Visible light-triggered catalytic conversion of D-glucose to sorbitol using magnesium oxide/graphitic carbon nitride nanocomposites

Salhah Hamed Alrefaee

doi:10.25259/JKSUS_458_2024

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Research Article

2025

:37;

4582024

doi:

10.25259/JKSUS_458_2024

Visible light-triggered catalytic conversion of D-glucose to sorbitol using magnesium oxide/graphitic carbon nitride nanocomposites

Salhah Hamed Alrefaee^a,*

aDepartment of Chemistry, Taibah University, College of Science, Yanbu, 30799, Madinah Saudi Arabia

*Corresponding author E-mail address: srefaee2000@gmail.com and srfaay@taibahu.edu.sa (S Alrefaee)

Received: 2024-12-08, Accepted: 2025-09-10, Published: 2025-10-18

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This is an open-access article distributed under the terms of the Creative Commons Attribution-Non Commercial-Share Alike 4.0 License, which allows others to remix, transform, and build upon the work non-commercially, as long as the author is credited and the new creations are licensed under the identical terms.

Abstract

The polymeric graphitic carbon nitride (g-C₃N₄) was modified by attaching magnesium oxide nanoparticles (MgO NPs) to improve charge separation efficiency. The resultant photo-responsive MgO/g-C₃N₄ nanocomposites (NCs) exhibited significantly greater catalytic activity for hydrogen generation compared to both g-C₃N₄ nanosheets and MgO NPs, producing hydrogen at rates that were 2.13 times and 8.12 times faster, respectively. Additionally, the ability of MgO/g-C₃N₄ NCs to catalyze the degradation of methylene blue (MB) dye was evaluated. A novel catalytic hydrogen transfer (CHT) method was developed to convert D-glucose to D-sorbitol using the MgO/g-C₃N₄ photonanocatalyst in a 1:1 mixture of aqueous ethanol and water at room temperature, under visible light irradiation, and atmospheric pressure, without the need for additional molecular hydrogen. After 4 h of irradiation, using 100 ppm of the catalyst and 10% NaHSO₃ as a hydrogen donor (NaHSO₃:catalyst, 1:10, w/w), a highly selective conversion rate of 93% of glucose to sorbitol was achieved. Catalyst recycling studies demonstrated sustained activity after five cycles. This methodology not only outperforms previously studied techniques but also offers a green and efficient approach to sorbitol production under mild conditions.

Keywords

Catalytic hydrogen transfer (CHT)

D-sorbitol; Photocatalysis

Graphitic carbon nitride (g-C3N4)

Magnesium oxide (MgO)

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1. Introduction

Research for developing effective and sustainable catalysts for a range of uses, such as chemical synthesis, energy conversion, and environmental remediation, has exponentially increased in recent years. Nanocomposites (NCs), which combine the properties of two or more materials at the nanoscale, have emerged as promising candidates for these applications (Mohamed 2022; Huang et al. 2024). Due to their unique properties and synergistic effects, MgO nanoparticles (NPs) and g-C₃N₄ have garnered significant interest (Taha et al. 2024a). Researchers have recently shown considerable interest in polymeric g-C₃N₄ due to its exceptional thermal and chemical stability, as well as its optimal bandgap of 2.7 eV. Owing to these characteristics, g-C₃N₄ is extremely useful in photocatalytic processes like the production of hydrogen via water splitting and the breakdown of organic dyes when exposed to visible light.

Its ability to absorb visible light and facilitate these reactions positions g-C₃N₄ as a promising candidate for sustainable energy solutions and environmental remediation (Attia et al. 2024). Moreover, g-C₃N₄ is highly attractive from a practical standpoint. It is cost-effective, environmentally friendly, and can be synthesized using readily available precursors like cyanamide, dicyandiamide, urea, and melamine. This ease of synthesis not only reduces production costs but also supports its application in various fields, from renewable energy to wastewater treatment (Zhang et al. 2019). Despite these advantages, g-C₃N₄ faces critical limitations that hinder its practical applications. One of the main challenges is the high recombination rate of photoexcited charge carriers, which significantly reduces its photocatalytic efficiency. This issue leads to a low rate of hydrogen production and limits the material’s effectiveness in degrading organic pollutants (Taha et al. 2024b: Wang et al. 2012; Wang et al. 2009). To address these challenges, scientists have explored various modification techniques aimed at enhancing the photocatalytic activity of g-C₃N₄.

Modifying the morphology of g-C₃N₄ to increase surface area and improve light absorption can enhance its catalytic activity (Wang et al. 2010; Zhang et al. 2010). Introducing non-metal (such as sulfur or phosphorus) and metal (such as iron or cobalt) heteroatoms can alter the electronic structure of g-C₃N₄, leading to improved charge separation and reduced recombination rates (Liu et al. 2010; Ge et al. 2011). Combining g-C₃N₄ with other semiconductor materials can create heterojunctions that facilitate charge transfer and enhance overall photocatalytic efficiency (Yan et al. 2010; Liu et al. 2018; Di et al. 2013). These modification approaches have shown promise in overcoming the inherent limitations of g-C₃N₄, making it a more viable option for practical applications. Continued research in this area will be essential for unlocking the full potential of g-C₃N₄ in sustainable energy and environmental technologies.

Because of their special qualities, MgO NPs have a variety of uses. According to Smith and Doe (2023) and Gatou et al. (2024), these NPs have a large surface area, good thermal stability, and robust fundamental characteristics. MgO NPs are perfect for catalysis and adsorption applications because of their enormous surface area, which offers a multitude of active sites for chemical reactions. Because of their exceptional thermal stability, magnesium oxide NPs can tolerate elevated temperatures without suffering appreciable deterioration. The basic nature of MgO NPs makes them useful for acid neutralization and as catalysts in various chemical reactions. MgO NPs are considered biocompatible and non-toxic, making them suitable for biomedical applications (Navarro et al. 2022; Ahmad et al. 2023). MgO NPs can function as both acid and base catalysts, making them versatile for a variety of reactions. They can be used as supports for metal catalysts, enhancing their catalytic activity and stability. MgO NPs can be used to remove heavy metals and organic pollutants from water. They can be employed to capture harmful gases, such as sulfur dioxide and nitrogen oxides. MgO NPs can be used as carriers for drug delivery, targeting specific cells or tissues. They exhibit antimicrobial properties, making them useful for wound healing and infection control. For imaging procedures such as magnetic resonance imaging (MRI), MgO NPs can be employed as contrast agents. MgO NPs can be used to treat ceramic materials to enhance their mechanical characteristics and thermal stability, added to battery electrodes to enhance their functionality, and function as catalysts for fuel cell processes (Zhang et al. 2013; Hakimioun et al. 2023; Saberi et al. 2024).

