Synthesis, Characterization and Catalytic Activity of Polyethylene Glycol (PEG) Functionalized MXene (Ti3C2Tx) for Methylene Blue Dye Degradation Under UV Light Irradiation

doi:10.21203/rs.3.rs-5192878/v1

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Synthesis, Characterization and Catalytic Activity of Polyethylene Glycol (PEG) Functionalized MXene (Ti₃C₂T_x) for Methylene Blue Dye Degradation Under UV Light Irradiation

https://doi.org/10.21203/rs.3.rs-5192878/v1

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The emerging field of two-dimensional (2D) transition metal carbides and nitrides, collectively known as MXene (Ti₃C₃Tx), has garnered significant attention in recent years due to their remarkable properties and multifaceted applications. This work explores the synthesis, characterization and functionalization of MXene with polyethylene glycol (PEG) and its influence on the degradation process of organic dye methylene blue (MB) is investigated. The functionalization of MXene with PEG is detailed, showcasing the diverse chemistries and functionalities these organic compounds bring to the MXene nanosheets. PEG imparts hydrophilicity and stability, and promotes catalytic activity. Further the mechanisms of dye degradation involving MXene-PEG materials are elucidated, highlighting the synergistic effects of MXene and functional groups on the enhanced degradation rates. This work underscores the versatility of MXene as a platform for environmental applications and the significant impact of functionalization with organic molecules on their performance. The findings of this work revealed that when MXene-based nanomaterials suitably functionalized with PEG, they exhibit immense potential in the reduction of methylene blue (MB) dye with a record breaking first order rate constant of 0.16581 ± 0.030 min^− 1.

Environmental Chemistry

2D material

Mxene

PEG

Organic dyes

Environmental remediation

MXene is a 2D metal nitrides, carbide and carbonitrides, that was discovered and initially reported in 2011 [1]. MXene structure can be expressed by M_n+1X_nT_x, where M is an early transition metal, X can be a nitrogen and/or carbon, T_x denoted as surface terminations, and n can have a value of 1–4 [2]. The usual layered structured MAX phases is made up of M_n+1X_n layers bonded together by atom layers [3]. While the M–A bond usually has a metallic character, the M–X bond displays a combination of covalent, ionic and metallic properties during the MAX phase [4]. Naguib et al. exploited the difference in reactivity between M-A and M-X bonds to produce exfoliated and loosely packed Ti₃C₂ 2D materials by meticulously etching the Al atom layer [1]. Owing to its unique morphology, MXene has a wide range of chemical properties. These properties allow MXene to be used in a variety of applications, such as environmental remediation, catalysts in the chemical industry, sensors, electrical device materials, electrochemical energy storage materials, and conductive reinforcement for polymers [5]. According to Ghidiu et al., a new high-yield, safer, simpler, and faster technique for MXene synthesis is provided by etching Al from Ti₃AlC₂ using ordinary hydrochloric acid (HCl) and lithium fluoride salts (LiF), in which etching and intercalation are accomplished in a single step [6]. In 2013, the isolation of single-layer MXene flakes revealed their two-dimensional character. Following, in 2014, Ti₃C₂T_x MXene was synthesized by employing an HF-assisted etching. Next, in 2016, the isolation of larger single Ti₃C₂T_x flakes was achieved by using the MILD method [7]. Many etchants have been employed, including aqueous hydrofluoric acid (HF) [7] [8], ammonium hydrogen bifluoride (NH₄HF₂) in H₂O [9–11], and a combination of lithium fluoride (LiF) and hydrochloric acid (HCl) [12–14]. Li⁺ ions spontaneously intercalate between MXene layers for the LiF/HCl etchant, increasing the interlayer space and decreasing the contact between MXene sheets. This finally causes the MXene sheets to delaminate during the washing step following etching [15].

The potential of MXene has been increased in a number of applications by surface functionalization techniques like as surface-initiated polymerization and single heteroatom doping, which have an impact on the material's optical, mechanical, electrical, magnetic, and hydrophilicity/hydrophobicity properties [16, 17]. Notwithstanding their many advantages, MXene has drawbacks such low mechanical flexibility, simple restacking, and weak stability [18, 19]. The kind and proportion of the T group affect these qualities, and surface functionalization and modification can improve their performance and stability [20]. The concentrations and the kinds of electrochemical active sites as well as electronic structures, are altered and improved by the surface modification achieved by manipulating the T groups of MXene [21]. Etching MXene with different etchants, such as LiF/HCl or HF, makes surface termination by the (-O) and (-F) groups easy to accomplish. Also, the surface termination can be adjusted by etching concentration, reaction time, temperature, natures of electrochemical active sites, and electronic structures [16].

