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Article

Enhancing the Adsorption Performance of HKUST-1 by Adding NH4F During Room-Temperature Synthesis for Desulfurization of Fuel Oil

by
Jiawei Fu
1,
Xinchun Liu
1,
Yuqing Kong
1,
Ruyu Zhao
1,
Yinyong Sun
1,* and
Ahmed S. Abou-Elyazed
2
1
MIIT Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage, School of Chemistry and Chemical Engineering, Harbin Institute of Technology, Harbin 150001, China
2
Institute of Intelligent Manufacturing Technology, Shenzhen Polytechnic University, Shenzhen 518055, China
*
Author to whom correspondence should be addressed.
Energies 2025, 18(20), 5344; https://doi.org/10.3390/en18205344 (registering DOI)
Submission received: 31 August 2025 / Revised: 7 October 2025 / Accepted: 8 October 2025 / Published: 10 October 2025
(This article belongs to the Special Issue Challenges and Opportunities in the Global Clean Energy Transition)
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Abstract

Adsorption desulfurization of fuel oil is regarded as one of the most promising technologies for obtaining clean fuel because it can remove refractory sulfur compounds at ambient temperature and pressure. Studies indicate that HKUST-1, as an important type of metal–organic framework (MOF), is a potential candidate for adsorption desulfurization of fuel oil. In this work, we report that defective HKUST-1 can be rapidly synthesized at room temperature with the aid of NH4F and exhibit superior adsorption desulfurization performance compared to conventional HKUST-1 by the solvothermal method. Moreover, the influence of adsorption parameters on the desulfurization performance of HKUST-1 prepared with the aid of NH4F was investigated. We used 50 mg of HKUST-1-5 synthesized with 5 wt% added NH4F to adsorb 5 g of model oil with a sulfur concentration of 1000 ppm at 25 °C for 1 h, and the adsorption capacity of the adsorbent reached 23.8 mgS/g, 46.8 mgS/g and 36.8 mgS/g for benzothiophene (BT), dibenzothiophene (DBT) and 4,6-dimethyldibenzothiophene (4,6-DMDBT), respectively, which are higher values than those of conventional HKUST-1. Such performance can be mainly attributed to its relatively small particle size and the presence of more unsaturated Cu sites. The results of regeneration experiments show that HKUST-1-5 still maintains excellent adsorption performance after four cycles. These findings highlight the great potential of this material as an efficient adsorbent for adsorption desulfurization of fuel oil.

1. Introduction

With the acceleration of industrial development, the consumption of fossil fuels is on the rise. In the process of fuel processing, sulfur compounds in fuel oil would cause not only corrosion of equipment and poison the catalyst used in the reaction [1,2], but also serious environmental problems and damage to the respiratory system due to the combustion of the subsequent processed products [3]. Therefore, it is important for protecting the environment and human health to develop relevant technologies to realize the deep removal of sulfur compounds in fuel oil.
Currently, the main desulfurization technology in industry is hydrodesulfurization (HDS) [4], which needs higher operating temperature (300–400 °C), pressure (20–60 bar) and expensive hydrogen. Comparatively, adsorption desulfurization technology without hydrogen consumption is simple to operate and can remove refractory sulfur compounds that are difficult to desulfurize by HDS technology [5]. It is regarded as one of the most promising technologies to obtain ultra-low-sulfur fuel. Therefore, the development of highly efficient adsorbents has been of great interest.
Metal–organic frameworks (MOFs), with advantages such as large specific surface area, adjustable pore structure and easy functionalization, are considered as a kind of ideal adsorbent for adsorption desulfurization of fuel oil [6,7,8,9,10]. Matzger et al. [11] reported for the first time that MOFs as adsorbents were utilized in adsorption desulfurization of model fuel oil. It was found that the adsorption capacity of MOFs was higher than that of zeolites. Achmann et al. [12] studied four kinds of MOFs for the adsorption desulfurization of different types of real fuel oils. The results indicated that HKUST-1 had highest adsorption capacity among these MOFs. Peralta et al. [13] compared the selectivity and reproducibility of HKUST-1 and CPO-27 in adsorption desulfurization. It was noted that HKUST-1 was more selective and reproducible than CPO-27. In addition, Duan et al. [14] synthesized several HKUST-1 materials by various methods. The results showed that HKUST-1 prepared by the hydrothermal method possessed the largest adsorption capacity for the removal of thiophene.
In this contribution, defective HKUST-1 was rapidly synthesized with the addition of NH4F at room temperature and exhibited superior adsorption desulfurization performance. The obtained materials were characterized by various techniques. Their adsorption desulfurization performance was evaluated by the adsorption of sulfur-containing compounds like dibenzothiophene (DBT) in model fuel oil. Based on the experimental results, a possible adsorption mechanism was proposed.