MgO/g-C₃N₄ NCs are a potential relative of materials with a wide range of uses, especially in photocatalysis. These NCs combine the special qualities of g-C₃N₄ and MgO to provide better catalytic activity, effective charge separation, and increased light absorption. MgO and g-C₃N₄ produce a heterojunction that promotes effective charge separation, minimizes recombination losses, and improves charge carrier duration. The strong interaction between MgO and g-C₃N₄ can promote efficient charge transfer, facilitating the reduction of protons to hydrogen gas. The combination of MgO and g-C₃N₄ can enhance the photocorrosion resistance of the composite, leading to longer-term stability (Pham et al. 2022; Dahiya et al. 2024; Mao and Jiang 2019). The conversion of glucose to sorbitol is a crucial industrial procedure, especially in the food and pharmaceutical industries. This process has historically depended on heterogeneous catalysts, like Raney nickel, which function at elevated temperatures and pressures. While these methods have been effective, they often come with significant energy costs and safety concerns associated with high-pressure environments (García et al. 2019; Rugolotto et al. 2007; Pandya et al. 2024). Highly effective nanocatalysts have been made available by recent developments in nanotechnology, improving the conversion of glucose to sorbitol in terms of both reaction efficiency and selectivity. Innovative approaches now focus on direct synthesis methods for sorbitol. For instance, studies have demonstrated that using Raney nickel catalysts with diols as hydrogen donors can yield high selectivity for D-sorbitol, although the process may require extensive reaction times, up to 550 hours (García et al. 2021). However, another study using porous carbon spheres supported by Ni-Ru bimetallic catalysts based on tannic acid achieved an astounding 99% conversion of glucose to sorbitol in under 150 min at 140°C (Xi et al. 2023). Furthermore, over a 6-h period at elevated temperatures (130-190°C), the potential of Raney nickel in catalytic transfer hydrogenation for glucose reduction has been investigated (García et al. 2020). Even though these techniques show considerable progress, they depend on conventional catalytic processes, which might not be the best for every application.

The goal of this work is to examine a different chemical pathway for the photocatalytic conversion of glucose to sorbitol. By leveraging photocatalytic techniques, it is possible to eliminate the need for pressurized hydrogen gas, potentially simplifying the process and making it more sustainable. Photocatalysis offers the advantage of utilizing visible light and can operate under milder conditions, thus reducing energy consumption and enhancing safety. This alternate strategy might pave the way for more effective sorbitol manufacturing, satisfying the growing need for more environmentally friendly and sustainable industrial operations. As research in this area progresses, it holds the promise of transforming how glucose is converted to valuable products like sorbitol while minimizing environmental impact and operational costs. In this study, g-C₃N₄ is modified by incorporating MgO NPs to enhance charge separation efficiency. The resulting photo-responsive MgO/g-C₃N₄ NCs exhibit superior catalytic activity for hydrogen generation compared to both g-C₃N₄ nanosheets and MgO NPs. Specifically, the NCs produce hydrogen at rates 2.13 and 8.12 times faster than the MgO NPs and g-C₃N₄, respectively. The capability of the MgO/g-C₃N₄ NCs to catalyze the degradation of methylene blue dye was also assessed. A novel CHT technique was developed, which utilizes the MgO/g-C₃N₄ photonanocatalysts in aqueous ethanol (EtOH:H₂O, 1:1) at ambient temperature, under visible light irradiation and atmospheric pressure. This method reduces D-glucose to D-sorbitol without requiring additional molecular hydrogen.

2. Materials and Methods

Magnesium nitrate hexahydrate (Mg(NO₃)₂·6H₂O, MW 256.41, BioUltra, ≥99.0% (KT), Merck), sodium hydroxide (NaOH, MW40, ACS reagent, ≥97.0%, pellets, Merck), melamine (2,4,6-Triamino-1,3,5-triazine, sym-Triaminotriazine (C₃H₆N₆), MW126.12, 99%, Merck), D-glucose (C₆H₁₂O₆, MW 180.16, ≥99.5% (GC), Merck), and sodium bisulfite (NaHSO₃, MW 104.06, ≥58.5% SO₂, Merck) were used without extra purification.

2.1 Characterization and preparation of NCs

Using an Empyrean Malvern Panalytical system (Netherlands), X-ray diffraction (XRD) was used to examine the crystal structure of the produced materials. Kα radiation (λ = 1.54060 Å) and a step size of 0.04° were used for measurements in the 2θ range of 5.0° to 100.0°. Using a Vertex 70 RAM II IR spectrometer (Bruker, Germany), Fourier-transform infrared (FT-IR) spectra were acquired. Energy dispersive X-ray spectroscopy (EDX) was used for elemental mapping, and a field emission scanning electron microscope (FESEM Quattro S, Thermo Scientific) was used for imaging and elemental analysis. A JASCO Corp. V-570 spectrophotometer was used to record the UV-visible diffuse reflectance spectra (UV-Vis DRS) between 200 and 2000 nm.

2.2 Synthesis of MgO NPs

MgO NPs were synthesized by adding 100 mL of 0.2 M magnesium nitrate dropwise to a 0.5 M sodium hydroxide solution with constant stirring. This resulted in a white precipitate of magnesium hydroxide. The precipitate was filtered and rinsed three or four times with methanol after being stirred for another 30 min. After that, the sample was dried at ambient temperature to get rid of ionic pollutants and centrifuged for 15 min at 5000 rpm to get rid of any last contaminants. According to Chandran et al. (2023), the resultant white powder was annealed in air for 2 h at 550°C.

