On the synthesis of vanadium containing molecular sieves by experimental design from a VOSO4·5H2O·Al(iPrO)3·Pr2NH·H2O gel: Occurrence of VAPO-41 as a secondary structure in the synthesis of VAPO-11

Ligia Frunza; Pascal Van Der Voort; Etienne F. Vansant; Robert A. Schoonheydt; Bert M. Weckhuysen

doi:10.1016/S1387-1811(00)00225-0

On the synthesis of vanadium containing molecular sieves by experimental design from a VOSO₄·5H₂O·Al(iPrO)₃·Pr₂NH·H₂O gel: Occurrence of VAPO-41 as a secondary structure in the synthesis of VAPO-11

Ligia Frunza
, Pascal Van Der Voort
, Etienne F. Vansant
, Robert A. Schoonheydt
, Bert M. Weckhuysen^*

^*Corresponding author for this work

Research output: Contribution to journal › Article › Academic › peer-review

Abstract

An experimental design was applied to the hydrothermal synthesis of VAPO-11 molecular sieve (AEL structure) from a VOSO₄·5H₂O·Al(iPrO)₃·Pr₂NH·H₂O gel. The influence of five synthesis parameters (synthesis temperature, synthesis time, vanadium content, water content and template content) on the crystallinity and physicochemical properties of the as-synthesized materials was studied. The obtained materials were characterized by electron spin resonance (ESR), diffuse reflectance spectroscopy (DRS), X-ray diffraction, thermal analysis measurements, scanning electron microscopy and in situ Fourier transform infrared (FTIR) spectroscopy. The AEL structure appears either as a single phase or as a physical mixture together with the AFO structure (VAPO-41). A statistical model is proposed, which relates the synthesis variables with the crystallinity allowing to indicate the optimal synthesis conditions for VAPO-11. Highly crystalline single-phase VAPO-11 can be best prepared at 170°C from a synthesis gel with a low vanadium content (0.02 mol) and a high water content (25 mol). The co-ordination of vanadium in these materials is discussed on the basis of the ESR and DRS spectra. The spectroscopic data are explained by the presence of a vanadium species in distorted octahedral co-ordination, composed of two V-O-T bonds with the framework, one bond with the vanadyl oxygen and three water molecules as ligands. (C) 2000 Elsevier B.V. All rights reserved.

Original language	English
Pages (from-to)	493-507
Number of pages	15
Journal	Microporous and Mesoporous Materials
Volume	39
Issue number	3
DOIs	https://doi.org/10.1016/S1387-1811(00)00225-0
Publication status	Published - Oct 2000
Externally published	Yes

Funding

The authors acknowledge financial support from the Flemish Community under the bilateral agreement BIL 22/96 with Romania as well as from the Fonds voor Wetenschappelijk Onderzoek-Vlaanderen (FWO) and the Geconcerteerde Onderzoeksacties (GOA). B.M.W. and P.V.D.V. acknowledge the FWO for postdoctoral fellowships. The authors thank Hugo Leeman for technical assistance and Fina Pelgrims for preparing the scanning electron micrographs. Spectral optimization software was provided by the Illinois ESR Research Center, NIH Division of research, grant RR01811, that includes the algorithm developed by Mattson et al. [30] .

Keywords

Experimental design
Synthesis and characterization
VAPO-11
VAPO-41

Access to Document

10.1016/S1387-1811(00)00225-0

Cite this

Frunza, L., Voort, P. V. D., Vansant, E. F., Schoonheydt, R. A., & Weckhuysen, B. M. (2000). On the synthesis of vanadium containing molecular sieves by experimental design from a VOSO₄·5H₂O·Al(iPrO)₃·Pr₂NH·H₂O gel: Occurrence of VAPO-41 as a secondary structure in the synthesis of VAPO-11. Microporous and Mesoporous Materials, 39(3), 493-507. https://doi.org/10.1016/S1387-1811(00)00225-0

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title = "On the synthesis of vanadium containing molecular sieves by experimental design from a VOSO4·5H2O·Al(iPrO)3·Pr2NH·H2O gel: Occurrence of VAPO-41 as a secondary structure in the synthesis of VAPO-11",

abstract = "An experimental design was applied to the hydrothermal synthesis of VAPO-11 molecular sieve (AEL structure) from a VOSO4·5H2O·Al(iPrO)3·Pr2NH·H2O gel. The influence of five synthesis parameters (synthesis temperature, synthesis time, vanadium content, water content and template content) on the crystallinity and physicochemical properties of the as-synthesized materials was studied. The obtained materials were characterized by electron spin resonance (ESR), diffuse reflectance spectroscopy (DRS), X-ray diffraction, thermal analysis measurements, scanning electron microscopy and in situ Fourier transform infrared (FTIR) spectroscopy. The AEL structure appears either as a single phase or as a physical mixture together with the AFO structure (VAPO-41). A statistical model is proposed, which relates the synthesis variables with the crystallinity allowing to indicate the optimal synthesis conditions for VAPO-11. Highly crystalline single-phase VAPO-11 can be best prepared at 170°C from a synthesis gel with a low vanadium content (0.02 mol) and a high water content (25 mol). The co-ordination of vanadium in these materials is discussed on the basis of the ESR and DRS spectra. The spectroscopic data are explained by the presence of a vanadium species in distorted octahedral co-ordination, composed of two V-O-T bonds with the framework, one bond with the vanadyl oxygen and three water molecules as ligands. (C) 2000 Elsevier B.V. All rights reserved.",

