Synthesis and physico-chemical characterization of Beta zeolite catalysts: Evaluation of catalytic properties in Prins cyclization of (−)-isopulegol

Anna O. Zaykovskaya; Narendra Kumar; Ekaterina A. Kholkina; Nikolai S. Li-Zhulanov; Päivi Mäki-Arvela; Atte Aho; Janne Peltonen; Markus Peurla; Ivo Heinmaa; Bright T. Kusema; Stéphane Streiff; Dmitry Yu. Murzin

doi:10.1016/j.micromeso.2020.110236

Synthesis and physico-chemical characterization of Beta zeolite catalysts: Evaluation of catalytic properties in Prins cyclization of (−)-isopulegol

Anna O. Zaykovskaya
, Narendra Kumar
, Ekaterina A. Kholkina
, Nikolai S. Li-Zhulanov
, Päivi Mäki-Arvela
, Atte Aho
, Janne Peltonen
, Markus Peurla
, Ivo Heinmaa
, Bright T. Kusema
, Stéphane Streiff
, Dmitry Yu. Murzin^*

^*Corresponding author for this work

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

13 Citations (Scopus)

129 Downloads (Pure)

Abstract

Synthesis of Beta zeolite catalysts was carried out using two different methods. The influence of such parameters as synthesis time and temperature, gel composition and gel ripening on the physico-chemical and catalytic properties of Beta zeolite catalysts was studied. A range of analytical methods was applied in this work including scanning and transmission electron microscopies, energy dispersive X-ray spectroscopy, X-ray powder diffraction, nuclear magnetic resonance spectroscopy – ²⁷A1-MAS-NMR and ²⁹Si-MAS-NMR, nitrogen physisorption, Fourier transform infrared spectroscopy and inductively coupled plasma optical emission spectrometry. The sodium forms of Beta zeolites were transformed to the proton forms H-Beta by ion-exchange using aqueous solutions of NH₄NO₃ and thereafter evaluated in Prins cyclization of (−)-isopulegol with benzaldehyde. The best catalyst synthesized at 150 °C in the rotation mode for 17 h possessing an optimal combination of morphological and structural properties as well as concentration of acid sites demonstrated high (−)-isopulegol conversion (93%) along with high selectivity to the desired product (79%).

Original language	English
Article number	110236
Number of pages	13
Journal	Microporous and Mesoporous Materials
Volume	302
DOIs	https://doi.org/10.1016/j.micromeso.2020.110236
Publication status	Published - 1 Aug 2020
MoE publication type	A1 Journal article-refereed

Funding

Solvay is gratefully acknowledged for funding. The research visit of Nikolai Li-Zhulanov to Åbo Akademi University was supported by the EDUFI Fellowship programme, funded by the Finnish National Agency for Education . Ivo Heinmaa has been supported by the Estonian Science Council Grant IUT23-7 and the European Regional Development Fund Grant TK134 .

Keywords

Beta zeolites
Catalyst synthesis
Catalytic materials
Characterization
Prins cyclization

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10.1016/j.micromeso.2020.110236

Synthesis and physico-chemical characterization of Beta zeolite catalysts: Evaluation of catalytic properties in Prins cyclization of (−)-isopulegolAccepted author manuscript, 2.05 MBLicence: CC BY-NC-ND

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Zaykovskaya, A. O., Kumar, N., Kholkina, E. A., Li-Zhulanov, N. S., Mäki-Arvela, P., Aho, A., Peltonen, J., Peurla, M., Heinmaa, I., Kusema, B. T., Streiff, S., & Murzin, D. Y. (2020). Synthesis and physico-chemical characterization of Beta zeolite catalysts: Evaluation of catalytic properties in Prins cyclization of (−)-isopulegol. Microporous and Mesoporous Materials, 302, Article 110236. https://doi.org/10.1016/j.micromeso.2020.110236

@article{4e3db790ab104cddabe023c5052e2bbe,

title = "Synthesis and physico-chemical characterization of Beta zeolite catalysts: Evaluation of catalytic properties in Prins cyclization of (−)-isopulegol",

abstract = "Synthesis of Beta zeolite catalysts was carried out using two different methods. The influence of such parameters as synthesis time and temperature, gel composition and gel ripening on the physico-chemical and catalytic properties of Beta zeolite catalysts was studied. A range of analytical methods was applied in this work including scanning and transmission electron microscopies, energy dispersive X-ray spectroscopy, X-ray powder diffraction, nuclear magnetic resonance spectroscopy {\textendash} 27A1-MAS-NMR and 29Si-MAS-NMR, nitrogen physisorption, Fourier transform infrared spectroscopy and inductively coupled plasma optical emission spectrometry. The sodium forms of Beta zeolites were transformed to the proton forms H-Beta by ion-exchange using aqueous solutions of NH4NO3 and thereafter evaluated in Prins cyclization of (−)-isopulegol with benzaldehyde. The best catalyst synthesized at 150 °C in the rotation mode for 17 h possessing an optimal combination of morphological and structural properties as well as concentration of acid sites demonstrated high (−)-isopulegol conversion (93\%) along with high selectivity to the desired product (79\%).",

keywords = "Beta zeolites, Catalyst synthesis, Catalytic materials, Characterization, Prins cyclization",

