Single [Ga(OH)]2+ species supported on mesoporous hollow-structured H-ZSM-5: A highly efficient light alkanes aromatization catalyst

doi:10.1016/S1872-2067(25)64678-X

Chinese Journal of Catalysis ›› 2025, Vol. 72: 359-375.DOI: 10.1016/S1872-2067(25)64678-X

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Single [Ga(OH)]²⁺ species supported on mesoporous hollow-structured H-ZSM-5: A highly efficient light alkanes aromatization catalyst

Dezhi Shi^a^,^b, Yanyan Chen^a, Xiao Chen^c, Sen Wang^a^,^*(), Qiang Wang^d, Pengfei Wang^a, Huaqing Zhu^a, Mei Dong^a, Jun Xu^d, Feng Deng^d, Jianguo Wang^a, Weibin Fan^a^,^*()

^aState Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, Shanxi, China
^bThe Cultivation Base of Shanxi Key Laboratory of Mining Area Ecological Restoration and Solid Wastes Utilization, Shanxi Institute of Technology, Yangquan 045000, Shanxi, China
^cBeijing Key Laboratory of Green Chemical Reaction Engineering and Technology, Department of Chemical Engineering, Tsinghua University, Beijing 100084, China
^dNational Center for Magnetic Resonance in Wuhan, State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Institute of Physics and Mathematics, Innovation Academy for Precision Measurement Science and Technology, Chinese Academy of Sciences, Wuhan 430071, Hubei, China

Received:2024-11-06 Accepted:2025-03-11 Online:2025-05-18 Published:2025-05-20
Contact: *E-mail: wangsen@sxicc.ac.cn (S. Wang), fanwb@sxicc.ac.cn (W. Fan).
Supported by:
National Key R&D Program of China(2023YFB4103700);National Key R&D Program of China(2020YFA0210900);National Key R&D Program of China(2020YFA0210902);National Key R&D Program of China(2020YFB0606402);National Natural Science Foundation of China(U1910203);National Natural Science Foundation of China(21991090);National Natural Science Foundation of China(21991092);National Natural Science Foundation of China(22322208);National Natural Science Foundation of China(22272195);National Natural Science Foundation of China(U22A20431);Natural Science Foundation of Shanxi Province of China(202203021224009);Natural Science Foundation of Shanxi Province of China(202303021222277);Scientific and Technological Innovation Programs of Higher Education Institutions in Shanxi(2021L586);China Postdoctoral Science Foundation(2022TQ0351);Innovation foundation of Institute of Coal Chemistry, Chinese Academy of Sciences(SCJC-DT-2023-06);Youth Innovation Promotion Association CAS(2021172)

Abstract

Abstract:

Aromatization of light alkanes is a value-added process in both petrochemical and coal chemical industries. Here, single [Ga(OH)]²⁺ ion-exchanged mesoporous hollow-structured ZSM-5 (Ga-MH-ZSM-5) material was prepared, and it shows unprecedented catalytic performance in light alkane aromatization, considering activity, product selectivity and catalytic stability. The average aromatics yields in ethane aromatization at 600 °C and WHSV of 0.8 h^-1 within 28 h and in propane aromatization at 580 °C and WHSV of 1.1 h^-1 within 20 h reach ’18.4% and ’70.8% with benzene, toluene and xylenes (BTX) accounting for ’96% and ’88% of aromatics, respectively. Ga-MH-ZSM-5-0.41 gave a TON for formation of aromatics (TON_aromatics) from propane as high as 57479, whereas the reported catalysts maximally show a TON_aromatics of 5514. This also holds true for ethane aromatization; the TON_aromatics obtained on Ga-MH-ZSM-5-0.41 was ≥ 3845 in contrast to £ 392 on reported non-noble metal catalysts. The catalytic activity of Ga-MH-ZSM-5 highly depends on Ga species structures. [Ga(OH)]²⁺ ions are predominant species at Ga loading ≤ 0.3 wt%, while more [Ga(OH)₂]⁺ and GaO_x oligomers are formed with increasing Ga content. Upon reduction with H₂, [Ga(OH)]²⁺ and [Ga(OH)₂]⁺ are transformed into [GaH]²⁺ and [GaH₂]⁺ species, which show a propane dehydrogenation rate of 300 and 15 times of that of Brønsted acid sites respectively. The light alkanes are mainly dehydrogenated into light olefins on [GaH]²⁺ species, and then, oligomerized and cyclized into (alkyl)cycloalkanes on H⁺ sites, which is followed by possible ring expansion on H⁺ and sequential dehydrogenations into aromatics primarily on [GaH]²⁺.

