Water interactions in molecular sieve catalysis: Framework evolution and reaction modulation

doi:10.1016/S1872-2067(25)64828-5

Chinese Journal of Catalysis ›› 2025, Vol. 79: 9-31.DOI: 10.1016/S1872-2067(25)64828-5

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Water interactions in molecular sieve catalysis: Framework evolution and reaction modulation

Linhai He^a^,^b^,¹, Caiyi Lou^a^,^b^,¹, Lu Sun^a^,^b, Jing Niu^a, Shutao Xu^a^,^b^,^*(), Yingxu Wei^a^,^b, Zhongmin Liu^a^,^b^,^*()

^aNational Engineering Research Center of Lower-Carbon Catalysis Technology, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^bUniversity of Chinese Academy of Sciences, Beijing 100049, China

Received:2025-06-27 Accepted:2025-08-10 Online:2025-12-18 Published:2025-10-27
Contact: Shutao Xu, Zhongmin Liu
About author:Shutao Xu (Dalian Institute of Chemical Physics, Chinese Academy of Science) received his B.S. degree from Fudan University (P. R. China) in 2004, and PhD from Dalian Institute of Chemical Physics (DICP), Chinese Academy of Sciences (CAS) in 2011. Then he joined Prof. Zhongmin Liu’s team at National Engineering Research Center of Lower-Carbon Catalysis Technology, DICP as a research assistant. He became a professor in 2017. His research interests are the developments various of solid-state Nuclear Magnetic Resonance Spectroscopy (ssNMR) methods, including in-situ/operando techniques, 2D ssNMR spectroscopy, Hyperpolarized (HP) ¹²⁹Xe and Pulse Field Gradient (PFG) NMR, as well as applying these advanced NMR methods to the study of the structure, acidity and reaction mechanism of catalytic materials. He has published more than 100 peer-reviewed papers.
Zhongmin Liu (Dalian Institute of Chemical Physics, Chinese Academy of Science) is the Director of Dalian Institute of Chemical Physics (DICP), Chinese Academy of Sciences (CAS) since 2017. He has long been working with the catalysis research, process development, and technology transfer in energy conversion and utilization, and made significant achievements. Prof. Liu led his team to successfully commercialize two of the most representative industrial processes, methanol to olefins (MTO) and methanol to ethanol (MTE), in 2010 and 2017 respectively, which are important advances in coal to chemicals. He has published more than 430 research papers and got 600 authorized patents or more.
¹Contributed equally to this work.
Supported by:
National Key R&D Program of China(2022YFE0116000);National Natural Science Foundation of China(22241801);National Natural Science Foundation of China(22288101);National Natural Science Foundation of China(22022202);National Natural Science Foundation of China(22032005);National Natural Science Foundation of China(21991090);National Natural Science Foundation of China(21991092);National Natural Science Foundation of China(21991093);Dalian Outstanding Young Scientist Foundation(2021RJ01);Liaoning International Joint Laboratory Project(2024JH2/102100005)

Abstract

Abstract:

Porous molecular sieve catalysts, including aluminosilicate zeolites and silicoaluminophosphate (SAPO) molecular sieves, have found widespread use in heterogeneous catalysis and are expected to play a key role in advancing carbon neutrality and sustainable development. Given the ubiquitous presence of water during catalyst synthesis, storage, and application, the interactions between water and molecular sieves as well as their consequent effects on frameworks and catalytic reactions have attracted considerable attention. These effects are inherently complex and highly dependent on various factors such as temperature, water phase, and partial pressure. In this review, we provide a comprehensive overview of the current understanding of water-molecular sieve interactions and their roles in catalysis, based on both experimental and theoretical calculation results. Special attention is paid to water-induced reversible and irreversible structural changes in aluminosilicate and SAPO frameworks at the atomic level, underscoring the dynamic and labile nature of these frameworks in water environments. The influence of water on catalytic performance and reaction kinetics in molecular sieve-catalyzed reactions is discussed from two perspectives: (1) its participation in reaction through hydrogen bonding interactions, such as competitive adsorption at active sites, stabilization of ground and transition states, and proton transfer bridge; (2) its role as a direct reactant forming new species via reactions with other guest molecules. Recent advancements in this area provide valuable insights for the rational design and optimization of catalysts for water-involved reactions.

Key words: Water, Molecular sieves, Host-guest interactions, Molecular sieve catalysis, Water-assisted/inhibited catalysis

Linhai He, Caiyi Lou, Lu Sun, Jing Niu, Shutao Xu, Yingxu Wei, Zhongmin Liu. Water interactions in molecular sieve catalysis: Framework evolution and reaction modulation[J]. Chinese Journal of Catalysis, 2025, 79: 9-31.

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Figures/Tables 14

Fig. 1. Schematic illustration of water-induced structural changes in molecular sieve frameworks, with interaction strengths varying from weak to strong, encompassing water adsorption and reversible or irreversible hydrolysis of framework T-O-T bonds.

Fig. 2. (a) DFT-optimized structures of Br?nsted acid sites in H-MFI zeolite at varying water/BAS ratios. Reprinted with permission from Ref. [24]. Copyright 2017, American Chemical Society. Exponential decay of the enthalpic contributions (b) and linear decay (c) of the entropic contributions to the generation of the hydrated hydronium ion on BAS in various zeolite frameworks (GIS, MFI, CHA, FAU). Reprinted with permission from Ref. [28]. Copyright 2021, Springer Nature. (d) Gas-phase water adsorption isotherm at 298 K for H-MFI zeolites of varying Si/Al ratios. (e) Heat of water adsorption on H-MFI zeolites at varying water/BAS ratios. (f) Schematic of species distribution (hydronium ion clusters and cyclohexanol) within H-MFI micropores before, during partial adsorption, and upon saturation of cyclohexanol. (g) The volume occupied by hydronium ion clusters in H-MFI micropores at saturated adsorption of cyclohexanol and phenol. Reprinted with permission from Ref. [35]. Copyright 2019, John Wiley and Sons.

Fig. 3. (a) 17O MQMAS NMR spectra with 1H decoupling at 14.1 T of SSZ-13/H217O slurry (25 μL/25 mg) aged 1?h at room temperature. The asterisk (*) denotes the H217O(l) signal. Reprinted with permission from Ref. [42]. Copyright 2019, Springer Nature. 17O MAS (b) and isotropic projections (c) of MQMAS NMR spectra at 14.1 T of H-MOR/H217O slurry (50 μL/50 mg) recorded after different aging durations. The spectra are normalized. Reprinted with permission from Ref. [43]. Copyright 2019, American Chemical Society.

Fig. 4. (a) Encapsulation of TMP and pyridine molecules into CHA cavities via reversible cleavage and reformation of T-O-T bonds under mild hydrothermal conditions. (b) Chemisorbed pyridine content in SAPO-34 with and without water at 100-300 °C. (c) 2D 1H-31P HETCOR NMR spectrum of TMP-SAPO-34-300HT recorded with a contact time of 3 ms. (d) CHA crystal structure. (e) Selectivity of ethene and light olefins during methanol conversion over fresh SAPO-34, Py-SAPO-34-200HT, and TMP-SAPO-34-300HT, the latter two prepared via hydrothermal encapsulation of pyridine at 200?°C or TMP at 300?°C, respectively. Reprinted with permission from Ref. [21]. Copyright 2020, John Wiley and Sons.

Fig. 5. Schematic illustration of dealumination and desilication processes induced by attack of a single H2O molecule (a,b) or two H2O molecules (c). PT and BB in (c) represent proton transfer and Al-O(H) bond breaking, respectively. Reprinted with permission from Ref. [66,68,70]. Copyright 2012, John Wiley and Sons. Copyright 2016, Elsevier. Copyright 2019, American Chemical Society.

Fig. 6. (a) Free energy diagram of H-SSZ-13 dealumination for the single-water (grey) and multi-water (blue) pathways, calculated using DFT-MD umbrella simulations. Insets show the corresponding transition states. Reprinted with permission from Ref. [71]. Copyright 2019, Royal Society of Chemistry. (b) Correlation between the broken Al-O bonds and activation energies (Ea) in adsorption states. Reprinted with permission from Ref. [63]. Copyright 2020, American Chemical Society.

Fig. 7. (a) 27Al{1H} D-HMQC spectra of dehydrated H-ZSM-5 (Si/Al = 15) acquired at 19.6 T. The signal regions labeled ii arise from Al(IV)-1 species, while those labeled i, iii, and iv arise from Al(IV)-2 species and its associated hydroxyl groups. (b) Schematic diagram of the structures of Al(IV)-1 and Al(IV)-2 species. (c) 27Al MQMAS spectra of dehydrated H-ZSM-5 (Si/Al = 15) recorded at 19.6 T before AHFS washing and (d) after AHFS washing. Reprinted with permission from Ref. [73]. Copyright 2021, American Chemical Society.

Fig. 8. (a) 27Al MQMAS (left) and 1H{27Al} MQ-D-RINEPT (right) spectra of dehydrated Na/H-Y cal923 zeolite (calcined at 923 K in air). (b) 1H{27Al} MQ-D-RINEPT spectra of dehydrated H-Y cal923 (calcined at 923 K in air) after pyridine-d5 adsorption. All spectra were recorded at 18.8 T. (c) Proposed zeolite dealumination mechanism. Reprinted with permission from Ref. [77]. Copyright 2024, American Chemical Society.

Fig. 9. Schematic illustration of desilication mechanisms induced by attack of a single H2O molecule (a,b) or two H2O molecules (c), and silicon island formation (d) via sequential Si/P and Si/Al exchanges within the SAPO structure. Reprinted with permission from Ref. [97-99]. Copyright 2013, American Chemical Society. Copyright 2015, American Chemical Society. Copyright 2015, American Chemical Society.

Fig. 10. (a,b) SAPO-34 loaded with methanol-water mixture (5:0 and 1:4 per BAS) at 330 °C and around ambient pressure. (x:y)mw,sim indicates x MeOH and y H2O molecules per BAS in the simulation. (c) Induction times of single H-SAPO-34 crystals was monitored via in-situ UV-vis microspectroscopy as a function of water content. Optical images and UV-vis spectra of single SAPO-34 crystals during MTO with methanol-water ratios of 1:0 (d), 1:4 (e), and 1:12 (f); showing proression from induction period (green) to aromatic formation (blue) and deactivation (black). Reprinted with permission from Ref. [102]. Copyright 2016, American Chemical Society. (g) Conversion of TRI (XTRI) during OME synthesis over H-beta zeolite at varying water contents in OME1 (T = 30 °C, 0.5 wt% catalyst, OME1:TRI = 3.3). (h) Schematic illustration of the proposed mechanism of water inhibition during OME synthesis over H-Beta zeolite. Reprinted with permission from Ref. [112]. Copyright 2020, American Chemical Society.

Fig. 11. (a) Schematic illustrating water driving benzene toward the surface methoxy species (SMS) to form the active SMS-benzene complex, promoting benzene methylation. Reprinted with permission from Ref. [13]. Copyright 2023, John Wiley and Sons. (b) Effects of water co-feeding on ethene conversion over H-ZSM-5 zeolite at 300 and 350 °C. Insets depict the density distributions of ethene and water around the BASs in H-ZSM-5 zeolite at both temperatures. The red and bluish clouds illustrate the adsorption probability distributions of water and ethene molecules, respectively. Reprinted with permission from Ref. [110]. Copyright 2020, American Chemical Society. (c) In the MTH reaction catalyzed by H-ZSM-5, the spatial distribution of hydrophilic cyclopentenyl cations, key intermediates, within the fixed-bed reactor generates a gradient distribution of adsorbed water along the axial positions, and the adsorbed water promotes the conversion of cyclopentenyl cations to aromatic compounds. Reprinted with permission from Ref. [117]. Copyright 2024, American Chemical Society.

Fig. 12. (a) Unit cell-normalized concentrations of H3O+hydr. (triangles) and ionic strength (circles) as a function of BAS concentration. (b) Reaction steps and energy profiles for cyclohexanol dehydration catalyzed by H3O+hydr. in H-MFI zeolite under ideal and nonideal aqueous conditions. (c) Reaction free-energy barriers and excess chemical potential (μexcess) of the ground state (GS) and transition state (TS) under the ideal condition and under an ionic strength. (d) TOF as a function of ionic strength under the catalysis of HCl (black) at 453 K and H-MFI (orange) at 423 K. (e) Schematic of H3O+hydr. and cyclohexanol in H-MFI micropore channels. (f) GS and TS enthalpies as a function of the mean distance (db-b) and volume (Vb-b) between the boundaries of neighboring H3O+hydr.. Reprinted with permission from Ref. [14]. Copyright 2021, American Association for the Advancement of Science (AAAS).

Fig. 13. (a) DFT-simulated methanol-to-olefins catalytic cycle via 1,4-DiMN over SAPO-34, showing Gibbs free energies and rate constants in the absence (black) and presence (red) of water at 773 K. (b) Optimized structures of the IM1 reactant without water and with water assistance. Reprinted with permission from Ref. [12]. Copyright 2024, Elsevier. (c) H2O-assisted proton transfer route over a dicopper [Cu]+-[Cu]+ site in Cu-BEA. (d) CH3OH productivities of Cu-BEA with different Cu loadings during N2O-DMTM in the presence (red) and absence (black) of H2O; reaction conditions: N2O:CH4:H2O:He = 30:15:10(0):45(55), GHSV = 12000 h-1, T = 320 °C. (e) Product selectivity of Cu-BEA-0.6% after 70 h of testing at 320 °C with and without H2O. Reprinted with permission from Ref. [125]. Copyright 2021, John Wiley and Sons.

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Water interactions in molecular sieve catalysis: Framework evolution and reaction modulation

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