2. Materials and Methods

2.1. Materials

N, N-Dimethylformamide (DMF, >99.5%), ethanol (>99.7%), methanol (>99%), copper nitrate trihydrate (Cu(NO3)2⋅3H2O, >99%) and ammonium fluoride (NH4F, >99%) were obtained from China National Pharmaceutical Group Limited. n-Octane(99.5%), 1,3,5-benzenetricarboxylic acid (H3BTC, 98%), benzothiophene (BT, 98%), dibenzothiophene (DBT, >98%) and 4,6-dimethyldibenzothiophene (4,6-DMDBT, 99%) were purchased from Beijing InnoChem Science & Technology Co., Ltd., China.

2.2. Solvothermal Synthesis of HKUST-1-S

HKUST-1-S was prepared by using previously established methodologies [15]: 1.00 g H3BTC was dissolved in 30 mL mixed solution of ethanol/DMF with a volume ratio of 1:1 to form solution A, and 2.077g Cu(NO3)2·3H2O was dissolved in 15 mL deionized water to form a transparent light blue solution, referred to as solution B. Under the condition of strong stirring, solution B was poured into solution A at room temperature and kept stirring for 10 min. The obtained solution was transferred into an autoclave with a PTFE lining and heated at 120 °C for 12 h. After that, the autoclave was naturally cooled to room temperature. The resultant product was washed with anhydrous ethanol at 60 °C for 2 h, dried at 70 °C for 3 h, and activated at 150 °C for 12 h under vacuum. The final product was named HKUST-1-S.

2.3. Room-Temperature Synthesis of HKUST-1-x with the Addition of NH4F

1.00 g H3BTC was dissolved in 30 mL mixed solution of ethanol/DMF with a volume ratio of 1:1 to form solution A, and 2.077 g of Cu(NO3)2·3H2O was dissolved in 15 mL of NH4F aqueous solution with different mass fractions (2.5%, 5%, 10%, 15%) to form a transparent light blue solution, referred to as solution B. Under strong stirring, solution B was poured into solution A at room temperature and keep stirring for 30 min. The resultant sample was centrifugally separated and then washed with deionized water trice and methanol twice at room temperature. Suction filtration and rotary evaporation were sequentially carried out on the separated liquid to recover NH4F. After drying in an oven at 70 °C for 3 h, the obtained sample was activated at 150 °C for 12 h under vacuum. The final product was named HKUST-1-x, where x represents the mass fraction of NH4F. The mass fraction of ammonium fluoride ranged from 2.5% to 15%, and the synthesized HKUST-1-x was 1.69 g, 1.52 g, 1.54 g and 1.49 g in turn.

2.4. Batch Adsorption Test

Model fuel oil with different sulfur concentrations (the sulfur atomic mass fraction in the compound) was prepared by mixing different amounts of sulfur compounds such as BT, DBT and 4,6-DMDBT with n-octane, respectively. The adsorbent was degassed at 150 °C in vacuum for 2 h in advance. Then, 50 mg of adsorbent was quickly added to a flask containing 5 g of model fuel oil. The flask was placed in a water bath at 25 °C. A few samples of liquid were taken at different times and then analyzed by an Agilent 7890A gas chromatography (GC) apparatus. The adsorption capacity was calculated by the following formula:
Q t = V ( C 0 − C t ) m
Qt, V, C0, Ct, and m represent the adsorption capacity at different times (mgS/g), the volume of model oil (mL), initial sulfur concentration (mgS/mL), sulfur concentration at different times (mgS/mL), and mass of adsorbent (g), respectively.

2.5. Cycle Test

The adsorbent was degassed at 150 °C in vacuum for 2 h in advance. Then, 100 mg of adsorbent was quickly added to a flask containing 10 g of model fuel oil. The flask was placed in a water bath at 25 °C. After the adsorption experiment, the simulated oil and adsorbent were separated by centrifugation. The resultant adsorbent was washed with anhydrous ethanol 3 times and dried at 70 °C for 3 h. Finally, the sample was activated at 150 °C under vacuum for 12 h for the next experiment.