2.3 Synthesis of g-C₃N₄ NSs

A The modified thermal condensation method was used to create g-C₃N₄ NSs. In this, 10 g of melamine was heated to 550°C for 2 h at a rate of 5°C/min in a lidded alumina crucible. After that, excess ammonia was removed by calcining the resulting bulk g-C₃N₄ at 600°C for 2 h outside, which exfoliated it into nanosheets.

2.4 Synthesis of MgO/g-C₃N₄ NCs

In 40 mL of ethanol, 0.5 g of g-C₃N₄ nanosheets and 0.4 g of MgO NPs were combined to create the MgO/g-C₃N₄ NCs. At 80°C, this mixture was agitated for 30 min. The precipitate was then centrifuged and repeatedly cleaned. The resultant precipitate was dried, and the MgO/g-C₃N₄ NSc were obtained by calcining the powder at 300°C for 30 min.

2.5 Photocatalytic hydrogen production

About 50 mg of the produced samples was added to a quartz flask that held a 100 mL ethanol and water mixture to produce hydrogen photocatalytically. After 30 min of dispersion in an ultrasonic bath, the mixture was bubbled for an additional 30 min with argon gas to remove any remaining dissolved oxygen. After that, the flask was magnetically swirled and exposed to an LED (LED COB Light, 20W, λmax = 360–700 nm) lamp for 6 h. Gas chromatography (GC) with a Molecular Sieve (MS 5 Å) column, argon as the carrier gas, and a Japanese thermal conductivity detector (TCD) was used to quantitatively measure gas samples at different irradiation time intervals using a locking-type syringe.

2.6 The general process for using photonanocatalysts to hydrogenate D-glucose is as follows

D-glucose was hydrogenated by dissolving 180 mg (0.1 mmol equivalent) of glucose in 100 mL of distilled water. To achieve concentrations of 0, 10, 25, 50, and 100 ppm, varying doses of MgO, g-C₃N₄, or MgO/g-C₃N₄ were added: 0 mg (control, no catalyst), 1 mg, 2.5 mg, 5 mg, and 10 mg. Both with and without 10% NaHSO₃ (w/w relative to the weight of glucose) as an external hydrogen source, this was conducted. To maximize conditions, reactions were conducted both in the dark and under visible light irradiation using an LED lamp (LED COB Light, 20W, λmax = 360-700 nm).

2.7 Quantitative analyses

Multiple chromatographic methods were employed to analyses the reaction aliquots. Utilizing high-performance liquid chromatography (HPLC), substrate conversion and product yields were evaluated. The Agilent 1260 Infinity II LC System, which has a UV diode array detector (DAD) and an evaporative light scattering detector (ELSD), was used to do HPLC analysis. Using an Aminex HPX-87C column and water as the mobile phase at a flow rate of 0.6 mL/min, reaction mixtures were separated. Additionally, an Agilent HP 6890 gas chromatograph equipped with a flame ionization detector was used to identify unknown compounds using gas chromatography-mass spectrometry (GC-MS). The HP INNOWax column (Agilent 19091N-113; film thickness: 0.25 μm; length: 30 m; inner diameter: 0.32 mm) ran at 30°C at the start, 150°C at the end, and 10°C/min at the ramp rate. At a flow rate of 40 mL/min, nitrogen gas was used as the carrier gas.

The following formulas were used to determine the conversion of substrate (S) and product yields (P):

(1)

Substrate Conversion (S): S (%) = (1 - \frac{C t}{C 0}) \times 100

where C₀ is the initial concentration of glucose and C_t is the concentration at time (t).

(2)

Product Yield (P): P (%) = (\frac{C t}{C 0}) \times 100

where C_t is the concentration of the product at time t. In this context: P_S = Sorbitol; P_M = Mannitol, S_G= Glucose, and P_F= Fructose.

2.8 Recyclability of catalysts

The MgO/g-C₃N₄ nanocatalyst was collected by filtration, and then it was washed with water (30 mL), acetone (30 mL), and Et₂O (30 mL). The recovered catalyst was then reused in another run under the same described reaction conditions (Attia and Mohamed 2022).

3. Results

As seen in the SEM image in Fig. 1(a), the pure g-C₃N₄ displays typical layered and stacked architectures. With a specific surface area of 21.311 m²/g, this material has a fluffier texture due to its nanosheet-like structures. With weight percentages of 35.27% for carbon (C), 52.47% for nitrogen (N), and 12.27% for oxygen (O), the EDS spectrum verifies the presence of only these three elements (Fig. 1b).

SEM images and EDS spectra of (a, b) g-C₃N₄ nanosheets, (c, d) MgO NPs, and (e, f) MgO/g-C₃N₄ NCs, illustrating their morphological characteristics and elemental compositions.

The synthesis of MgO NPs through co-precipitation is a well-established method. This technique involves precipitating a metal salt solution by adding a base, which forms a metal hydroxide precipitate. Subsequent calcination at high temperatures produces MgO NPs. With an average particle size of 31 ± 0.2 nm and a spherical shape with a uniform size distribution, the synthesized MgO NPs are effectively produced within the intended size range, according to SEM images (Fig. 1c).

The EDS spectrum shows the presence of magnesium (Mg) and oxygen (O), with weight percentages of 39.60% for Mg and 55.15% for O, confirming the absence of impurities (Fig. 1d). When MgO NPs and g-C₃N₄ nanosheets are combined, a synergistic effect occurs that improves the composite material’s overall performance. When MgO NPs are added, the composite’s average particle size drops to 22 ± 0.9 nm (Fig. 1e).

This size reduction can be attributed to the interactions between the two components during synthesis. Notably, the wrinkled nanosheet structure of g-C₃N₄ NSs is preserved in the composite, suggesting that the addition of MgO does not significantly alter the fundamental structure of g-C₃N₄. The composite’s EDS spectrum confirms the lack of contaminants by displaying the presence of Mg, C, N, and O with weight percentages of 2.19% for Mg, 53.38% for C, 24.39% for N, and 19.72% for O (Fig. 1f). Additionally, the composite has a specific surface area of 91.15 m²/g.