Organic dyes have long been employed in a variety of sectors such as textile, leather and paper printing, leading to environmental pollution through the release in wastewater. Due to the poisonous, non-biodegradable and hazardous qualities of organic dyes, wastewater poses a significant environmental issue [22, 23]. Simple procedures, energy efficiency, strong chemical stability, affordability, and the absence of secondary pollutants make photodegradation a preferred technique. The molecular structure of the pollutant is photochemically broken-down during photo-degradation by light and active radicals generated by photocatalysts [24]. Radicals are created and the chemical structure of pollutants is destroyed when light strikes the photocatalysts, thus causing the excited electrons in the valance band to hop to the conductive band [25, 26]. Owing to the physicochemical characteristic such mixture structure, stability, hydrophilicity, and metallic conductivity, Ti₃C₂T_x is a viable option for wastewater treatment [27]. However, because of hydrophilic surface groups and van der Waals forces, MXenes have a tendency to agglomerate and restack in aqueous solutions. By offering steric stability, functionalizing MXene with PEG enhances its dispersibility in water. Because PEG is hydrophilic, it has a stronger connection with the dye molecules by preventing aggregation [28]. By enhancing their capacity to absorb light and produce more electrons and holes—two essential components for dye degradation reactions-functionalizing MXenes with PEG can improve their photocatalytic qualities [29].

In this work, MXene is synthesized by successfully etching MAX with LiF/HCl at room temperature. Furthermore, MXene is functionalized with PEG to achieve enhanced properties. Characterization was done with the help of UV-Visible absorption spectroscopy, ATR, X-ray Photoelectron Spectroscopy (XPS), Time-of-Flight Secondary Ionization Mass Spectrometry (ToF-SIMS), SEM, EDX. Later catalytic performance of both Ti₃C₂T_x and Ti₃C₂T_x-PEG were evaluated in the methylene blue (MB) dye degradation in water upon both with and without UV light irradiation. Notably, The MXene-PEG variant exhibited significant efficacy in the degradation of methylene blue dye under UV light irradiation with a record-breaking degradation rate constant.

Materials

The Ti₃AlC₂ powders available for purchase (90 µm in particle size) from Nanjing Xianfeng Nanomaterials Technology Co. Ltd. were selected as the raw material. Shanghai Alighting Biochemical Technology Co., Ltd. provided the methylene blue (MB), Polyethylene glycol (PEG) and lithium fluoride. Every reagent utilized in this study was analytically pure and didn't require any additional purification.

Synthesis of MXene (TiCT)

Ti₃C₂T_x was synthesized following the previous report with modification [30]. Shortly, 4g of LiF was added into 9M HCl and was continuously stirred for 30 minutes. Following, 2g of Ti₃AlC₂ was gradually added to mixture for 5 minutes, and mixture was let to stir for 24 hours. The reaction temperature was kept in the range of 25–35°C. MXene residue was washed several times with deionized water under centrifugation to remove any remaining residuals of LiF and HCl. The washing and the agitation of the precursor with water continued until the pH level of the wash water reaches a neutral value of 6; simultaneously, the color of the supernatant was continuously monitored. This step is important to remove any residuals of LiF and HCl, ensuring the safety and quality of the MXene product. As continuously washing, the supernatant gradually became clearer and changed to a lighter color. The change in color from dark to light or clear can be an indicator of the removal of etching byproducts and the progress of the washing process. The synthesis process is shown in Fig. S1.

Synthesis of MXene-PEG

2g of the Ti₃C₂T_x MXene precursor and 4 mL of PEG were added to a glass beaker. After a 30-minute ultrasonic treatment at room temperature, the mixture was then subjected to centrifugation to isolate the MXene-PEG composite.