2.6. Characterization

Powder X-ray diffraction (XRD) patterns were recorded on a Bruker D8 advance diffractometer in Bragg–Brentano geometry equipped with a Ge-focusing primary monochromator (Cu-Kα radiation, λ = 0.15406 nm) at 40 kV and 40 mA with a scanning speed of 9° min−1 and a step size of 0.02°. Scanning electron microscopy (SEM) images were obtained using a SUPRA 55 instrument with an acceleration voltage of 15 kV. Fourier transform infrared (FT-IR) spectra were collected in the range of 400–4000cm−1 on the Thermo Fisher Scientific Nicolet iS20 spectrometer. The N2 adsorption–desorption isotherms were obtained at 77 K on a BSD-PS1 Static Volumetric Specific Surface and Aperture Analyzer. Before nitrogen adsorption, the samples were pretreated at 423 K for 2 h under vacuum to remove the impurities. The total surface area was calculated via the Brunauer–Emmett–Teller (BET) equation. An X-ray photoelectron spectrometer (XPS) was used to analyze the chemical composition of all the samples on the Thermo Scientific K-Alpha spectrometer. Thermogravimetric analysis (TGA) was performed on a HITACHI STA200 instrument under air atmosphere at a ramp rate of 10 °C/min. The NH3-TPD test was carried out on a chemisorption instrument with the model Micromeritics AutochemIII2930.

3. Results and Discussion

3.1. Structural Characterization

The power XRD patterns of HKUST-1-x are shown in Figure 1a. As seen, all the samples showed well-resolved diffraction peaks, which are in good agreement with the simulated ones belonging to the crystal structure of HKUST-1. The diffraction peaks of 2θ = 7.2°, 9.4° and 11.8° correspond to (200), (220) and (222) crystal planes, respectively [16,17]. Obviously, the addition amount of NH4F during synthesis had a great influence on the crystallinity of HKUST-1. Notably, when the mass fraction of NH4F is less than or equal to 5%, the intensity of diffraction peaks is high, meaning that most of the crystal planes can be well observed. When the mass fraction of NH4F is more than 5%, the intensity of diffraction peaks becomes weak. It is possible that excessive NH4F would lead to a drop in the pH of the reaction system, which is harmful for the crystallization of products [18].
Figure 1b shows the FT-IR spectra of HKUST-1-x. The absorption peak at 730 cm−1 corresponds to the C-H bending vibration of the benzene ring in trimellitic acid [19]. The absorption peak at 1550 cm−1 is associated with the asymmetric stretching vibration of -COO- in the structure [20]. Additionally, the absorption peaks at 1371 cm−1 and 1447 cm−1 are ascribed to the symmetric stretching vibration of the -COO- group [21]. The vibration of Cu-O absorption peaks at 1110 cm−1 and 938 cm−1 directly confirm the successful coordination of metal ions with ligands [22]. Based on the above results, it can be concluded that HKUST-1 has been rapidly synthesized at ambient temperature and pressure with the aid of NH4F. Compared with the traditional solvothermal method, the NH4F-assisted synthesis does not require a long heating and crystallization process. Under the same feeding conditions, the production efficiency of HKUST-1 by the solvothermal method and the NH4F-assisted synthesis method is 0.18 g/h and 3.04 g/h, respectively. Therefore, the NH4F-assisted method has lower energy consumption and cost.
Figure 2 shows the N2 adsorption–desorption isotherms and corresponding pore size distribution curves. As seen in Figure 2a, all the samples exhibited typical type I isotherm, indicating the existence of micropores [23,24]. Their average micropore size is between 0.6 and 0.8 nm (Figure 2b). The detailed sorption data are shown in Table 1. Apparently, HKUST-1-5 gave the highest BET specific surface area (1507 m2/g) among these studied materials, which is in agreement with the XRD results. We speculated that a low NH4F concentration is not beneficial for the rapid crystallization of HKUST-1. If a high NH4F concentration is used, the pH value of the system would decrease and thus result in the formation of amorphous product.
Figure 3 presents the SEM images of HKUST-1-x. It is noted that HKUST-1 prepared with a low mass fraction of NH4F (HKUST-1-2.5 and HKUST-1-5) possessed small particle size (100~200 nm) and a morphology of irregular polyhedrons. Differently, the surface of HKUST-1-2.5 is smooth. The surface of HKUST-1-5 is rough and there are some obvious dimples. Comparatively, HKUST-1 samples prepared with a high mass fraction of NH4F (HKUST-1-10 and HKUST-1-15) have large particle size (2–8 μm) and a rodlike morphology. These results indicate that the addition amount of NH4F had a great influence on the particle size and morphology of HKUST-1. Such effect can be also observed in the synthesis of HKUST-1 with the addition of certain metal ions like K+ or Na+ [25].