author = "Zaykovskaya, \{Anna O.\} and Narendra Kumar and Kholkina, \{Ekaterina A.\} and Li-Zhulanov, \{Nikolai S.\} and P{\"a}ivi M{\"a}ki-Arvela and Atte Aho and Janne Peltonen and Markus Peurla and Ivo Heinmaa and Kusema, \{Bright T.\} and St{\'e}phane Streiff and Murzin, \{Dmitry Yu.\}",

note = "Anna O. Zaykovskaya is also affiliated with {\AA}AU AAM, 24 m{\aa}n, CC BY NC-ND Mail till P{\"a}ivi 24.2.2021 /LN",

year = "2020",

month = aug,

day = "1",

doi = "10.1016/j.micromeso.2020.110236",

language = "English",

volume = "302",

journal = "Microporous and Mesoporous Materials",

issn = "1387-1811",

publisher = "Elsevier",

}

Zaykovskaya, AO, Kumar, N , Kholkina, EA, Li-Zhulanov, NS, Mäki-Arvela, P , Aho, A, Peltonen, J, Peurla, M, Heinmaa, I, Kusema, BT, Streiff, S & Murzin, DY 2020, 'Synthesis and physico-chemical characterization of Beta zeolite catalysts: Evaluation of catalytic properties in Prins cyclization of (−)-isopulegol', Microporous and Mesoporous Materials, vol. 302, 110236. https://doi.org/10.1016/j.micromeso.2020.110236

Synthesis and physico-chemical characterization of Beta zeolite catalysts: Evaluation of catalytic properties in Prins cyclization of (−)-isopulegol. / Zaykovskaya, Anna O.; Kumar, Narendra ; Kholkina, Ekaterina A. et al.
In: Microporous and Mesoporous Materials, Vol. 302, 110236, 01.08.2020.

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

TY - JOUR

T1 - Synthesis and physico-chemical characterization of Beta zeolite catalysts: Evaluation of catalytic properties in Prins cyclization of (−)-isopulegol

AU - Zaykovskaya, Anna O.

AU - Kumar, Narendra

AU - Kholkina, Ekaterina A.

AU - Li-Zhulanov, Nikolai S.

AU - Mäki-Arvela, Päivi

AU - Aho, Atte

AU - Peltonen, Janne

AU - Peurla, Markus

AU - Heinmaa, Ivo

AU - Kusema, Bright T.

AU - Streiff, Stéphane

AU - Murzin, Dmitry Yu.

N1 - Anna O. Zaykovskaya is also affiliated with ÅAU AAM, 24 mån, CC BY NC-ND Mail till Päivi 24.2.2021 /LN

PY - 2020/8/1

Y1 - 2020/8/1

N2 - Synthesis of Beta zeolite catalysts was carried out using two different methods. The influence of such parameters as synthesis time and temperature, gel composition and gel ripening on the physico-chemical and catalytic properties of Beta zeolite catalysts was studied. A range of analytical methods was applied in this work including scanning and transmission electron microscopies, energy dispersive X-ray spectroscopy, X-ray powder diffraction, nuclear magnetic resonance spectroscopy – 27A1-MAS-NMR and 29Si-MAS-NMR, nitrogen physisorption, Fourier transform infrared spectroscopy and inductively coupled plasma optical emission spectrometry. The sodium forms of Beta zeolites were transformed to the proton forms H-Beta by ion-exchange using aqueous solutions of NH4NO3 and thereafter evaluated in Prins cyclization of (−)-isopulegol with benzaldehyde. The best catalyst synthesized at 150 °C in the rotation mode for 17 h possessing an optimal combination of morphological and structural properties as well as concentration of acid sites demonstrated high (−)-isopulegol conversion (93%) along with high selectivity to the desired product (79%).

AB - Synthesis of Beta zeolite catalysts was carried out using two different methods. The influence of such parameters as synthesis time and temperature, gel composition and gel ripening on the physico-chemical and catalytic properties of Beta zeolite catalysts was studied. A range of analytical methods was applied in this work including scanning and transmission electron microscopies, energy dispersive X-ray spectroscopy, X-ray powder diffraction, nuclear magnetic resonance spectroscopy – 27A1-MAS-NMR and 29Si-MAS-NMR, nitrogen physisorption, Fourier transform infrared spectroscopy and inductively coupled plasma optical emission spectrometry. The sodium forms of Beta zeolites were transformed to the proton forms H-Beta by ion-exchange using aqueous solutions of NH4NO3 and thereafter evaluated in Prins cyclization of (−)-isopulegol with benzaldehyde. The best catalyst synthesized at 150 °C in the rotation mode for 17 h possessing an optimal combination of morphological and structural properties as well as concentration of acid sites demonstrated high (−)-isopulegol conversion (93%) along with high selectivity to the desired product (79%).

KW - Beta zeolites

KW - Catalyst synthesis

KW - Catalytic materials

KW - Characterization

KW - Prins cyclization

UR - https://www.scopus.com/pages/publications/85083739851

U2 - 10.1016/j.micromeso.2020.110236

DO - 10.1016/j.micromeso.2020.110236

M3 - Article

AN - SCOPUS:85083739851

SN - 1387-1811

VL - 302

JO - Microporous and Mesoporous Materials

JF - Microporous and Mesoporous Materials

M1 - 110236

ER -

Synthesis and physico-chemical characterization of Beta zeolite catalysts: Evaluation of catalytic properties in Prins cyclization of (−)-isopulegol

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