Effect of Synthesized ZnWO 3 /MIL-101(Cr) Nanocomposite on Lactoferrin Adsorption for Wastewater Treatment

doi:10.21203/rs.3.rs-5296064/v1

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Effect of Synthesized ZnWO 3 /MIL-101(Cr) Nanocomposite on Lactoferrin Adsorption for Wastewater Treatment

https://doi.org/10.21203/rs.3.rs-5296064/v1

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In this research, we increase the efficiency of the ZnWO₃ catalyst by using the MIL-101(Cr) catalyst. By coupling these two catalysts, we can use them to achieve faster adsorption of lactoferrin in wastewater treatment. Regarding the adsorption of lactoferrin in wastewater, using nanocomposite can significantly improve the absorption of lactoferrin. Oxidizing lactoferrin can help reduce organic pollutants in wastewater and improve water quality. This nanocomposite can increase the speed of chemical reactions, which leads to higher efficiency in adsorbing lactoferrin and other organic pollutants. Also, these photocatalysts can improve the recyclability and reusability of ZnWO₃/MIL-101(Cr), help reduce the costs of treatment operations, and remove other pollutants in wastewater. On the other hand, using this type of nanocomposite may reduce environmental damage and help preserve natural resources. ZnWO₃/MIL-101(Cr) nanocomposite was identified using FT-IR, XRD, UV-vis, and SEM analyses.

Catalyst

Environmental

Lactoferrin

nanocomposite

Pollutants

ZnWO3

One of the most well-known catalysts is titanium dioxide (TiO₂), widely used in various applications due to its catalytic properties. Some typical applications of catalysts include environmental remediation, self-cleaning surfaces, air purification, hydrogen production, and catalytic synthesis. Overall, the unique properties of catalysts make them versatile tools for a wide range of applications, particularly in environmental protection, energy production, and chemical synthesis [1].

Heterojunction photocatalysts are constructed by coupling two semiconductor catalysts to create a junction interface. This nanocomposite structure can enhance the catalytic performance of the individual components by promoting charge separation, improving light adsorption, and facilitating interfacial reactions. TiO₂, SiO₂, ZnO, CeO_2, and g-C₃N₄ are all photocatalysts reported for water-purifying pollutants [2]. Semiconductor oxides such as magnetite (Fe₃O₄), tin oxide (SnO₂), silver phosphate (Ag₃PO₄), zinc oxide (ZnO), tungsten oxide (WO₃), titanium oxide (TiO₂), cerium oxide (CiO₂), bismuth tungstate (Bi₂WO₆) and graphene oxide (GO) are widely used as photocatalysts. Combining two semiconductor catalysts with different band structures in a heterojunction configuration offers several advantages: enhanced charge separation, expanded light absorption range, facilitated interfacial reactions, and synergistic effects [3].

Advancements in adsorption technology have revolutionized the field of separations and environmental remediation. The ability of adsorption to achieve challenging or impractical separations with traditional methods like distillation, adsorption, or membrane-based systems has opened up new possibilities for addressing complex water treatment and purification challenges. The rapidly expanding adsorption applications are driven by the increasing environmental and quality standards that industries and municipalities must meet [4]. The need for efficient removal of pollutants, contaminants, and impurities from water sources has propelled the development and adoption of innovative adsorbent materials and technologies. The availability of a wide range of off-the-shelf adsorbents with satisfactory performance has facilitated the implementation of adsorption processes in various applications [5]. These commercially available adsorbents can effectively address many water treatment requirements and help industries comply with regulatory standards.

However, the continuous research and development efforts in adsorbent technology are focused on creating new materials with superior properties and enhanced performance [6]. The synthesis of novel adsorbents with improved characteristics can lead to more efficient and cost-effective solutions for specific applications [7]. Despite the ongoing advancements in adsorbent technology, the time and resources required to develop and optimize a new adsorbent for a particular urgent application can be significant. Therefore, researchers and practitioners need to balance the need for rapid solutions with the pursuit of long-term innovations in adsorption technology to address evolving water treatment challenges effectively [8]. Integrating adsorption and catalysis processes in wastewater treatment offers several benefits and advantages over using each technique individually. By combining these two processes, the hybrid system can leverage the strengths of both methods while mitigating their respective limitations [9].