Key words: Light alkane aromatization, Mesoporous hollow-structured, H-ZSM-5, Isolated Ga species, Active site, Reaction mechanism

Dezhi Shi, Yanyan Chen, Xiao Chen, Sen Wang, Qiang Wang, Pengfei Wang, Huaqing Zhu, Mei Dong, Jun Xu, Feng Deng, Jianguo Wang, Weibin Fan. Single [Ga(OH)]²⁺ species supported on mesoporous hollow-structured H-ZSM-5: A highly efficient light alkanes aromatization catalyst[J]. Chinese Journal of Catalysis, 2025, 72: 359-375.

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Figures/Tables 9

Fig. 1. (a) Schematic illustration for the preparation of MH-ZSM-5. TEM images of parent ZSM-5 (b), HH-ZSM-5 (c) and MH-ZSM-5 (d) samples. (e,f) Aberration-corrected HAADF-STEM images (the generated mesopores are highlighted by yellow circles). iDPC-STEM image (the Ga species are highlighted by red circles) (g) and corresponding EDX elemental mappings (h-j) of Ga-MH-ZSM-5-0.41. STEM-HAADF images with EDS line scanning profiles of Ga/H-ZSM-5 (k), Ga/HH-ZSM-5 (l) and Ga/MH-ZSM-5 (m) samples.

Fig. 2. Propane conversion, product selectivity and aromatic product distribution with the time-on-stream (TOS) over Ga/H-ZSM-5 (a,b), Ga/HH-ZSM-5 (c,d) and Ga/MH-ZSM-5 (e,f) sample. Reaction conditions: 540 °C, 1 atm, WHSVpropane = 1.4 h-1 (N2/C3H8 = 2.5 (vol/vol)).

Fig. 3. Propane conversions, aromatics selectivities and yields (a), and aromatic product distributions (b) obtained on MH-ZSM-5 and Ga-MH-ZSM-5-x samples (reaction conditions: T = 540 °C, 1 atm, WHSVpropane = 0.96 h-1 and N2/C3H8 = 2.5 (vol/vol)). Propane conversion, product selectivity (c), and aromatic products distribution (d) with TOS obtained on the Ga-MH-ZSM-5-0.41 (reaction conditions: T = 580 °C, 1 atm, WHSVpropane = 1.1 h-1 and N2/C3H8 = 2.5 (vol/vol)). (e) Aromatics and BTX yields obtained on our synthesized and reported catalysts. (f) TONs (green and pink columns represent the catalytic results of various reported Ga and Zn catalysts respectively). Data in this work were obtained from Fig. S14(c) (540 °C and TOS of 100 h) and Fig. S10 (580 °C and TOS of 50 h). TON is the accumulated amount (moles) of generated aromatics per mole of Ga or Zn species, as obtained from the equation of TON = $\left[F_{\mathrm{C}_{3} \mathrm{H}_{8}} \times \int_{0}^{t} Y_{\text {aro }, t} d t\right] / \mathrm{n}_{\mathrm{M}}$, where FC3H8 is propane carbon molar flow rate; Yaro,t is instantaneous aromatics carbon molar yield at the time on stream of t; t is reaction time, and nM is the moles of Ga or Zn species of catalysts.