The stretching modes of CN heterocycles linked to the skeletal vibrations of aromatic rings are represented by unique peaks in the FTIR spectrum of g-C₃N₄, which are located at 1145, 1213, 1393, 1587, and 1648 cm⁻¹. Furthermore, the breathing mode of the triazine units is responsible for a peak at 810 cm⁻¹ (Fig. 2a). In contrast, the FTIR spectrum of MgO NPs reveals a stretching vibration mode indicative of Mg-O-Mg bonds in the range of 566 to 1100 cm⁻¹. A notable band is present at 1630 cm⁻¹, corresponding to the bending vibration of surface hydroxyl groups, while a broad peak at 3429 cm⁻¹ arises from the O-H stretching vibration of water molecules (Fig. 2a). The formation of the MgO structure is further supported by the broad peak observed in the 3300-3600 cm⁻¹ region. O-H and N-H bond stretching vibrations are responsible for the peaks between 3000 and 3345 cm⁻¹, whereas the benzene ring stretching vibration is responsible for the peak at 1635 cm⁻¹. The C-N bond extending from the s-triazine ring is linked to the peaks in the 800-1500 cm⁻¹ range.

FTIR spectra (a) XRD patterns and (b) DRS of MgO NPs, g-C₃N₄ NSs, and MgO/g-C₃N₄ NCs, highlighting their structural and optical properties.

According to Fig. 2(b), the two primary diffraction peaks for pure g-C₃N₄ in the XRD study are found at 13.1° and 27.5°, which correspond to the (100) and (002) planes, respectively. While the greater peak at the (002) plane shows the interlayer distance of the g-C₃N₄ nanosheets, the smaller peak at the (100) plane shows the stacking of aromatic rings between interlayers. The primary diffraction peaks for pure MgO are situated at 36.8°, 42.9°, and 62.3°, which correspond to the (111), (002), and (220) planes, respectively. The XRD patterns of the MgO/g-C₃N₄ NCs reveal distinct peaks associated with both components. Specifically, MgO exhibits characteristic peaks at 42.9° and 62.3°, while g-C₃N₄ displays a prominent peak at 27.8°.

The addition of MgO to g-C₃N₄ nanosheets (bandgap of 2.98 eV) appears to enhance UV-VIS absorption while reducing reflectivity. In comparison to MgO NPs, which exhibit a sharp fundamental reflectance edge at around 415 nm, the MgO/g-C₃N₄ NCs extend absorption into both the UV and visible regions, indicating successful composite formation (Fig. 2c). The smaller ionic radius of MgO may contribute to reduced lattice distortion and a modified refractive index. These electronic properties of MgO could lead to unique interactions with g-C₃N₄, slightly increasing its refractive index and resulting in a reduced bandgap of 2.77 eV. In addition to improving the optical characteristics, this component interaction raises the possibility of using MgO/g-C₃N₄ NCs in photocatalysis and other fields where better light absorption and charge separation are advantageous. The results highlight the importance of structural and compositional changes in enhancing photocatalytic material performance.

3.1 Photocatalytic activity for methylene blue (MB) dye degradation

MgO NPs, MgO/g-C₃N₄ NCs, and g-C₃N₄ nanosheets were used to study the degradation of MB dye in aqueous solution when exposed to visible light. UV-visible absorption spectroscopy was used to track the photodegradation process. As illustrated in Fig. 3, the degradation efficiency varied significantly among the different photocatalysts. Specifically, the MgO NPs achieved photodegradation of MB within 300 minutes, while the g-C₃N₄ nanosheets required only 180 min for similar results. remarkably, when the MgO/g-C₃N₄ NCs were used as the photocatalyst, total MB degradation was seen in just 30 min. Under UV irradiation, the rates of photodegradation are arranged as follows: NCs of MgO/g-C₃N₄ > NSs of g-C₃N₄ > MgO NPs.

UV-Vis absorption spectra illustrating the photodegradation of MB dye under various conditions: (a) dark conditions, (b) visible light irradiation without catalysts, (c) with 50 mg of MgO NPs, (d) with g-C₃N₄ NSs, (e) with MgO/g-C₃N₄ NCs under visible light irradiation, and (f) normalized spectra of different nanocatalysts at various exposure times.

These results imply that decreasing the size of the photocatalyst particles can improve the photocatalytic performance. This aligns with the fundamental principle that smaller NPs possess a larger surface area, which facilitates more effective interactions with the dye molecules. The claim that the MgO/g-C₃N₄ NCs display strong photocatalytic activity is supported by the fact that, after 3 h, there was no discernible absorption or degradation under dark conditions, as seen in Fig. 3(a). The promise of the MgO/g-C₃N₄ NCs as extremely effective catalysts for the breakdown of organic contaminants in aquatic environments is confirmed by their improved photocatalytic performance. The photocatalytic degradation of MB was conducted both in the dark and under visible light to further assess their effectiveness. The following formula was used to determine the percentage deterioration of MB:

(3)

Degradation (%) = (\frac{A 0 - A t}{A 0}) \times 100

Where A₀ is the initial absorbance of the solution and A_t is the absorbance after time t in minutes.

Without the addition of MgO NPs, the photocatalytic degradation of MB after 30 min of visible light irradiation was only 5.6%. In contrast, the inclusion of different NPs significantly improved the photocatalytic efficiencies: 18.42% for MgO NPs, 56.8% for g-C₃N₄, and an impressive 98.71% for the MgO/g-C₃N₄ NCs.

Using liquid chromatography-time of flight mass spectrometry (LC-TOF-MS) for additional investigation made it possible to identify the intermediate compounds that were created during the degradation of MB. One sustainable advanced oxidation process (AOP) for the elimination of organic contaminants is heterogeneous photocatalysis. Effective electron transfer between the dye molecules and the photocatalyst is made possible by the MB molecules’ easy adsorption onto the MgO/g-C₃N₄ NC surface during the photodegradation process. During photocatalytic degradation, phenol (m/z = 94) and the intermediate products adduct A (m/z = 270), adduct B (m/z = 256), and adduct C (m/z = 228) were produced by demethylation cleavage (refer to Scheme 1 and Fig. 4). These results highlight the effectiveness of the MgO/g-C₃N₄ NCs in breaking down complex organic molecules, paving the way for more efficient remediation strategies in environmental applications.

Detected intermediates from the MB dye degradation using MgO/g-C3N4 NCs.

(a-d) LC/MS spectra for each intermediate from MB dye degradation.