One common approach is to incorporate noble metal cocatalysts, such as platinum or gold, onto the surface of MIL-101. These cocatalysts can act as electron sinks, promoting charge separation and reducing the recombination of electron-hole pairs, leading to enhanced catalytic activity. Another strategy is incorporating non-metal cocatalysts, such as carbon-based materials like graphene or carbon nanotubes, onto MIL-101 [10]. MIL-101 has a very high surface area, which provides more active sites for photocatalytic reactions, enhancing the efficiency of the process. Its porous nature allows for better diffusion of reactants and products, improving reaction rates and overall photocatalytic performance. Also, MIL-101 exhibits good thermal and chemical stability, crucial for maintaining photocatalytic activity over time and under various reaction conditions. It can absorb light effectively, particularly in the UV-visible range, making it suitable for various photocatalytic applications. [11]. MIL-101 can be combined with other materials to create composite photocatalysts, further enhancing its performance through synergistic effects. Many studies have shown that MIL-101 can be reused multiple times without significant loss in activity, making it cost-effective for industrial applications. [12]. Although MIL-101 can absorb light in the UV-visible range, its absorption spectrum may not extend into the near-infrared region, which limits its effectiveness under sunlight.

The text highlights the importance of enhancing the catalytic efficiency of zinc oxide (ZnO) by modifying its band gap to enable the adsorption of a broader range of electromagnetic radiation, particularly in the visible region. The high recombination rate of photogenerated electron-hole pairs in ZnO limits its catalytic efficacy, prompting the exploration of doping transition metals or incorporating elements like C, N, and S to inhibit recombination and improve performance [13]. Additionally, tungsten trioxide (WO₃) is discussed as a visible-light responsive catalyst with a smaller band gap than ZnO, making it suitable for various optoelectronic applications. The potential of combining WO₃ with ZnO for enhanced catalytic degradation of organic pollutants is also suggested [14]. Overall, the text underscores the importance of nanocomposites and tailored modifications to optimize the catalytic properties of semiconductor materials like ZnO and WO₃ for diverse applications in environmental remediation and energy conversion [15]. ZnWO₃ can be an electron acceptor, facilitating the separation of photogenerated charge carriers (electrons and holes) from MIL-101. This reduces recombination rates and increases the availability of active species for photocatalytic reactions. While MIL-101 primarily absorbs in the UV-visible range, ZnWO₃ can extend light absorption into the visible range. This combination can enhance overall photocatalytic activity under natural sunlight. The porous nature of MIL-101 can facilitate the diffusion of reactants to the active sites on ZnWO₃, improving reaction kinetics. The coupling may enable a Z-scheme mechanism where electrons from ZnWO₃ are transferred to MIL-101, allowing both materials to effectively utilize their respective energy levels. Also, the combination can enhance the generation of reactive oxygen species, which is crucial for many photocatalytic reactions, including the degradation of pollutants.

Lactoferrin (Lf) is an iron-binding protein closely related in structure to the iron transport protein transferrin [16]. Unlike transferrin, only traces are usually present in serum. Instead, it is found mainly in milk and other external secretions and in the secondary granules of neutrophils. Although Lf was first isolated 30 years ago, its biological role remains unclear. Recent X-ray crystallographic studies have advanced knowledge of the structure of Lf, and the structure and iron-binding properties of Lf are reviewed in detail elsewhere [17]. Briefly, Lf, like transferrin, reversibly binds two ferric ions, for which synergistic binding of an anion, usually bicarbonate or carbonate, is necessary [18].

However, its affinity constant for iron is 300 times greater than that of transferrin, and even in the presence of a competing iron chelator such as citrate, it can retain iron down to pH three or less. In contrast, transferrin loses it at pH 5. Unlike transferrin, Lf is strongly basic [19]. Human Lf has been cloned and sequenced, and the recombinant protein is expressed in baby hamster kidney cells. This study uses the synthesized ZnWO3/MIL-101(Cr) nanocomposite to adsorb Lf [20].

2.1. Materials and Methods

Sodium hydroxide (NaOH,100%), zinc acetate (ZnC₄H₆O₄,98%), sodium tungstate dihydrate (Na₂WO₄.2H₂O,99%), Cr (NO₃)₃.9H₂O(99%), terephthalic acid (C₆H₄(CO₂H)₂,98%), glacial acetic acid(99.5–100%), were bought from Sigma-Aldrich. As a pure protein, Lf was purchased from Merck (Germany). Other chemical compounds were prepared from local resources.

