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Effect of silica/alumina ratio and structure-directing agent on the physical and chemical properties of SAPO-34

  • Original Paper: Industrial and technological applications of sol-gel and hybrid materials
  • Published:
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Abstract

This work describes how the silica/alumina ratio (SAR) affects the framework, texture, chemical composition, and acidity of SAPO-34 molecular sieves synthesized via hydrothermal crystallization using morpholine (MOR) or triethylamine (TEA) as structure-directing agents (SDA’s). The solids were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), N2 adsorption-desorption isotherms, thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FT-IR), X-ray fluorescence spectrometry (XRF), silicon-29 MAS NMR spectroscopy (29Si MAS NMR), aluminum-27 MAS NMR spectroscopy (27Al MAS NMR), and temperature-programmed desorption of ammonia (NH3-TPD). The solids synthesized in this work had crystalline phases, vibrational modes, and morphology characteristics of silicoaluminophosphate (SAPO) materials. Pure SAPO-34 was obtained only with morpholine, while SAPO-18/34 was crystallized with TEA. The SAPO-34 synthesized with MOR had the higher relative crystallinity and incorporation of Si into the framework. The SAPO-18/34 prepared with TEA had the larger surface areas. The solids prepared with SAR 0.3 had only Si(4Al) coordination, independently of the SDA used. The SAPO-34 synthesized with MOR and SAR 0.6 had the highest total acidity (9.75 μmol NH3 m−2).

SAPO molecular sieves were synthesized hydrothermally with different structure-directing agents and silica/alumina ratios. The effects of both variables on the physical and chemical properties of the samples obtained were evaluated. Pure SAPO-34 was obtained with morpholine, while SAPO-18/34 was crystallized with TEA. The SP34T-0.6 sample prepared with triethylamine and SAR 0.6 showed promising characteristics for use as catalyst in MTO reactions: AEI/CHA intergrowths, the lowest acidity, the smallest crystallite size, and a large BET surface area.

Highlights

  • Simultaneous effects of SAR and MOR or TEA on the SAPO-34 properties were studied.

  • SAPO-34 synthesized with morpholine (MOR) had the higher relative crystallinity.

  • AEI/CHA intergrowths were synthesized with triethylamine (TEA) and had the larger surface areas.

  • SAPO prepared with a silica/alumina ratio (SAR) of 0.3 had only the Si(4Al).

  • The SAPO-18/34 synthesized with TEA and SAR 0.6 had the lowest total acidity.

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Data availability

The data that support the results of this study are available on request to the corresponding author, GPV.

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Acknowledgements

The authors acknowledge the financial support for this research by the Foundation for Research Support of the State of Amazonas (FAPEAM) and the Coordination for the Improvement of Higher Education Personnel (CAPES).

Funding

Foundation for Research Support of the State of Amazonas (FAPEAM) and Coordination for the Improvement of Higher Education Personnel (CAPES).

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Authors and Affiliations

  1. Laboratory for the Study of Adsorptive and Catalytic Processes (LEPAC), School of Chemical Engineering, University of Campinas (UNICAMP), P.O. Box 6066, Campinas, SP, 13083-970, Brazil

    William Lima dos Anjos & Gustavo Paim Valença

  2. Food Engineering Department, Federal University of Tocantins (UFT), Palmas, TO, 77001-090, Brazil

    Sergio Andres Villalba Morales

  3. Laboratory of Chemical Reaction Engineering (LERC), Engineering Department, Federal University of Lavras (UFLA), Lavras, MG, 37200-000, Brazil

    Natália Maira Braga Oliveira

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  1. William Lima dos Anjos
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  2. Sergio Andres Villalba Morales
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  3. Natália Maira Braga Oliveira
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WLA and GPV provided the idea for the research. All authors wrote, read, and approved the final manuscript.

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Correspondence to Gustavo Paim Valença.

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dos Anjos, W.L., Morales, S.A.V., Oliveira, N.M.B. et al. Effect of silica/alumina ratio and structure-directing agent on the physical and chemical properties of SAPO-34. J Sol-Gel Sci Technol 100, 466–476 (2021). https://doi.org/10.1007/s10971-021-05669-w

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