3.2 Production of hydrogen using MgO/g-C₃N₄ NCs

As shown in Fig. 5, the hydrogen generation activities of the synthesized g-C₃N₄ NSs, MgO NPs, and MgO/g-C₃N₄ NCs were carefully examined. According to the findings, the hydrogen evolution rate for 50 mg of MgO NPs was 30.5 μmol g⁻¹h⁻¹. The rate of hydrogen production was increased when MgO NPs were attached onto the surface of g-C₃N₄, resulting in 247.8 μmol g⁻¹h⁻¹ and 64.9 μmol g⁻¹h⁻¹, respectively.

Hydrogen evolution rate of the prepared samples MgO NPs, g-C3N4 NSs, and MgO/g-C₃N₄ NCs.

3.3 The impact of photonanocatalysts on D-glucose hydrogenation when exposed to visible light

A control study was conducted in the first stage of the research to evaluate the reduction of D-glucose to D-sorbitol in the absence of any catalyst (0 ppm). The findings showed that there was no reaction and that glucose was completely restored in both dark and visible light circumstances (Table 1, entries 1 and 2). This discovery emphasizes how important a catalyst is to the hydrogenation process. The tests were then conducted again with 10% NaHSO₃ present as a hydrogen donor. Nevertheless, no products were found in the dark, even in these conditions (Table 1, entry 3). It is interesting to note that traces of products, notably mannitol and sorbitol, were seen when the control experiment was carried out using the same hydrogen donor under visible light (Table 1, entry 4). This suggests that despite light-assisted NaHSO₃ activity, a catalyst is still crucial for substantial product generation.

Table 1. GC-MS analysis for the detection of the progress of the hydrogenation reaction of D-glucose.

Entry	Reaction condition	MgO NPs	g-C₃N₄ NSs	MgO/g-C₃N₄ NCs
Entry	Reaction condition	*S_G:P_M:P_S	S_G:P_M:P_S	S_G:P_M:P_S
1	Dark/No catalyst	100:0:0	100:0:0	100:0:0
2	Light/No catalyst	100:0:0	100:0:0	100:0:0
3	NaHSO₃/dark/No catalyst	100:0:0	100:0:0	100:0:0
4	NaHSO₃/light/No catalyst	99.6:0.2:0.2	99.4:0.2:0.6	99.3:0.2:0.5
5	NaHSO₃/light/5 ppm of catalyst	89.8:0.7:9.5	87.0:0.2:2.8	82.3:0.2:17.5
6	NaHSO₃/light/10 ppm of catalyst	86.7:0.8:12.7	83.6:0.2:31.2	79.3:0.2:20.5
7	NaHSO₃/light/25 ppm of catalyst	85.8:0.6:13.6	78.4:0.2:31.4	64.6:0.2:35.2
8	NaHSO₃/light/50 ppm of catalyst	77.1:0.6:23.3	49.1:0.2:50.7	34.1:0.2:65.7
9	NaHSO₃/light/100 ppm of catalyst	72.7:0.7:26.6	46.0:0.2:53.8	6.8:0.2:93

* S_G= Glucose, P_M= Mannitol, P_S= Sorbitol

** Optimized reaction conditions: nanocatalysts (conc. 10 ppm), 10% NaHSO₃, visible light irradiation using LED lamp, 4 h.

A third set of tests examined different photonanocatalyst concentrations (5, 10, 25, 50, and 100 ppm) under ideal reaction circumstances (Table 1, entries 5-9). The findings showed a distinct pattern: the percentage conversion yield of the products improved noticeably as the catalyst concentration rose in the presence of NaHSO₃ when exposed to visible light. This illustrates how essential photonanocatalysts are to raising the efficiency of the hydrogenation reaction. Higher catalyst concentrations resulted in a higher product yield, indicating that photonanocatalysts efficiently promote electron transfer and enhance the interaction between the hydrogen donor and D-glucose. The catalyst is activated by exposure to visible light, which encourages the production of reactive species that improve the kinetics of the reaction. Given the circumstances, these results show how crucial photonanocatalysts are to the hydrogenation of D-glucose and show how they can increase conversion rates in organic transformations when exposed to visible light. In addition to helping to clarify the catalytic processes at play, this study offers ways to improve the circumstances in subsequent investigations to increase product yields (Xi et al. 2023; García et al. 2019; García et al. 2021).

Under visible light, the results unequivocally show that MgO/g-C₃N₄ NCs function as efficient catalysts for the hydrogenation of D-glucose. Under ambient conditions, a considerable conversion was attained after 4 h at a concentration of 100 ppm (Table 2, entry 9). The effectiveness of MgO/g-C₃N₄ NCs as extremely active photocatalysts for this process is demonstrated by this discovery. The optimized reaction conditions presented in Table 2, entry 9, underscore the potential of these NCs to facilitate the reduction of D-glucose to D-sorbitol, a process crucial for various commercial applications, including the production of sugar alcohols. The ability to achieve notable conversion rates under visible light not only enhances the sustainability of the reaction but also aligns with the growing interest in utilizing renewable energy sources in chemical processes. The effectiveness of the MgO/g-C₃N₄ NCs can be attributed to their unique structural and electronic properties, which promote efficient charge separation and enhance the photocatalytic activity. The hydrogenation reaction is facilitated by the synergistic effect of MgO and g-C₃N₄, which enhances light absorption and electron transfer processes (Attia et al. 2019). Overall, these findings indicate that optimizing the reaction conditions and utilizing advanced photocatalysts like MgO/g-C₃N₄ NCs can significantly enhance the yield of D-sorbitol from D-glucose, paving the way for more efficient and environmentally friendly synthetic pathways in the production of valuable chemical intermediates. This research contributes to the broader field of photocatalysis and underscores the importance of developing effective catalytic systems for sustainable chemistry.

Table 2. Comparison of different catalysts reported in the literature with the catalytic production of sorbitol using MgO/g-C₃N₄ NCs.