3.2. Evaluation of Adsorption Desulfurization Performance

The adsorption desulfurization performance of HKUST-1-x was firstly evaluated by the removal of DBT in model fuel oil. As seen in Figure 4, HKUST-1-5 exhibited the best adsorption performance among these HKUST-1-x materials. Its adsorption capacity for DBT could reach 46.8 mgS/g in 20 min at room temperature. Comparatively, the adsorption capacity of HKUST-1-S prepared by the solvothermal method is 40.9 mgS/g under the same conditions. Such adsorption performance is still outstanding compared with that of some reported MOFs (Table 2).
To further assess the adsorption performance of HKUST-1-5, a comprehensive comparison was made with HKUST-1-S. Firstly, the influence of sulfur compounds on adsorption desulfurization of HKUST-1-5 was investigated. As shown in Figure 5, the adsorption equilibrium of both adsorbents can be reached in 20 min for three kinds of simulated fuel oils. Overall, the adsorption performance of HKUST-1-5 for the removal of all sulfur compounds was better than that of HKUST-1-S. Nevertheless, the adsorption capacity varies with the different sulfur compounds. The order of adsorption capacity is DBT > 4,6-DMDBT > BT. Such difference might be mainly caused by the different electron cloud density distributions around S atoms in sulfur compounds and steric hindrance effects [33,34]. Interestingly, as for the removal of bulky 4,6-DMDBT that is difficult to desulfurize by the HDS technique, HKUST-1-5 gave a adsorption capacity of 36.8 mgS/g, which is much higher than that (22.4 mgS/g) of HKUST-1-S. This result suggests that HKUST-1-5 could be a good adsorbent for deep desulfurization of fuel oil.
A pseudo-first-order reaction model and pseudo-second-order reaction model were used to fit the adsorption data (Figures S1 and S2). The important parameters are shown in Table 3 and Table 4. All correlation coefficients are less than 0.90 based on the pseudo-first-order reaction model and higher than 0.99 according to the pseudo-second-order reaction model, revealing that the adsorption desulfurization process on HKUST-1 should belong to pseudo-second-order kinetics. In addition, the measured adsorption equilibrium capacities for BT, DBT and 4,6-DMDBT are close to the Qe values calculated by the pseudo-second-order kinetic model. This suggests that the rate-limiting step of the adsorption process should be a chemical interaction process. Moreover, K2 of HKUST-1-5 is higher than that of HKUST-1-S, which is consistent with the results for adsorption capacity.
In order to confirm the adsorption model, the adsorption isotherms are shown in Figure 6. For three kinds of sulfur compounds, the initial sulfur content was tuned from 250 ppm to 1000 ppm. As seen, the adsorption capacity of both adsorbents displayed a similar upward trend with the increase in initial concentration. The Langmuir model and Freundlich model were used to fit the desulfurization isotherms (Figures S3 and S4). The important parameters are shown in Table 5 and Table 6. The obtained R2 value based on the Freundlich model is larger than that from the Langmuir model. Obviously, the Freundlich model can better simulate the adsorption desulfurization process of both materials, indicating that the adsorption of three sulfur compounds on HKUST-1 should belong to multi-layer chemical adsorption [35].
To evaluate the adsorption performance of HKUST-1-5 and HKUST-1-S in complex oil, 10 wt% benzene was added to the model oil. The experimental results are shown in Figure 7. The adsorption capacity of both materials would greatly decrease with the addition of benzene. However, HKUST-1-5 still exhibited better adsorption performance than HKUST-1-S, which shows that HKUST-1-5 has stronger adsorption selectivity for sulfur-containing compounds and is more suitable for adsorption desulfurization of real fuel.
The stability of adsorbents is of practical importance during adsorption. In this study, a cycle experiment on HKUST-1-5 was carried out. HKUST-1-5 materials before and after adsorption were characterized (Figure 8, Table 7). In the beginning, the adsorption capacity for DBT was 49.4 mgS/g. After four consecutive cycles of adsorption, the adsorption capacity for DBT can still stay above 45 mgS/g, indicating that HKUST-1-5 may be reused for several cycles. In addition, the XRD patterns of used HKUST-1-5 are consistent with those of fresh HKUST-1-5, demonstrating that the crystal structure of HKUST-1-5 is stable. Furthermore, the fact that the used HKUST-1-5 has a similar specific surface area to its fresh counterpart can support this point. Notably, the average micropore size and volume are slightly decreased after reuse, which might be attributed to the case that partial adsorption active sites in the pores are covered by adsorbates [14]. Also, it may hinder the effective contact between adsorbates and adsorption active sites, resulting in a decrease in adsorption performance.