2.2. Synthesis of Zinc tungstate trioxide (ZnWO₃)

To synthesize ZnWO₃, 30 ml of NaOH (4 M) was added dropwise to the mixture of 20 ml of zinc acetate (1 M) and 2 ml of Na₂WO₄.2H₂O (0.5 M). The suspension was stirred for 3 hours at room temperature on a stirrer until the desired mixture was produced. Then, it was transferred to a glass conical flask with a volume of 250 ml and stirred for 10 hours at a temperature of 95°C. Then, the sediment was washed entirely with water and dried under ambient air conditions. In the next step, the characterization of ZnWO₃ was carried out by using different analyses such as FTIR, XRD, and SEM.

Synthesis of (MIL-101/ZnWO ₃ (Cr))

A mixture of 4.0 g Cr (NO₃)₃.9H₂O, 1.66 g terephthalic acid, 50 mL deionized water, and 0.58 mL glacial acetic acid, meanwhile 0.2 g presynthesized ZnWO₃ was placed in a 75 mL stainless steel autoclave. It was charged with a Teflon cover and placed in an oven at 220°C for 72 hours. Then, the autoclave was allowed to cool to room temperature, filtered, washed with distilled water, and dried in an oven at 80°C overnight.

3.1 Characterization and physicochemical properties of (ZnWO₃/MIL-101(Cr))

SEM

SEM (scanning electron microscopy) analysis is a powerful technique to characterize materials' surface morphology and microstructure at a high resolution. When applied to synthesized catalysts, SEM analysis can provide valuable information about particle size, shape, and distribution within the catalyst material [21]. For SEM analysis, the synthesized ZnWO3/Mil101 catalyst is first coated on a layer of conductive substrate such as gold. This coating helps prevent charging effects and improve the image quality. The sample is placed in the SEM chamber, where a focused beam of electrons is scanned across the material's surface. As the electrons interact with the sample, they generate signals such as secondary electrons, backscattered electrons, and X-rays. These signals are detected by the SEM instrument and used to create an image of the sample's surface.

The SEM images are shown in Fig. 1. It reveals important details about the morphology of the synthesized nanocomposite, such as the size and shape of individual particles, the presence of agglomerates or clusters, and the distribution of particles within the material. This information can help us understand how the catalyst's structure influences its catalytic activity and performance. As can be seen, the cohesion of the particles is very suitable, leading to better adsorption of the protein particles into the catalyst. Due to the viscosity of Lf nanoparticles [22], catalyst particles' surface continuity and adhesion cause better coupling, increased retention time, and better adsorption. Figure 1-a shows the synthesized nanocomposite's surface properties around 200 nm. Figure 1-b leads to the morphology of synthesized ZnWO₃/Mil101, which can explain the physical characteristics of catalysts well.

FT-IR

Figure 2 shows the FT-IR spectra of the ZnWO₃. In the ZnWO₃, the specified bands in 578 cm^-1 and 673 are related to the stretching bands Zn-O and W-O. The band at 2329 cm^− 1 is due to air CO₂ vibration. The 1625 and 1404 cm-1 bands correspond to the O-C-O symmetric stretching vibration of water adsorbed on MIL-101 (Cr), respectively. Other bands between 600 and 1600 cm^-1 confirm the presence of the benzene ring, which includes C = C stretching vibration at 1508 cm^-1 and C-H deformation vibrations at 750, 884, 1018, and 1160 cm^-1, respectively. In this spectrum, the peak observed at 674 cm^-1 is associated with the vibration of CrO. The peaks related to the stretching vibrations of oxygen with metals are usually observed in 400 to 800 cm^-1(9).

XRD

Figure 3 shows the XRD pattern of the synthesized ZnWO₃/MIL-101(Cr) nanocomposite. In monoclinic tungsten trioxide, the diffraction peaks are apparent at 23.1° and 23.7° relative to (002) and (020) crystal planes. Low-intensity peaks at 31.6, 34.4, 36.3, 47.6, 67.8, and 69.1 degrees are, respectively, due to the Miller indices (100), (002), (101), (102), (112), and (201), which are corresponded to ZnO. The main peaks at 2θ values are equal to 0.927°, 1.558°, 2.661°, 3.112°, 3.804° and 4.673°. The synthesized MIL101 (Cr) has a very high crystallinity with strong peaks at small 2θ angles. It proves that there are many pores in the synthesized MIL101(Cr) structure.