Catalyst	Rx condition	Solvent	Time (hours)	Yield (%)	References
Ru/CCD	120°C, 3 MPa H₂ gas	H₂O	1.5	98.6	Li et al. 2018
Ru/ASMA@AC	130°C, 4 MPa H₂ gas	H₂O	3	99.7	Yang et al. 2023
Raney nickel catalyst	190°C, 9-26 MPa H₂ gas	H₂O	6	60	García et al. 2020
Ni–Ru	140°C, 3 MPa H₂ gas	H₂O	2.5	100	Xi et al. 2023
NiNPs/AlOH	140°C, 3 MPa H₂ gas	H₂O	24	98	Rodiansono and Shimazu 2013
Ag/AgBr/g-C₃N₄	80°C	Et: H₂O	8	89	Taha et al. 2022
MgO/g-C₃N₄ NCs	80°C	Et: H₂O	4	93	In this report

3.4 HPLC chromatograms and sugar analysis

The HPLC chromatograms provide valuable insights into the reaction progress and product distribution (Fig. 6). By comparing the chromatograms of the reaction mixtures with and without the catalyst, we can assess the effectiveness of the MgO/g-C₃N₄ NCs in catalyzing the conversion of glucose to sorbitol. The absence of glucose in the control experiment (0 ppm catalyst) confirms that the photocatalyst is essential for the reduction reaction. The addition of the catalyst, particularly at 10 ppm, significantly increases the yield of sorbitol. This implies that the hydrogenation of glucose to sorbitol is efficiently promoted by the MgO/g-C₃N₄ NCs. The HPLC analysis reveals that sorbitol is the major product, with minimal formation of other sugar byproducts like mannitol.

Evaluation of hydrogenation of glucose methods by testing various concentrations: (a) control (0 ppm), (b) 50 ppm, and (c) 100 ppm.

3.5 Catalyst reusability

One essential component of the catalyst’s effectiveness is its reusability. The data presented in Fig. 7 demonstrates that the MgO/g-C₃N₄ NCs exhibit excellent stability and reusability. After five cycles, the catalyst retains high activity, yielding 91-93% sorbitol. This excellent reusability is due to the robust nature of the NC, which endures multiple reaction cycles with minimal loss of activity. The stability of the catalyst can be further improved through careful optimization of the synthesis and reaction conditions. MgO/g-C₃N₄ NCs have the potential to be efficient and sustainable catalysts for the conversion of glucose to sorbitol, according to the HPLC analysis and reusability experiments.

Study the reusability of MgO/g-C₃N₄ NCs photocatalyst.

4. Discussion

The remarkable photocatalytic activity of the MgO/g-C₃N₄ NCs for hydrogen production can be attributed to the synergistic effects of their bandgap properties and the formation of a heterojunction. g-C₃N₄ has a bandgap of about 2.7 eV, which allows it to efficiently absorb visible light and produce electron-hole pairs. However, the rapid recombination of these charge carriers limits their overall photocatalytic efficiency. In contrast, MgO NPs have a wide bandgap that primarily absorbs UV light. The formation of a heterojunction with g-C₃N₄ makes effective charge separation possible, which is essential for improving photocatalytic activity. A built-in electric field created by the interface between MgO and g-C₃N₄ facilitates the separation of photogenerated charge carriers. While holes migrate to the valence band of g-C₃N₄, electrons from the conduction band move to the conduction band of MgO NPs. This spatial separation significantly reduces the recombination of charge carriers, thereby prolonging their lifetime. After that, protons from water molecules can be reduced by the electrons in MgO’s conduction band, producing hydrogen gas. At the same time, water molecules may be oxidized by the holes in the g-C₃N₄ valence band, producing oxygen gas (Ling et al. 2023; Bhanderi et al. 2024; Yan et al. 2024). Furthermore, when the separated charge carriers combine with water molecules or dissolved oxygen, reactive species, including hydroxyl radicals (•OH) and superoxide radicals (•O₂⁻), are created. By attacking and dissolving organic contaminants like MB dye into smaller, less hazardous components, these extremely reactive species efficiently destroy them.

The combination of g-C₃N₄ and MgO NPs not only broadens the light absorption range, allowing for more efficient utilization of solar energy, but also enhances charge separation, thereby reducing recombination losses. Additionally, MgO’s large surface area increases the number of active sites available for MB molecule adsorption and reactive species production, which speeds up the degradation process. Importantly, the materials used in synthesizing MgO/g-C₃N₄ NCs are non-toxic and environmentally friendly, making these nanocomposites promising candidates for sustainable hydrogen production and pollutant degradation applications (Alqarni et al. 2024).

Table 2 highlights that MgO/g-C₃N₄ NCs are exceptionally promising catalysts without an external source of H₂ gas and under mild conditions due to their unique structural and compositional characteristics. The large surface area of the NC facilitates the adsorption of reactants, significantly enhancing catalytic activity. Additionally, the synergistic effect resulting from the interaction between MgO NPs and g-C₃N₄ components further enhances catalytic performance compared to the individual components. The complementary properties of both materials drive this beneficial interaction: g-C₃N₄ serves as a stable substrate for charge separation and transfer, while MgO NPs contribute to redox activity. Consequently, MgO/g-C₃N₄ NCs effectively and selectively catalyze the hydrogenation of glucose to sorbitol.

4.1 Proposed mechanism for glucose hydrogenation catalyzed by MgO/g-C₃N₄ NCs:

The proposed mechanism for the MgO/g-C₃N₄ NCs-catalyzed hydrogenation of glucose to sorbitol involves a complex interplay of factors, including the role of sodium persulfate and the solvent. The MgO/g-C₃N₄ NCs produce electron-hole pairs and absorb photons when exposed to visible light. Reactive species can develop because of the excited electrons and holes taking part in redox processes. Sodium persulfate-mediated H₂ cleavage: Sodium persulfate can function as an oxidant, leading to the heterolytic cleavage of H₂. This mechanism involves the formation of sulfate radicals, which can abstract hydrogen atoms from water or other hydrogen donors. Solvent-mediated H₂ activation: The presence of aqueous ethanol can facilitate the homolytic cleavage of H₂. The solvent molecules can interact with the hydrogen molecule, weakening the H-H bond and promoting the formation of hydrogen radicals. The activated hydrogen species, generated through either the persulfate-mediated or solvent-mediated pathways, can react with the carbonyl group of glucose. The hydrogen atoms are added to the carbonyl group, leading to the formation of sorbitol (Taha et al. 2022). The combination of MgO NPs and g-C₃N₄ broadens the light absorption range, allowing for efficient utilization of solar energy. By facilitating charge carrier separation, the heterojunction between MgO NPs and g-C₃N₄ lowers recombination losses. The NC’s extensive surface area provides numerous active sites for the adsorption of reactants and the desorption of products.