3.3. Relationship Between Adsorption Desulfurization Performance and Structure

To clarify the relationship between adsorption performance and structure, XPS of HKUST-1-5 and HKUST-1-S was measured. As shown in Figure 9, the results confirm that both adsorbents contain elements such as carbon (C), oxygen (O), and copper (Cu). The peaks of 284.8 eV, 286 eV and 288.65 eV are attributed to C=C, C=O and O=C-O respectively [36,37]. The relative content of C=O in HKUST-1-5 is higher than that in HKUST-1-S. In the high-resolution O 1s spectrum, the peaks at 231.64 eV, 232.46 eV and 233.68 eV belong to C-O, C=O and adsorbed oxygen, respectively [38]. However, all peaks corresponding to HKUST-1-5 shifted toward high binding energy, indicating that the chemical environment of O was different and the electron cloud density around O decreased. Moreover, the high-resolution XPS spectra of copper only exhibited the existence of Cu (II) associated with Cu-O bonds in the HKUST-1 framework and both adsorbents possessed similar proportions of Cu species. This result revealed that the difference in the adsorption desulfurization performance for both adsorbents had no close relationship with the valence of Cu species.
From the SEM results, it can be seen that there a big difference in the particle size of both adsorbents (Figure S5). HKUST-1-5 had much smaller average particle size (around 0.15 μm) than HKUST-1-S (about 16 μm). This suggests that the surface on HKUST-1-5 might expose more adsorption sites. Moreover, the average pore size of HKUST-1-5 is slightly larger than that of HKUST-1-S (Figure S6, Table S1). The large average pore size can make adsorbates enter the pore channels of HKUST-1 easily and thus enhance the adsorption performance.
Thermogravimetric analysis is an effective method for characterizing ligand defects in MOFs [39]. In order to determine the defects and their thermal stability, TG curves of HKUST-1-5 and HKUST-1-S were measured (Figure 10). The whole weight loss process of both samples can be divided into three stages. The first weight loss is attributed to the removal of water or other gases trapped in micropores. The second one corresponds to the evaporation of physically adsorbed water and the removal of μ-OH in clusters [40]. The third one originates from the removal of organic ligands [41]. The mass fractions of organic ligands in HKUST-1-S and HKUST-1-5 are 50.57% and 39.23%, respectively. Meanwhile, the mass fraction of the remaining CuO is 38.43% and 42.06%, respectively. The molar ratios of Cu to organic ligand in HKUST-1-S and HKUST-1-5 are 3:1.516 and 3:1.075, respectively. It is known that the molar ratio of Cu to organic ligand in perfect HKUST-1 crystals is 3:2 [42]. Based on these data, the calculated ligand loss rates for HKUST-1-S and HKUST-1-5 are 24.2% and 44.2%, respectively. This means that HKUST-1-5 has more Cu unsaturated coordination sites (defects), which can be helpful for improving the adsorption desulfurization performance.
To further confirm the defects in both samples, the NH3-TPD technique was used [43]. As obtained from Figure 11, the number of Lewis acid sites in HKUST-1-5 and HKUST-1-S was 6.59 mmol/g and 6.19 mmol/g, respectively. This means that HKUST-1-5 possessed more Cu unsaturated coordination sites than HKUST-1-S, which is consistent with the results from TG analysis.
FT-IR spectra of HKUST-1-5 before and after DBT adsorption were performed. As shown in Figure 12, a new absorption peak appears at 1252 cm−1 after DBT adsorption, which is attributed to the C-S stretching vibration in the thiophene ring from DBT [44]. This result indicates that there is a strong interaction between HKUST-1-5 and DBT.
Based on the above results, it is concluded that the main reason why HKUST-1-5 exhibited enhanced adsorption desulfurization performance could be attributed to the existence of more defects and its smaller particle size. For this, a plausible adsorption process is shown in Figure 13. In this process, sulfur compounds like DBT were possibly adsorbed by two modes. One mode involves the unsaturated Cu sites in the structure of HKUST-1 behaving as electron acceptors and sulfide acting as an electron donor. The sulfur compounds can be adsorbed by the formation of Cu–S coordination bonds. As an alternative mode, these unsaturated Cu sites possessed acidic properties and sulfur compounds had weak basicity. Consequently, the adsorption desulfurization process may run through Lewis acid–base interactions [45]. There are also weak interactions such as π-π stacking, π-π interactions and Van der Waals forces between adsorbate molecules. These cumulative interactions with the strong chemical adsorption at the coordinatively unsaturated Cu sites acting as the primary anchor collectively justify the “multi-layer chemical adsorption” behavior.