Procedure for reduction of dye

The photocatalytic degradation activities of the synthesized MXene and MXene-PEG photocatalysts were tested by using a prepared methylene blue solution. A one mL of 5 mM sodium borohydride solution was mixed with 5 mL of 0.2 mM MB. To the solutions, sufficient quantities (0.1 g/L) of synthesized MXene and MXene-PEG were added individually. Then, the solution was left in the dark for one hour. Later, the experiment continued by irradiating the solution with a ultra violet light source (8 W halogen lamp) with continuous stirring. The photocatalytic reaction was maintained at room temperature. The results were analyzed by using a UV-Vis spectrophotometer and the degradation activity of methylene blue solution was studied using the following equation:

Degradation of Methylene Blue (%) = \(\:\left[\frac{Ab{s}_{0}-Ab{s}_{f}}{Ab{s}_{0}}\right]\times\:100\%\)

where Abs₀ and Abs_F are the initial and final absorbance of methylene blue solution, respectively, at a designated time [31].

The UV-vis spectra of the Ti₃C₂T_x and Ti₃C₂T_x-PEG show the structural difference induced by the PEG modification as shown in Fig. 1. The maximum absorbance was observed at 227 nm and 295 nm, respectively, for Ti₃C₂T_x and Ti₃C₂T_x-PEG, as can be observed from Fig. 1 (a). The shift in UV peaks indicates a change in the electronic transition due to interactions between Ti₃C₂T_x and PEG.

According to Iqbal et al, pristine MXene shows a good optical response for an incident light range of 200–800 nm [31], due to the black color of Ti₃C₂ with no clear absorption edge, indicating the metallic nature of Ti₃C₂ [32–34]. The pure MXene contains distinctive peaks of –OH stretching at ~ 3500 cm^− 1 and C = O stretching at ~ 1718 cm^− 1, as illustrated in Fig. 1(b), showing a typical chemical structure of MXene [35]. The ATR spectra of MXene-PEG show additional peaks at ~ 1412 cm^− 1 and ~ 1168 cm^− 1 after functionalization with PEG. These peaks are attributed to the PEG's –CH₂ and C-O-C bond [36]. Furthermore, the FTIR spectra of MXene-PEG indicate that hydrogen bonds have formed between MXene and PEG based on the redshifts of the -OH peaks [16].

The X-ray photoelectron spectroscopy is employed to analyze the elemental composition of the facial structure of both Ti₃C₂T_x and Ti₃C₂T_x-PEG. X-ray Photoelectron Spectroscopy (XPS) survey spectra of the pristine Ti₃C₂T_x MXene and the Ti₃C₂T_x-PEG structures are presented in Fig. 2a. For both the intrinsic and PEG-functionalized MXene, several primary peaks are observed at the binding energies of 684.5, 532.5, 465, and 300 eV, which are assigned to F 1s, O 1s, Ti 2p, and C 1s, respectively. The Ti 2p and C 1s spectra for the structure represent the presence of the Ti₃C₂T_x phase. Moreover, the sharp C 1s peak on MXene-PEG confirms the absorption of PEG. These observed peaks match prviously reported results [37]. This represents that materials include Ti₃C₂T_x and the Ti₃C₂T_x-PEG are terminated with –F and O/–OH. After etching with LiF/HCl, Ti atoms are linked to termination groups F, as shown in Fig. 2b. The loss of Al peaks from MXene confirms the successful etching. The Gaussian-Lorentzian curve of Ti 2p_1/2 and Ti 2p_3/2 peaks are shown at 464.8 and 458.2 in Fig. 2c respectively which is confirmed by the literature review [38]. The C–Ti–Ox peak is observed at 533 eV, as shown in Fig. 2d. Ti atoms are linked to O (Ti-O), which may be a consequence of surface oxidation. These indicate that the Ti₃C₂T_x MXene is functionalized with PEG on its surface. The shift of the Ti-O peak to the lower energy may be caused by oxygen vacancies. So, these confirm the etching of MXene and absorption of PEG in the MXene.

The functionalization of MXene with PEG is further confirmed by the Time-of-flight secondary ion mass spectroscopy (SIMS) shown in Fig. 3. Measurement was conducted in positive ion mode on 300 × 300 µm² area of MoS₂. The amplitude of the color scale resembles the maximum number of counts per pixel (MC) while TC is the total number of counts recorded for the specified m/z (it is the sum of the counts in all the pixels). Figure 3 (a) represents the elemental mapping image of Ti⁺ found in MXene with a total count of 4.197 × 10⁴ whereas after PEF functionalization this value decreases to 1.44 × 10⁴ displayed in Fig. 3 (b). The decrease of Ti⁺ total count signifies the surface coverage by PEG. Figure 3 (c) shows the absorption of PEG through the sharp peak of [M + H] ⁺ at the 415 m/z, confirming the absorption of PEG on the MXene surface.

The surface morphology is determined by Scanning electron microscopy. The image shown in Fig. 4 (a) shows the formation of a multilayer stack of Ti₃C₂Tx. The PEG is adsorbed in Ti₃C₂Tx and the interlayer distance is increased as shown in in the image displayed in Fig. 4 (b). EDX analysis was conducted to get quantitave elemental composition of MXene and MXene-PEG represented in Fig. 4 (c). After Ti₃C₂T_x is functionalized by PEG, the number of carbon increases; the weight percentage of C at Ti₃C₂T_x was found to be 6.77% and at Ti₃C₂T_x-PEG was found to be 9.34%. The weight percentage of oxygen also increases from 8.76–9.56% for Ti₃C₂T_x and Ti₃C₂T_x-PEG, respectively. The weight (%) of fluorine atom decreased after the synthesis of Ti₃C₂T_x-PEG to reaches 3.47% indicates the MXene surface coverage by the PEG.

The degradation of methylene blue was monitored by the UV-Vis spectrophotometry in a wavelength range of 400–800 nm at room temperature. Without UV illumination, the reduction of MB dye by NaBH₄ is depicted in Fig. 5(a). It is evident that there is no discernible change in absorption up to 40 minutes. In other words, nothing was reduced. The MB reduction utilizing NaBH₄ under UV light is shown in Fig. 5(b). After 40 minutes, there was a small decreasing trend in the absorption of MB dye. Following that, 0.1g/L of MXene was added to the combination of MB and NaBH₄, and Fig. 5(c) and Fig. 5(d) depict the catalytic action of MXene without UV light and with UV light irradiation, respectively. Using MXene as a catalyst, 95.8% of the MB dye could be reduced in 35 minutes. Reproduced data is displayed in Fig. S2.

Lastly, the reduction capability of the reaction mixture of MB and NaBH₄ was observed after adding 0.1g/L of MXene-PEG. Without exposure to UV light, Fig. 5(e) shows the time-dependent absorbance spectra of MB utilizing MXene-PEG as a reductant. In this instance, there was no such decrease. On the other hand, 100% reduction occurred under UV radiation in less than 20 minutes, as shown in Fig. 5(f). This data was reproduced which is displayed in Fig. S3. This amazing action of MXene-PEG may be explained by the UV light providing sufficient energy to excite the electron in the conduction band, which aided in the reduction process [39].

The MXene and MXene-PEG band gaps were calculated using the optical band gap equation (Optical Bandgap = 1240/λcut off) in order to explain this behavior. As seen in Fig. 6(a), the λ cutoff points for Ti₃C₂Tx and Ti₃C₂Tx-PEG are 250.5 nm and 360.2 nm, respectively. Ti₃C₂Tx and Ti₃C₂Tx-PEG have bandgaps of 4.95 eV and 3.44 eV, respectively. Binding energies were derived from the XPS data for Ti₃C₂Tx in Fig. 6(b) and Ti₃C₂Tx-PEG in Fig. 6(c) in order to define the HOMO and LUMO values. Ti₃C₂Tx and Ti₃C₂Tx-PEG were discovered to have binding energies of 1.78 and 0.9 eV, respectively. Moreover, it was discovered that the HOMO of MXene is 1.38 and that of MXene-PEG is 0.65 eV, whereas the LUMO values for Ti₃C₂Tx and Ti₃C₂Tx-PEG are 6.33 and 4.09 eV, respectively. The aforementioned computation demonstrated that Ti₃C₂Tx has a larger optical band gap than Ti₃C₂Tx –PEG. It took about 35 minutes to destroy the MB dye because there are less free electrons when the band gap widens for Ti₃C₂Tx. However, it took 20 minutes for the dye to decay in Ti₃C₂Tx-PEG. Free electrons are more readily available when the band gap is less, which aids in the degradation of dye.