The MgO NPs can improve the stability of the catalyst, preventing degradation under reaction conditions. The MgO/g-C₃N₄ NCs catalyst exhibits appreciable water tolerance, allowing the hydrogenation reaction to proceed even in the presence of moisture. This is a significant advantage, as it simplifies the reaction setup and reduces the need for stringent drying conditions. In conclusion, the MgO/g-C₃N₄ NCs, in conjunction with sodium persulfate or aqueous ethanol, provide an efficient and sustainable approach for the photocatalytic conversion of glucose to sorbitol. Further research is needed to fully elucidate the detailed mechanism and to optimize the reaction conditions for improved yields and selectivity.

This study provides novel contributions that advance the fields of photocatalysis and sustainable chemical processes. The development of a novel catalytic hydrogen transfer (CHT) method utilizing MgO/g-C₃N₄ NCs represents a significant advancement in the efficient conversion of D-glucose to D-sorbitol without the need for additional molecular hydrogen. The modification of g-C₃N₄ with MgO to create photo-responsive NCs demonstrates a unique strategy for improving charge separation efficiency. This leads to hydrogen generation rates that are 2.13 times and 8.12 times faster than those of unmodified g-C₃N₄ and MgO NPs, respectively. The study emphasizes a green methodology by conducting reactions at room temperature and atmospheric pressure, utilizing a 1:1 mixture of aqueous ethanol and water, which aligns with sustainable chemistry principles. Achieving a selective conversion rate of 93% for glucose to sorbitol and demonstrating catalyst stability over multiple cycles highlights the practical applicability of the MgO/g-C₃N₄ system in sustainable synthesis. The findings open pathways for further exploration of MgO/g-C₃N₄ NCs in various photocatalytic applications, including dye degradation and other organic transformations, enhancing their potential in environmental and energy-related fields. These aspects collectively underscore the innovative nature of the research, contributing valuable insights and methodologies to the field of photocatalysis and green chemistry.

The limitations of this study can be concluded as follows. The catalytic performance was evaluated under specific conditions (e.g., temperature, light intensity, and reaction medium). The scalability and efficiency of the process under varying conditions or in real-world applications remain to be assessed. The study primarily focuses on the conversion of D-glucose to D-sorbitol. Investigating the catalyst’s performance on a broader range of substrates would enhance the understanding of its versatility and applicability in various reactions. While the study emphasizes a green methodology, a detailed assessment of the environmental impact of the materials used and the overall process sustainability would strengthen the study’s contributions to green chemistry. Addressing these limitations in future research could provide a more robust understanding of the MgO/g-C₃N₄ NCs’ properties and its potential applications in photocatalysis.

5. Conclusions

This study offers a productive and environmentally responsible way to convert glucose to sorbitol, marking a breakthrough in the field of green chemistry. The utilization of visible light as an energy source is particularly advantageous, as it aligns with sustainable energy principles and reduces reliance on fossil fuels. The synergistic combination of MgO NPs and g-C₃N₄ creates a highly efficient photocatalyst capable of generating reactive species under visible light irradiation. The addition of NaHSO₃ serves as a crucial hydrogen source, facilitating the reduction of glucose to sorbitol. The reaction is conducted at ambient temperature and pressure, minimizing energy consumption and simplifying the process. The process exhibits high selectivity towards sorbitol, minimizing the formation of unwanted byproducts. This innovative approach offers a promising pathway for the sustainable production of sorbitol, a versatile chemical with applications in various industries. Further optimization of the catalyst and reaction conditions may lead to even higher yields and selectivity. Additionally, exploring this catalytic system’s potential for other reduction reactions could open new avenues in green chemistry.

Acknowledgment

This scientific research paper was derived from a research grant funded by Taibah University, Madinah, Kingdom of Saudi Arabia - with the grant number (446-13-986)

CRediT authorship contribution statement

Salhah Hamed Alrefaee: Conceptualization, supervision, validation, data curation, software, methodology, visualization, investigation, writing-original draft preparation, writing-reviewing and editing.

Declaration of competing interest

The authors declare that they have no competing financial interests or personal relationships that could have influenced the work presented in this paper.

Declaration of Generative AI and AI-assisted technologies in the writing process

The authors confirm that there was no use of Artificial Intelligence (AI)-Assisted Technology for assisting in the writing or editing of the manuscript and no images were manipulated using AI.

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1. Introduction

2. Materials and Methods

2.1 Characterization and preparation of NCs
2.2 Synthesis of MgO NPs
2.3 Synthesis of g-C₃N₄ NSs
2.4 Synthesis of MgO/g-C3N4 NCs
2.5 Photocatalytic hydrogen production
2.6 The general process for using photonanocatalysts to hydrogenate D-glucose is as follows
2.7 Quantitative analyses
2.8 Recyclability of catalysts

3. Results

3.1 Photocatalytic activity for methylene blue (MB) dye degradation
3.2 Production of hydrogen using MgO/g-C₃N₄ NCs
3.3 The impact of photonanocatalysts on D-glucose hydrogenation when exposed to visible light
3.4 HPLC chromatograms and sugar analysis
3.5 Catalyst reusability

4. Discussion

4.1 Proposed mechanism for glucose hydrogenation catalyzed by MgO/g-C3N₄ NCs:

5. Conclusions

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[1] Ahmad A., Khan M., Khan S., Luque R., Almutairi T.M., Karami A.M.. Bio-construction of MgO nanoparticles using Texas sage plant extract for catalytical degradation of methylene blue via photocatalysis. Int J Environ Sci Technol. 2023;20:1451-1462. https://doi.org/10.1007/s13762-022-04090-2
[Google Scholar]