4. Conclusions

In summary, a series of HKUST-1 samples have been rapidly prepared with different addition amounts of NH4F at room temperature. Under the conditions of that 50 mg HKUST-1-5 synthesized with the addition amount of 5wt% NH4F was used to adsorb 5 g of model oil with a sulfur concentration of 1000 ppm at 25 °C for 1 h, the adsorption capacity of the adsorbent reached 23.8 mgS/g, 46.8 mgS/g and 36.8 mgS/g for benzothiophene (BT), dibenzothiophene (DBT) and 4,6-dimethyldibenzothiophene (4,6-DMDBT), respectively, which exhibited enhanced adsorption desulfurization performance compared with conventional HKUST-1 prepared by the solvothermal method. The characterization results from various techniques suggested that such superior adsorption performance could be attributed to the existence of more defects and its smaller particle size. In addition, the recycling experiments demonstrate that HKUST-1-5 can maintain good adsorption desulfurization performance after several cycles. This work will pave a way to design and synthesize new highly efficient adsorbents for desulfurization of fuel oil.

Supplementary Materials

The following supporting information can be downloaded at: https://www.mdpi.com/article/10.3390/en18205344/s1, Figure S1: Pseudo-first-order kinetic fitting of adsorption desulfurization between HKUST-1-S and HKUST-1-5: (a) BT, (b) DBT, (c) 4,6-DMDBT; Figure S2: Pseudo-second-order kinetic fitting of adsorption desulfurization between HKUST-1-S and HKUST-1-5: (a) BT, (b) DBT, (c) 4,6-DMDBT; Figure S3: Langmuir model fitting of adsorption of different sulfur compounds by HKUST-1-S and HKUST-1-5: (a) BT, (b) DBT, (c) 4,6-DMDBT; Figure S4: Freundlich model fitting of adsorption of different sulfur compounds by HKUST-1-S and HKUST-1-5: (a) BT, (b) DBT, (c) 4,6-DMDBT; Figure S5: The SEM images of (a) HKUST-1-5 and (b) HKUST-1-S; Figure S6: (a) The N2 sorption and desorption isotherms and (b) the corresponding pore size distributions of HKUST-1-5 and HKUST-1-S; Figure S7: Adsorption desulfurization performance of HKUST-1-S and HKUST-1-5 for the removal of DBT; Figure S8: Non-linear pseudo-second-order kinetic fitting of adsorption desulfurization for HKUST-1-S and HKUST-1-5; Table S1: Comparison of pore structure parameters for HKUST-1-5 and HKUST-1-S.

Author Contributions

Writing—Original Draft, Experiments, Methodology, Investigation, J.F.; Writing—Review and Editing, Data Curation, X.L.; Writing—Review and Editing, Resources, Y.K.; Writing—Review and Editing, R.Z.; Writing—Review and Editing, Conceptualization, Methodology, Funding Acquisition, Supervision, Y.S. Writing—Review and Editing, Supervision, A.S.A.-E. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by the National Natural Science Foundation of China (No. 22172042).

Data Availability Statement

The original contributions presented in this study are included in the article or Supplementary Material. Further inquiries can be directed to the corresponding author.

Acknowledgments

The authors acknowledge the financial support from the National Natural Science Foundation of China (No. 22172042).

Conflicts of Interest

The authors declare no conflicts of interest.