Fig. 4. (a) Normalized Ga K-edge XANES spectra collected at ambient temperature of Ga-MH-ZSM-5-0.082 (1), Ga-MH-ZSM-5-0.13 (2), Ga-MH-ZSM-5-0.30 (3), Ga-MH-ZSM-5-0.47 (4), Ga-MH-ZSM-5-0.70 (5), Ga-MH-ZSM-5-1.10 (6), Ga-MH-ZSM-5-1.62 (7) and β-Ga2O3 in the first-coordination shell. (b) The magnitudes of the k3-weighted Fourier-transformed Ga K-edge EXAFS spectra of Ga-MH-ZSM-5-x, Ga foil and β-Ga2O3 samples. (c) The wavelet transform of the k3-weighted EXAFS spectra of Ga-MH-ZSM-5-0.13, Ga-MH-ZSM-5-0.30, Ga-MH-ZSM-5-0.47, Ga-MH-ZSM-5-1.62, Ga foil and β-Ga2O3 samples. (d) 71Ga MAS NMR spectra of Ga-MH-ZSM-5-0.13, Ga-MH-ZSM-5-0.3, Ga-MH-ZSM-5-0.47 and Ga-MH-ZSM-5-1.6. (e) Optimized structures for ion-exchanging [Ga(OH)2]+ and [Ga(OH)]2+ cations in Ga-MH-ZSM-5. (f) Schematic illustrations of two or one Br?nsted protons exchanged with one Ga3+ cation to form [Ga(OH)]2+ and [Ga(OH)2]+, respectively. (g) Relationship between the content of Br?nsted protons exchanged with Ga3+ cations, as determined by comparing the bridged OH vibration band areas at 3610 cm-1 (IR) of Ga-MH-ZSM-x samples with that of MH-ZSM-5, and the Ga/Al ratio of Ga-MH-ZSM-5-x samples (black dotted lines refers to the faction of two Br?nsted H+ exchanged with one Ga3+ cations in total Br?nsted H+).

Fig. 5. Propane conversion (a) and products carbon molar selectivity (b,c) obtained on the Ga-MH-ZSM-5-0.3 at atmospheric pressure, propane partial pressure of 0.54 kPa, 500 °C and WHSVpropane of 1.18 h?1 (hollow circles represent the catalytic results obtained on the sample pretreated in N2 at 500 °C for 1 h after calcining in static air; hollow blocks and solid balls are the catalytic results on the samples pretreated at 500 °C for 5 min and 1 h in 10%H2/Ar respectively). (d) The ratios of the difference in carbon molar selectivity of propene to those of (aromatics + ethene) and aromatics every 40 min from TOS of 10 to 170 min on the Ga-MH-ZSM-5-0.3 pretreated at 500 °C for 1 h in N2. (e) In situ FTIR spectra obtained at 150 °C on the Ga-MH-ZSM-5-0.15, Ga-MH-ZSM-5-0.25, Ga-MH-ZSM-5-0.38 and Ga-MH-ZSM-5-0.41 samples treated at 500 °C for 1 h in 10% H2/Ar (background spectrum was collected at 150 °C after the self-supported sample wafer was dehydrated at 500 °C and 7 × 10?3 Pa for 1 h).

Fig. 6. (a) Proposed alkyl mechanism for propane dehydrogenation over [GaH]2+ cations. (b) Dependence of the apparent propane dehydrogenation rate coefficients on Ga-MH-ZSM-5-x samples, and for comparison and on parent MH-ZSM-5, on the Ga contents in the samples; calculated free energy profiles for propane dehydrogenation via alkyl mechanism on [GaH]2+ (c) and [GaH2]+ (d) at 500 °C.

Fig. 7. Reaction network for propane aromatization. The blue data are calculated free energy barriers (kJ/mol) of various elemental steps on MH-ZSM-5 (a) and Ga-MH-ZSM-5-0.3 (b) DH, CR, O, C, HT and RE represent dehydrogenation, cracking, oligomerization, cyclization, hydrogen transfer and ring expansion reactions, respectively.

Fig. 8. GC-MS chromatograms of effluents on MH-ZSM-5 (a) and Ga-MH-ZSM-5-0.3 (b) in temperature-dependent propene conversion probe experiments. Reaction conditions: the temperature was ramped from room temperature to 440 °C at a rate of 5 °C/min in a (propene (1 mL/min) and N2 (160 mL/min)) gaseous mixture flow. The reaction was conducted in a U-type quartz tube micro-reactor loaded 20 mg catalyst. The gaseous products were collected for 30 s with a gas sample bag each time and analyzed by GC-MS.

Fig. 9. PTR-TOF-MS results for the formation of various cyclic hydrocarbon intermediates and aromatic products in temperature-programmed surface reaction of propane on MH-ZSM-5 (a-c) and Ga-MH-ZSM-5-0.3 (d-f).

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Single [Ga(OH)]²⁺ species supported on mesoporous hollow-structured H-ZSM-5: A highly efficient light alkanes aromatization catalyst

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