UV-vis

Figure 4 presents a UV analysis of synthesized ZnWO₃/MIL-101(Cr) nanocomposite. For Cr-MIL, adsorption close to 360 nm and another absorption in the 450 to 700 nm range were observed, and they are related to the d-d transition band of Cr³⁺ ions. Also, WO₃ gives absorption in the region of 375 nm. The band at 369 nm shows a sharp band corresponding to the formation of ZnO particles. Due to the adsorption of these two compounds, the nanocomposite has been successfully formed.

Bed Expansion Properties

In general, the wet density plays a significant role in the expansion characteristics of the substrate. Therefore, determining the substrate's physical characteristics is one of this article's goals. Catalyst samples in different conditions, including water, glycerol, ethanol, and an environment free of solution, were taken to analyze bed expansion better. The wet density of the composite was estimated to be about 5 g/ml, which is slightly increased compared to the synthesized ZnWO₃/MIL-101(Cr) nanocomposite (5.4 g/ml). Perhaps this increase in density is due to the presence of MIL-101 on the layer. One of the essential factors for having a suitable environment for separating hydrophobic protein products is a high amount of water. In this regard, the porosity of the adsorbent is also reported to be about 88%. However, higher performance is expected due to the increased density and good coupling of MIL-101. Therefore, it can be concluded that the synthesized ZnWO₃/MIL-101(Cr) nanocomposite can potentially adsorb lactoferrin for wastewater treatment and can be used at high flow rates. In addition, substrate expansion is one of the critical factors in adsorption efficiency. The bed expansion coefficient decreases with increasing density. The characteristics of bed expansion and its relationship with particle velocity are shown in Fig. 5.

Figure 6 shows the effect of nanocomposite according to pH on lactoferrin protein absorption in wastewater treatment. These studies have shown that solution pH and catalyst activity can significantly affect lactoferrin protein adsorption efficiency. For example, increasing the pH of the solution can lead to a decrease in protein adsorption because this increase may lead to a change in the protein's electrical charge and the catalyst's activity. On the other hand, the use of heterogeneous catalysts can significantly improve the efficiency of lactoferrin protein adsorption. This is due to the increased number of active sites and surface energy to interact with proteins. Figure 6 shows the pH values as a function of the adsorption rate. Maximum absorption (60 mg/ml) was observed at pH 2.0. It may be because of the new composite.

Based on the information, the ZnWO₃ catalyst exhibited higher activity in adsorbing albumin from sewage effluent than the Mil101 (Cr) catalyst. Figure 7 presents the adsorption efficiency versus time. However, when a nanocomposite of ZnWO₃/MIL-101(Cr)was used with the same optimal amount of 0.006 g, it showed even higher activity in adsorbing albumin from wastewater effluent. This suggests that combining ZnWO₃ and Mil101(cr) in a nanocomposite form resulted in synergistic effects that enhanced the adsorption capacity for albumin in wastewater effluent. The nanocomposite likely provided a more efficient and effective adsorption process due to the combined properties of both catalysts. Overall, the results indicate that the ZnWO₃/MIL-101(Cr)nanocomposite may be a promising material for albumin adsorption from sewage effluent, offering improved performance compared to using either catalyst alone. Further research and optimization of this nanocomposite could enhance wastewater treatment processes.

Based on the observation that the ZnWO₃/MIL-101(Cr) nanocomposite maintained high and promising activity in adsorbing Lf from sewage effluent even after five cycles of reuse, it can be concluded that the structure and activity of the catalyst remained relatively constant and stable throughout the experiment. The consistent performance of the catalyst over multiple cycles suggests that it possesses good stability and durability under the experimental conditions. This stability is crucial for practical applications in wastewater treatment, as it ensures the continued effectiveness of the catalyst over an extended period of use. Figure 8 describes catalyst recycling versus efficiency. As can be seen, when the amount of recycling increases, the efficiency goes down. In the first stage, the efficiency is close to 96%, whereas the efficiency value is near 88% at five times recycling.