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Energies 18 05344 g001
Figure 1. (a) XRD patterns; (b) FT-IR spectra of HKUST-1 prepared with different addition amounts of NH4F.
Figure 1. (a) XRD patterns; (b) FT-IR spectra of HKUST-1 prepared with different addition amounts of NH4F.
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Energies 18 05344 g002
Figure 2. (a) N2 sorption and desorption isotherms; (b) pore size distribution curves of HKUST-1 prepared with different addition amounts of NH4F.
Figure 2. (a) N2 sorption and desorption isotherms; (b) pore size distribution curves of HKUST-1 prepared with different addition amounts of NH4F.
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Energies 18 05344 g003
Figure 3. SEM images of HKUST-1 prepared with different addition amounts of NH4F: (a) 2.5%; (b) 5%; (c) 10%; (d) 15%.
Figure 3. SEM images of HKUST-1 prepared with different addition amounts of NH4F: (a) 2.5%; (b) 5%; (c) 10%; (d) 15%.
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Energies 18 05344 g004
Figure 4. The adsorption desulfurization performance of HKUST-1-x prepared with different addition amounts of NH4F for the removal of DBT in model fuel oil.
Figure 4. The adsorption desulfurization performance of HKUST-1-x prepared with different addition amounts of NH4F for the removal of DBT in model fuel oil.
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Energies 18 05344 g005
Figure 5. Adsorption desulfurization performance of HKUST-1-S and HKUST-1-5 for various sulfur compounds: (a) BT; (b) DBT; (c) 4,6-DMDBT.
Figure 5. Adsorption desulfurization performance of HKUST-1-S and HKUST-1-5 for various sulfur compounds: (a) BT; (b) DBT; (c) 4,6-DMDBT.
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Energies 18 05344 g006
Figure 6. Adsorption desulfurization isotherms of HKUST-1-S and HKUST-1-5 for various sulfur compounds: (a) BT; (b) DBT; (c) 4,6-DMDBT.
Figure 6. Adsorption desulfurization isotherms of HKUST-1-S and HKUST-1-5 for various sulfur compounds: (a) BT; (b) DBT; (c) 4,6-DMDBT.
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Energies 18 05344 g007
Figure 7. The adsorption desulfurization performance of HKUST-1-S and HKUST-1-5 in the presence or absence of 10% benzene in model oil.
Figure 7. The adsorption desulfurization performance of HKUST-1-S and HKUST-1-5 in the presence or absence of 10% benzene in model oil.
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Energies 18 05344 g008
Figure 8. (a) Reusability of HKUST-1-5; (b) XRD patterns; (c) N2 adsorption–desorption isotherms; (d) pore size distribution curves of HKUST-1-5 before and after adsorption.
Figure 8. (a) Reusability of HKUST-1-5; (b) XRD patterns; (c) N2 adsorption–desorption isotherms; (d) pore size distribution curves of HKUST-1-5 before and after adsorption.
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Energies 18 05344 g009
Figure 9. XPS spectra of HKUST-1-5 and HKUST-1-S: (a) full spectrum; (b) C 1s; (c) O 1s; (d) Cu 2p.
Figure 9. XPS spectra of HKUST-1-5 and HKUST-1-S: (a) full spectrum; (b) C 1s; (c) O 1s; (d) Cu 2p.
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Energies 18 05344 g010
Figure 10. TG curves of HKUST-1-5 and HKUST-1-S.
Figure 10. TG curves of HKUST-1-5 and HKUST-1-S.
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Energies 18 05344 g011
Figure 11. NH3-TPD curves of HKUST-1-5 and HKUST-1-S. To validate the adsorption mechanism.
Figure 11. NH3-TPD curves of HKUST-1-5 and HKUST-1-S. To validate the adsorption mechanism.
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Energies 18 05344 g012
Figure 12. FT-IR spectra of HKUST-1-5 before and after DBT adsorption.
Figure 12. FT-IR spectra of HKUST-1-5 before and after DBT adsorption.
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Energies 18 05344 g013
Figure 13. Schematic diagram showing adsorption desulfurization process of HKUST-1-5.