[2] Alqarni L.S., Alghamdi M.D., Alhussain H., Elamin N.Y., Taha K.K., Modwi A.. S-scheme MgO–TiO₂@g-C₃N₄ nanostructures as efficient photocatalyst for alizarin red S photodegradation. J Mater Sci: Mater Electron. 2024;35 https://doi.org/10.1007/s10854-024-11996-9
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[3] Attia Y.A., Ezet A., Saeed S., Galmed A.H.. Nano carbon-modified air purification filters for removal and detection of particulate matters from ambient air. Sci Rep. 2024;14:621. https://doi.org/10.1038/s41598-023-50902-x
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[4] Attia Y.A., Mohamed Y.M.. Silicon-grafted Ag/AgX/rGO nanomaterials (X = Cl or Br) as dip-photocatalysts for highly efficient p-nitrophenol reduction and paracetamol production. Appl Organomet Chem. 2019;33:e4757. https://doi.org/10.1002/aoc.4757
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[5] Attia Y.A., Mohamed Y.M.A.. Nano Ag/AgCl wires-photocatalyzed hydrogen production and transfer hydrogenation of Knoevenagel-type products. New J Chem. 2022;46:1677-1686. https://doi.org/10.1039/d1nj04985b
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[6] Bhanderi D., Lakhani P., Modi C.K.. Graphitic carbon nitride (g-C₃N₄) as an emerging photocatalyst for sustainable environmental applications: a comprehensive review. RSC Sustain.. 2024;2:265-287. https://doi.org/10.1039/D3SU00382E
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[7] Chandran A., Prakash J., Naik K.K., Srivastava A.K., Dąbrowski R., Czerwiński M., łBiradar A.M.. Preparation and characterization of MgO nanoparticles/ferroelectric liquid crystal composites for faster display devices with improved contrast. J Mater Chem C. 2014;2:1844. https://doi.org/10.1039/c3tc32017k
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[8] Dahiya S., Sharma A., Chaudhary S.. Eco-inspired synthesis of MgO-infused g-C₃N₄ nanocomposites from tulsi seeds for advanced photocatalytic environmental remediation. Phys Chem Chem Phys. 2024;26:28064-28081. https://doi.org/10.1039/d4cp03673e
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[9] Di J., Xia J., Yin S., Xu H., He M., Li H., Xu L., Jiang Y.. A g-C₃N₄/BiOBr visible-light-driven composite: Synthesis via a reactable ionic liquid and improved photocatalytic activity. RSC Adv. 2013;3:19624. https://doi.org/10.1039/c3ra42269k
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[10] García B., Moreno J., Iglesias J., Melero J.A., Morales G.. Transformation of glucose into sorbitol on raney nickel catalysts in the absence of molecular hydrogen: Sugar disproportionation vs. catalytic hydrogen Transfer. Top Catal. 2019;62:570-578. https://doi.org/10.1007/s11244-019-01156-3
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[11] García B., Moreno J., Morales G., Melero J.A., Iglesias J.. Production of sorbitol via catalytic transfer hydrogenation of glucose. Appl Sci. 2020;10:1843. https://doi.org/10.3390/app10051843
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[12] García B., Orozco-Saumell A., Granados M.L., Moreno J., Iglesias J.. Catalytic transfer hydrogenation of glucose to sorbitol with raney Ni catalysts using biomass-derived diols as hydrogen donors. ACS Sustainable Chem Eng. 2021;9:14857-14867. https://doi.org/10.1021/acssuschemeng.1c04957
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[13] Gatou M.A., Skylla E., Dourou P., Pippa N., Gazouli M., Lagopati N., Pavlatou E.A.. Magnesium oxide (MgO) nanoparticles: Synthetic strategies and biomedical applications. Crystals. 2024;14:215. https://doi.org/10.3390/cryst14030215
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[14] Ge L., Han C., Liu J., Li Y.. Enhanced visible light photocatalytic activity of novel polymeric g-C3N4 loaded with Ag nanoparticles. Appl Catal A: Gen. 2011;409-410:215-222. https://doi.org/10.1016/j.apcata.2011.10.006
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[15] Hakimioun A.H., Vandegehuchte B.D., Curulla-Ferre D., Kaźmierczak K., Plessow P.N., Studt F.. Metal–support interactions in heterogeneous catalysis: DFT Calculations on the interaction of copper nanoparticles with magnesium oxide. ACS Omega. 2023;8:10591-10599. https://doi.org/10.1021/acsomega.3c00502
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[16] Huang Z., Chen L., Zhang H., Humayun M., Duan J., Zhu Q., Bououdina M., Cao Y., Attia Y.A., Kardas G., Wang C.. Manipulating interfacial charge redistribution in Mott-Schottky electrocatalyst for high-performance water/seawater splitting. Chem Eng J. 2024;501:157628. https://doi.org/10.1016/j.cej.2024.157628
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Visible light-triggered catalytic conversion of D-glucose to sorbitol using magnesium oxide/graphitic carbon nitride nanocomposites

Abstract

Keywords

Catalytic hydrogen transfer (CHT)

D-sorbitol; Photocatalysis

Graphitic carbon nitride (g-C3N4)

Magnesium oxide (MgO)

1. Introduction

2. Materials and Methods

2.1 Characterization and preparation of NCs

2.2 Synthesis of MgO NPs

2.3 Synthesis of g-C₃N₄ NSs

2.4 Synthesis of MgO/g-C3N4 NCs

2.5 Photocatalytic hydrogen production

2.6 The general process for using photonanocatalysts to hydrogenate D-glucose is as follows

2.7 Quantitative analyses

2.8 Recyclability of catalysts

3. Results

3.1 Photocatalytic activity for methylene blue (MB) dye degradation

3.2 Production of hydrogen using MgO/g-C₃N₄ NCs

3.3 The impact of photonanocatalysts on D-glucose hydrogenation when exposed to visible light

3.4 HPLC chromatograms and sugar analysis

3.5 Catalyst reusability

4. Discussion

4.1 Proposed mechanism for glucose hydrogenation catalyzed by MgO/g-C3N₄ NCs:

5. Conclusions

Acknowledgment

CRediT authorship contribution statement

Declaration of competing interest

Declaration of Generative AI and AI-assisted technologies in the writing process

References

Suggested read for related articles:

2.4 Synthesis of MgO/g-C₃N₄ NCs

4.1 Proposed mechanism for glucose hydrogenation catalyzed by MgO/g-C₃N₄ NCs: