIR spectroscopy was used to determine the functional groups of N-doped FeNi3/Tio2 magnetic nanocomposite. Figure 1 displays the desired spectrum.
The presence of a peak at 494 cm− 1 is related to the tensile vibrations of Fe-Ni, Ni-Fe-Ni, and Fe-Ni-Ni. The presence of a peak at 1347.73 cm− 1 is related to C-H and N-O vibrations due to the residue of some raw materials such as hydrazine hydrate during manufacturing. The adsorption band at 3937.85 cm− 1 is associated with the vibrations of the hydroxyl functional group (O-H) in the sample due to the presence of moisture or water during adsorption. The FT-IR spectrum of Fe-Ni3/TiO2 indicates that TiO2 is well coated on the FeNi3 surface. The vibration peaks at 792 cm− 1 and 1102 cm− 1 have been assigned to the Ti-O-Ti bond. The broad peak appearing at 3819 cm− 1 is due to the tensile vibration of the O-H bond. On the other hand, the vibrations of 1626, 675, and 590 cm− 1 confirm the presence of shell on the surface of FeNi3 nanoparticles. Also, the FTIR spectrum of the first Fe-Ni3/TiO2 N-doped nanocomposite at 667 was assigned to the presence of oxidized nitrogen such as Ti-O-N. The compact and broad band at the low wave number range between 1078 and 964 cm− 1 was attributed to the strong tensile vibrations of the Ti -O and Ti -O-Ti bonds, indicating that the distance between the TiO2 band and N doping was reduced.
4.1.2 FESEM analysis
Scanning electron microscope (FESEM) was used to study the shape, surface, and average grain diameter, with Fig. 2 presenting the corresponding FESEM image. According to the figure, it can be found that N-doped FeNi3/Tio2 particles have aggregation properties which is due to their magnetic nature, causing the particles to adsorb each other well. Also, the closer it is taken from the surface to the material, the more its shape has not changed that. This is due to their amorphous state, because in different modes of the image, the shapes have not changed, so a regular structure is not recommended for it. The size of magnetic nanoparticles is within 33.5-67.31 nm and the texture of the material is dense in terms of compressibility, which indicates its high density.
4.1.3 VSM analysis
To determine the magnetic properties of the synthesized magnetic nanocomposite, a magnetic measuring device was used and the sample vibration (VSM) was measured at room temperature.
Figure 3 indicates that in the first step where the FeNi3 nanoparticle was synthesized, its magnetization was 5 emu g− 1. In the next stage of synthesis (FeNi3/TiO2), its magnetization increased to 7 emu g− 1. The synthesized adsorbent was dispersed and could be dispersed again. These particles had also good magnetization in the N-doped FeNi3/Tio2 phase, indicating the potential use of a magnetic adsorbate which can be easily separated using an external magnet.
4.1.4 BET analysis
BET analysis was employed to measure the specific surface area of FeNi3/TiO2 N-doped magnetic nanocomposite with its results presented in Table 1. Its effective surface area is 112.42 m2g− 1, considering that the specific surface area and total pore volume of N-doped FeNi3/TiO2nanoparticles are suitable therefore, it is expected to have good adsorption activity.
|
Nanoparticle |
Surface area (m2 g− 1) |
Average pore diameter (nm) |
Pore volume (cm3 g− 1) |
|---|---|---|---|
|
N-doped FeNi3/Tio2 |
112.48 |
7.7477 |
o.2186 |
4.2 Effect of different parameters on RR 195 adsorption on Fe-Ni3/TiO2 N-doped nanocomposite
4.2.1 Effect of pH
pH is an important factor in adsorption processes which can affect the surface load of the adsorbent. pHzpc of the synthesized nanocomposite was estimated before the adsorption test. The data show that the pzc pzc of N-doped Fe-Ni3/TiO2 nanocomposite was approximately 7.2. RR 195 is an anionic color, which is also used as an acid and alkaline marker (Munagapati & Kim 2017; Ojedokun & Bello 2017; Prasad et al. 2017). Figure 4 displays the effect of pH on the effectiveness and adsorption capacity of RR 195 using N-doped Fe-Ni3/TiO2 nanocomposite. As shown in the figure, in RR 195, which lowers the pH from 3 to 11, the removal efficiency has decreased. This is related to the adsorbent pHzpc, pKa, and the ionic structure of RR 195. pHzpc is a parameter used in adsorption studies and indicates the point at which the adsorbent surface charge is zero. If solution pH < pHzpc, the adsorbent surface charge is positive, if solution pH > pHzpc, the adsorbent surface charge is negative, and if pH = pHzpc, the adsorbent surface has no charge (positive and negative charges are equal) (Mohammadi & Aliakbarzadeh Karimi 2017; Taqui et al. 2017). Thus, with increasing pH, the electrostatic attraction force between the adsorbent and RR 195 diminishes and the adsorption efficiency in RR 195 decreases due to the anionic color property of RR 195. In the study, the highest removal percentage is related to pH of 3, where adsorbent surface charge is positive.