A mechanism of MXene-PEG catalyst performance is depicted in Fig. 7. Higher energy photons that interact with the MXene-PEG photocatalyst cause the formation of an electron-hole pair. The electron that is generated quickly transfers to MXene, delaying the rate of recombination. The MXene is charged by this electron, and it combines with O₂ to form the superoxide anion O₂. Hydroxyl radical (-OH) is created when moisture that has previously lost electrons interacts with the positive holes in the valance band. The organic dye molecules then react with these superoxide anions and hydroxyl strong radicals to produce dye pollutants at the MXene-PEG surface that are both oxidizing and reducing, subsequently breaking down the dye molecules into mineralization products (H₂O, CO₂) [40]. MXene-PEG degraded methylene blue in under 20 minutes, compared to 35 minutes for MXene. Using PEG with MXene improves its capacity to break down the dye.

Considering the reduction of MB-NaBH₄-Mxene follows pseudo-first-order reaction kinetics, as seen by the linear connection between ln(A/A₀) and the reduction time in minutes displayed in Fig. 8 (a). Based on the graph’s slope, the rate constant is determined to be 0.08375 ± 0.005 min^-1. Assuming the reduction for MB-NaBH₄-MXene-PEG exhibits pseudo-first-order reaction kinetics, as seen by the linear correlation between ln(A/A₀) and reduction time in minutes displayed in Fig. 8 (b). This graph's slope is used to determine the rate constant, which comes out to be 0.16581 ± 0.030 min^-1.

A comparative study of the degradation efficiency of Methylene blue dye with previously reported literatures is given in Table 1. MXene-PEG showed the best performance among the reported works with a record breaking first order rate constant of 0.16581 ± 0.030 min^-1.

Table 1

Comparative study of the degradation efficiency of Methylene blue dyes with previously reported literature
Catalyst	Efficiency (%)	Dye	Time (min)	References
BFO/MXene	100	CR	42	[40]
BiVO₄/MXene	99.1	MO	130	[41]
TiO₂/MXene	96.44	MB	60	[42]
AgNPs/TiO₂/Ti₃C₂T_x	99	MB	30	[43]
Ti₃C₂T_x	100	MB	180	[44]
Ti₃C₂T_x	99.32	MB	30	[45]
NiMnO₃ / NiMn₂O₄-Ti₃C₂Tx MXene	100	MB	50	[46]
Ti₃C₂T_x-PEG	100	MB	20	This work

Due to its outstanding features and wide range of applications, the field of two-dimensional (2D) transition metal carbides and nitrides, or MXene, has gained a lot of attention recently. The functionalization of MXene with polyethylene glycol (PEG) and its impact on the organic dye methylene blue's (MB) breakdown process are examined in this work. In-depth information about the functionalization of MXene with PEG is provided, highlighting the variety of chemistries and features these organic compounds impart to the MXene nanosheets. PEG increases catalytic activity and imparts hydrophilicity and stability. The mechanisms of dye degradation pertaining to MXene-PEG materials are further clarified, emphasizing the mutually beneficial impacts of MXene and functional groups on the elevated rates of degradation. The adaptability of MXene as a platform for environmental applications and the notable influence of functionalization with organic molecules on its performance are highlighted by this work.

CRediT authorship contribution statement

Maisha Rahman: Conceptualization, data curation, formal analysis, writing original draft; Muhammad Shamim Al Mamun: Conceptualization, formal analysis, methodology, supervision, writing and reviewing original draft. Tsuyoshi Takaoka: Data curation;writing and reviewing original draft; Tadahiro Komeda:Data curation, writing and reviewing original draft; Mohamed Aly Saad Aly: Conceptualization, writing and reviewing original draft; Md Nasiruddin: Writing and reviewing original draft;Waleed Alahmad: Writing and reviewing original draft.

Competing Interest

There are no conflicts to declare.

Acknowledgements

Authors love to acknowledge Chemistry Discipline, Khulna University for the facilities and lab support to pursue this research.

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The authors declare no competing interests.

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Synthesis, Characterization and Catalytic Activity of Polyethylene Glycol (PEG) Functionalized MXene (Ti₃C₂T_x) for Methylene Blue Dye Degradation Under UV Light Irradiation

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Introduction

Experimental Section

Materials

Synthesis of MXene (TiCT)

Procedure for reduction of dye

Results and Discussion

Conclusion

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References

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Supplementary Files

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