TiO₂ is one of the most essential components, and it is of paramount importance as an active catalyst due to its stability, cost-effectiveness, and efficiency. Heterojunction catalysts are fabricated by coupling two semiconductor catalysts to create a junction interface. Integrating adsorption and catalysis processes in wastewater treatment offers several gains over using each method individually. MIL-101 was used as a cocatalyst that can act as an electron sink, promoting charge separation and reducing the recombination of electron-hole pairs, leading to enhanced catalytic activity. The results showed that it is possible to increase the catalytic efficiency of zinc oxide by changing its band gap to enable the adsorption of a broader range of electromagnetic radiation, especially in the visible region. An SEM image of the synthesized catalyst at around 200 nm reveals that the cohesion of the particles is very suitable, leading to better adsorption of the Lf nanoparticles into the catalyst. FT-IR analysis shows that the catalyst matches the original sample well. This means that the different bands of the graph agree with interpreting and confirming the scientific data. The XRD pattern of the synthesized ZnWO3/MIL-101(Cr)nanocomposite is very close to that of a pure one, and the peaks in the two theta angles explain the properties and characteristics of the component. The UV analysis of the synthesized ZnWO3/MIL-101(Cr) nanocomposite presents the adsorption of these two compounds, and the nanocomposite has been successfully formed and shaped well.

Bed expansion behavior shows the physical conditions of the catalyst. As we know, water is vital in separating hydrophobic protein products, and the porosity of the adsorbent is also reported to be close to 88%. However, higher performance is expected due to the increased density and good coupling of MIL-101. The catalyst samples were measured in different bed expansion conditions, including water, glycerol, and ethanol. In a solution-free environment, the results showed that the catalysts synthesized in solution-free conditions have better adsorption efficiency. Catalysts are resistant to pH and have better adsorption in acidic conditions. Considering that Lf is alkaline and its isoelectric point is around 9, the environment's acidity causes better adsorption and separation of the protein layer from the wastewater solution. The effects of time on efficiency show that the efficiency will rise with increasing time. From the recycling analysis, it can be concluded that the structure and activity of the catalyst remained relatively constant and stable throughout the experiment. Finally, the results indicate that the ZnWO₃/MIL-101(Cr) nanocomposite catalyst is a reliable and robust material for adsorbing Lf from sewage effluent, with its activity remaining high and consistent even after repeated use. This finding further supports the potential of this catalyst for efficient and sustainable wastewater treatment processes.

Ethical Approval:

Not applicable.

Consent to participate:

Not applicable.

Consent for publishing

All authors have given their final approval for the publication of this manuscript.

Competing Interest:

The authors declare that they have no conflict of interest.

Funding:

No funding has been given to support this work.

Author Contribution

Roozbeh Mofidian: Conceptualization, investigation, methodology, data curation, formal analysis and writing. Behnaz Abdi: Methodology. Hosna Malmir: Investigation and supervision.

Acknowledgement:

Not applicable.

Data Availability:

Not applicable.

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No competing interests reported.

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Effect of Synthesized ZnWO 3 /MIL-101(Cr) Nanocomposite on Lactoferrin Adsorption for Wastewater Treatment

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Version 1

Abstract

Figures

1. Introduction

2. Experimental

2.1. Materials and Methods

2.2. Synthesis of Zinc tungstate trioxide (ZnWO₃)

3. Results and Discussion

3.1 Characterization and physicochemical properties of (ZnWO₃/MIL-101(Cr))

Conclusion

Declarations

Competing Interest:

Funding:

Author Contribution

Acknowledgement:

Data Availability:

References

Additional Declarations

Status:

Version 1

Effect of Synthesized ZnWO 3 /MIL-101(Cr) Nanocomposite on Lactoferrin Adsorption for Wastewater Treatment

Status:

Version 1

Abstract

Figures

1. Introduction

2. Experimental

2.1. Materials and Methods

2.2. Synthesis of Zinc tungstate trioxide (ZnWO3)

3. Results and Discussion

3.1 Characterization and physicochemical properties of (ZnWO3/MIL-101(Cr))

Conclusion

Declarations

Competing Interest:

Funding:

Author Contribution

Acknowledgement:

Data Availability:

References

Additional Declarations

Status:

Version 1

2.2. Synthesis of Zinc tungstate trioxide (ZnWO₃)

3.1 Characterization and physicochemical properties of (ZnWO₃/MIL-101(Cr))