4.2.2 Effect of N-doped Fe-Ni3/TiO2 nanocomposite dose
As depicted in Fig. 5, regarding the effect of the concentration of N-doped Fe-Ni3/Tio2 nanocomposite (1–2-4-6 g L− 1) on the removal of RR 195, elevation of the concentration of adsorbent has enhanced the removal of RR. The efficiency increased due to the growth in the number of nanocomposites and the availability of more adsorption sites. An important factor in our studies is eliminating the effect of dose concentration at certain times. The results of this study can be consistent with studies conducted by Khani Abadi et al., which are related to the removal of RR 195 using activated carbon and montmorillonite (Wanyonyi et al. 2014).
4.2.3 Effect of concentration of RR 195
Figure 6 indicates the content of RR 195 adsorbed by the synthesized nanoparticles. This figure shows that as the initial concentration of RR 195 dye increases, its adsorption decreases due to the rise in the number of dye molecules to bind to the surface and thus the saturation of the adsorption sites on the adsorbent surface. On the other hand, the adsorption of RR 195 was rapid in the early stages and then slowed down as there are fewer binding sites on the adsorber surface to absorb the dye. Also, in a study conducted by Lambropoulou et al. on the removal of red reactive dye 195 by TiO2 nanoparticles, it was shown that the removal percentage increased at lower concentrations (Chládková et al. 2015).
4.2.4 Isotherm absorption and kinetics studies
The most important parameter in the adsorption method is the study of adsorption isotherms expressing the adsorbent capacity and adsorbent concentration. Table 2 reports the results for the isotherm parameters for the adsorption of the red reactive dye 195 by N-dopedFeNi3/Tio2. Based on the results, the adsorption isotherm follows the Langmuir model, which shows the graph of Ce versus Ce/qe. Since the value of R2 was 0.97 for the Langmuir model and 0.93 for the Freundlich model, the adsorption isotherm follows the Langmuir model. Figure 7 displays the study of the Langmuir isotherm model on the adsorption of reactive red 195 with N-doped FeNi3/Tio2 magnetic nanocomposite. Kuleyin et al.'s (2011) study on the adsorption isotherm of Remazol Brillant Bhue R and Remazol Yellow dyes by surfactant-modified natural zeolite showed that the obtained data are more consistent with the Langmuir isotherm model (Kuleyin & Aydin 2011).
|
Langmuir isotherm |
Freundlich isotherm |
||||
|---|---|---|---|---|---|
|
R2 |
qmax (mg g− 1) |
B (L mg− 1) |
R2 |
N |
Kf (mg g− 1) |
|
0.97 |
0.35 |
35.58 |
0.93 |
1.74 |
1.73 |
Table 3 lists the kinetic parameters of 195-N-dopedFeNi3/Tio2 reactive red dye adsorption. The pseudo-first-order kinetics model is obtained by plotting ln (qe-qt) versus t and quadratic kinetics in terms of t/qt versus t (Fig. 8). The first-order kinetic graph is used to obtain the coefficient R2 and the constant value K1, while the second-order kinetic graph is used to obtain k2 and qe which is obtained by calculating the slope of the curve and the intercept. In this study, considering that in pseudo-second-order kinetics, the value of R2 was equal to 0.99, so it follows the pseudo-second-order model. In a study by Raghunath et al. on the removal of textile dyes from industrial wastewater by the polymer nanocomposite of the amino acid proline, it was shown that isotherms obtained from different concentrations of adsorbent on dye adsorption kinetics followed a pseudo-second-order model .
|
pseudo-first-order kinetics |
pseudo-second-order kinetics |
|||||
|---|---|---|---|---|---|---|
|
R2 |
qe(mg g− 1) |
K1(min− 1) |
K2(min− 1) |
qe(mg g− 1) |
R2 |
|
|
0.507 |
2.8 |
0.047 |
0.026 |
17.95 |
0.999 |
|
Examination of the effect of pH revealed that the highest percentage of removal of reactive red 195 dye was observed at pH 3 (82%). In this study, it was found that elevation of the initial concentration of reactive red 195 dye reduced the efficiency in the adsorption process by N-doped FeNi3/TiO2. The results of the optimal dose of nanocomposite indicated that the efficiency was enhanced with increasing the dose in the adsorption stage, but then the efficiency dropped due to the turbidity caused by the nanocomposite dose. The results of the N-doped FeNi3/TiO2 reactive red dye adsorption process indicated that the adsorption isotherm was consistent with the Langmuir model and the adsorption process followed pseudo-second-order kinetics. Based on the results, the synthesized N-doped FeNi3/TiO2 magnetic nanocomposite has a high ability to remove the reactive red 195 dye and can be used as a suitable and available nanocomposite.
Data availability statement
The authors have no competing interests to declare that are relevant to the content of this article.
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.
Acknowledgments
The authors gratefully acknowledge the support of this work by Birjand university of Medical sciences.
Author contributions Statement
Sahebdadzehi and Dorri carried out the experiment. Sahebdadzehi wrote the manuscript with support from Khodadadi and Dorri. Sahebdadzehi fabricated the N-doped FeNi3/TiO2 magnetic nanocomposite and Khodadadi helped supervise the project. Dorri and Khodadadi conceived the original idea. Khodadadi supervised the project.
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- GraphicalAbstract.png
Graphical abstract of N-doped FeNi3/Tio2 magnetic nanocomposite