Figure 13. Schematic diagram showing adsorption desulfurization process of HKUST-1-5.
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Table 1. Nitrogen sorption data of HKUST-1-x materials.
Table 1. Nitrogen sorption data of HKUST-1-x materials.
SamplesBET Surface Area (m2/g)Micropore Volume (mL/g)Average Micropore Size (nm)
HKUST-1-2.59270.360.68
HKUST-1-515080.580.73
HKUST-1-105740.220.68
HKUST-1-152450.090.66
Table 2. Comparison of adsorption desulfurization performance of HKUST-1-5 with some reported MOFs.
Table 2. Comparison of adsorption desulfurization performance of HKUST-1-5 with some reported MOFs.
AdsorbentsSulfur CompoundsSulfur Concentration (ppm)Qe (mgS/g)References
MIL-53(Al)BT10004.5[26]
MIL-53(Cr)BT10009.5
MIL-47BT100021.5
MIL-53(Cr)-GDBT100086.4[27]
MIL-100(Fe)BT100014.3[28]
MIL-101(Cr)DBT10006.5[29]
Co-ZIF-67-MDBT5002.2[30]
UiO-66BT10019.8[31]
ZIF-8
UMCM-150		BT10006.6[32]
BT150040[7]
DBT150083
4,6-DMDBT60041
HKUST-1BT150025
DBT150045
4,6-DMDBT60016
HKUST-1-SBT100016.6This work
DBT100040.9
4,6-DMDBT100022.4
HKUST-1-5BT100023.8
DBT100046.8
4,6-DMDBT100036.8
Table 3. Pseudo-first-order kinetic parameters of adsorption desulfurization on HKUST-1-S and HKUST-1-5.
Table 3. Pseudo-first-order kinetic parameters of adsorption desulfurization on HKUST-1-S and HKUST-1-5.
AdsorbentsSulfur Compounds
BTDBT4,6-DMDBT
K1R2K1R2K1R2
HKUST-1-S0.08960.86120.10770.60820.00560.8910
HKUST-1-50.06790.41030.12810.80370.09360.6381
Table 4. Pseudo-second-order kinetic parameters of adsorption desulfurization on HKUST-1-S and HKUST-1-5.
Table 4. Pseudo-second-order kinetic parameters of adsorption desulfurization on HKUST-1-S and HKUST-1-5.
AdsorbentsSulfur Compounds
BTDBT4,6-DMDBT
K2R2K2R2K2R2
HKUST-1-S0.02740.99820.00840.99360.00560.9959
HKUST-1-50.02970.99770.00930.99530.00770.9939
Table 5. Langmuir model parameters of adsorption desulfurization.
Table 5. Langmuir model parameters of adsorption desulfurization.
AdsorbentsSulfur Compounds
BTDBT4,6-DMDBT
Qmax (mgS/g)R2Qmax (mgS/g)R2Qmax (mgS/g)R2
HKUST-1-S29.10.993156.80.988729.90.9854
HKUST-1-51250.996960.20.988545.70.9798
Table 6. Freundlich model parameters of adsorption desulfurization.
Table 6. Freundlich model parameters of adsorption desulfurization.
AdsorbentsSulfur Compounds
BTDBT4,6-DMDBT
KFnR2KFnR2KFnR2
HKUST-1-S0.2981.1680.99891.7912.0240.99451.2012.2810.9989
HKUST-1-50.0641.1200.99932.9392.2590.99952.9642.5760.9975
Table 7. Nitrogen sorption data of fresh and used HKUST-1-5.
Table 7. Nitrogen sorption data of fresh and used HKUST-1-5.
AdsorbentsBET Surface Area (m2/g)Micropore Volume (mL/g)Average Pore Size (nm)
Fresh HKUST-1-515080.580.73
Used HKUST-1-514500.510.71
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Fu, J.; Liu, X.; Kong, Y.; Zhao, R.; Sun, Y.; Abou-Elyazed, A.S. Enhancing the Adsorption Performance of HKUST-1 by Adding NH4F During Room-Temperature Synthesis for Desulfurization of Fuel Oil. Energies 2025, 18, 5344. https://doi.org/10.3390/en18205344

AMA Style

Fu J, Liu X, Kong Y, Zhao R, Sun Y, Abou-Elyazed AS. Enhancing the Adsorption Performance of HKUST-1 by Adding NH4F During Room-Temperature Synthesis for Desulfurization of Fuel Oil. Energies. 2025; 18(20):5344. https://doi.org/10.3390/en18205344

Chicago/Turabian Style

Fu, Jiawei, Xinchun Liu, Yuqing Kong, Ruyu Zhao, Yinyong Sun, and Ahmed S. Abou-Elyazed. 2025. "Enhancing the Adsorption Performance of HKUST-1 by Adding NH4F During Room-Temperature Synthesis for Desulfurization of Fuel Oil" Energies 18, no. 20: 5344. https://doi.org/10.3390/en18205344

APA Style

Fu, J., Liu, X., Kong, Y., Zhao, R., Sun, Y., & Abou-Elyazed, A. S. (2025). Enhancing the Adsorption Performance of HKUST-1 by Adding NH4F During Room-Temperature Synthesis for Desulfurization of Fuel Oil. Energies, 18(20), 5344. https://doi.org/10.3390/en18205344

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