keywords = "Experimental design, Synthesis and characterization, VAPO-11, VAPO-41",

author = "Ligia Frunza and Voort, \{Pascal Van Der\} and Vansant, \{Etienne F.\} and Schoonheydt, \{Robert A.\} and Weckhuysen, \{Bert M.\}",

year = "2000",

month = oct,

doi = "10.1016/S1387-1811(00)00225-0",

language = "English",

volume = "39",

pages = "493--507",

journal = "Microporous and Mesoporous Materials",

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Frunza, L, Voort, PVD, Vansant, EF, Schoonheydt, RA & Weckhuysen, BM 2000, 'On the synthesis of vanadium containing molecular sieves by experimental design from a VOSO₄·5H₂O·Al(iPrO)₃·Pr₂NH·H₂O gel: Occurrence of VAPO-41 as a secondary structure in the synthesis of VAPO-11', Microporous and Mesoporous Materials, vol. 39, no. 3, pp. 493-507. https://doi.org/10.1016/S1387-1811(00)00225-0

On the synthesis of vanadium containing molecular sieves by experimental design from a VOSO₄·5H₂O·Al(iPrO)₃·Pr₂NH·H₂O gel: Occurrence of VAPO-41 as a secondary structure in the synthesis of VAPO-11. / Frunza, Ligia; Voort, Pascal Van Der; Vansant, Etienne F. et al.
In: Microporous and Mesoporous Materials, Vol. 39, No. 3, 10.2000, p. 493-507.

Research output: Contribution to journal › Article › Academic › peer-review

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T1 - On the synthesis of vanadium containing molecular sieves by experimental design from a VOSO4·5H2O·Al(iPrO)3·Pr2NH·H2O gel

T2 - Occurrence of VAPO-41 as a secondary structure in the synthesis of VAPO-11

AU - Frunza, Ligia

AU - Voort, Pascal Van Der

AU - Vansant, Etienne F.

AU - Schoonheydt, Robert A.

AU - Weckhuysen, Bert M.

PY - 2000/10

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N2 - An experimental design was applied to the hydrothermal synthesis of VAPO-11 molecular sieve (AEL structure) from a VOSO4·5H2O·Al(iPrO)3·Pr2NH·H2O gel. The influence of five synthesis parameters (synthesis temperature, synthesis time, vanadium content, water content and template content) on the crystallinity and physicochemical properties of the as-synthesized materials was studied. The obtained materials were characterized by electron spin resonance (ESR), diffuse reflectance spectroscopy (DRS), X-ray diffraction, thermal analysis measurements, scanning electron microscopy and in situ Fourier transform infrared (FTIR) spectroscopy. The AEL structure appears either as a single phase or as a physical mixture together with the AFO structure (VAPO-41). A statistical model is proposed, which relates the synthesis variables with the crystallinity allowing to indicate the optimal synthesis conditions for VAPO-11. Highly crystalline single-phase VAPO-11 can be best prepared at 170°C from a synthesis gel with a low vanadium content (0.02 mol) and a high water content (25 mol). The co-ordination of vanadium in these materials is discussed on the basis of the ESR and DRS spectra. The spectroscopic data are explained by the presence of a vanadium species in distorted octahedral co-ordination, composed of two V-O-T bonds with the framework, one bond with the vanadyl oxygen and three water molecules as ligands. (C) 2000 Elsevier B.V. All rights reserved.

AB - An experimental design was applied to the hydrothermal synthesis of VAPO-11 molecular sieve (AEL structure) from a VOSO4·5H2O·Al(iPrO)3·Pr2NH·H2O gel. The influence of five synthesis parameters (synthesis temperature, synthesis time, vanadium content, water content and template content) on the crystallinity and physicochemical properties of the as-synthesized materials was studied. The obtained materials were characterized by electron spin resonance (ESR), diffuse reflectance spectroscopy (DRS), X-ray diffraction, thermal analysis measurements, scanning electron microscopy and in situ Fourier transform infrared (FTIR) spectroscopy. The AEL structure appears either as a single phase or as a physical mixture together with the AFO structure (VAPO-41). A statistical model is proposed, which relates the synthesis variables with the crystallinity allowing to indicate the optimal synthesis conditions for VAPO-11. Highly crystalline single-phase VAPO-11 can be best prepared at 170°C from a synthesis gel with a low vanadium content (0.02 mol) and a high water content (25 mol). The co-ordination of vanadium in these materials is discussed on the basis of the ESR and DRS spectra. The spectroscopic data are explained by the presence of a vanadium species in distorted octahedral co-ordination, composed of two V-O-T bonds with the framework, one bond with the vanadyl oxygen and three water molecules as ligands. (C) 2000 Elsevier B.V. All rights reserved.

KW - Experimental design

KW - Synthesis and characterization

KW - VAPO-11

KW - VAPO-41

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DO - 10.1016/S1387-1811(00)00225-0

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