SiO2-supported dodecatungstophosphoric acid and Nafion-H prepared by ball-milling for catalytic application

B. Rác, Gabriele Mulas, Anikó Csongrádi, Katalin Lóki, Árpád Molnár

Research output: Contribution to journalArticle

27 Citations (Scopus)

Abstract

Dodecatungstophosphoric acid (HPW) and Nafion-H were supported on SiO2 using the ball-milling technique. Samples were characterized by physical (BET surface, SEM, DSC, XRD, DRIFT and Raman spectroscopies) and chemical (acid-base titration) methods. Catalytic properties were studied in a range of chemical transformations, which can be induced by electrophilic catalysts including Friedel-Crafts reactions (alkylation of toluene with benzyl alcohol, acylation of anisole with acetic anhydride) and the dimerization of α-methylstyrene. Milling conditions (stainless steel or polystyrene apparatus, milling time), loading of the active components, and the type of support were found to have profound effects on the physical characteristics and catalytic performance of the samples. Ball-milled HPW-SiO2 samples prepared under appropriately selected conditions exhibit catalytic properties similar to catalysts made by impregnation. HPW in ball-milled samples, in turn, proved to be more resistant to extraction with polar solvents (hot methanol) and these catalysts display higher stability in recycling studies. Supported Nafion-H samples prepared by ball-milling show high activities in test reactions. The best catalyst exceeds SAC-13 in the selective synthesis of 1,1,3-trimethyl-3-phenylindane in the dimerization of 2-phenylpropene. Catalysts with high catalytic performance require the use of optimal milling time, because particle coalescence and the resulting decrease in BET surface area hinder the accessibility of the active sites.

Original languageEnglish
Pages (from-to)255-265
Number of pages11
JournalApplied Catalysis A: General
Volume282
Issue number1-2
DOIs
Publication statusPublished - Mar 30 2005

Fingerprint

Ball milling
Catalysts
Acids
alpha-methylstyrol
Dimerization
Friedel-Crafts reaction
Benzyl Alcohol
Acylation
Polystyrenes
Stainless Steel
Alkylation
Toluene
Coalescence
Titration
Impregnation
Particles (particulate matter)
Methanol
Raman spectroscopy
Recycling
Alcohols

Keywords

  • Ball-milling
  • Catalyst recycling
  • Dimerization of 2-phenylpropene
  • Dodecatungstophosphoric acid
  • Friedel-Crafts acylation
  • Friedel-Crafts alkylation
  • Nafion-H

ASJC Scopus subject areas

  • Catalysis
  • Process Chemistry and Technology

Cite this

SiO2-supported dodecatungstophosphoric acid and Nafion-H prepared by ball-milling for catalytic application. / Rác, B.; Mulas, Gabriele; Csongrádi, Anikó; Lóki, Katalin; Molnár, Árpád.

In: Applied Catalysis A: General, Vol. 282, No. 1-2, 30.03.2005, p. 255-265.

Research output: Contribution to journalArticle

Rác, B. ; Mulas, Gabriele ; Csongrádi, Anikó ; Lóki, Katalin ; Molnár, Árpád. / SiO2-supported dodecatungstophosphoric acid and Nafion-H prepared by ball-milling for catalytic application. In: Applied Catalysis A: General. 2005 ; Vol. 282, No. 1-2. pp. 255-265.
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AU - Lóki, Katalin

AU - Molnár, Árpád

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AB - Dodecatungstophosphoric acid (HPW) and Nafion-H were supported on SiO2 using the ball-milling technique. Samples were characterized by physical (BET surface, SEM, DSC, XRD, DRIFT and Raman spectroscopies) and chemical (acid-base titration) methods. Catalytic properties were studied in a range of chemical transformations, which can be induced by electrophilic catalysts including Friedel-Crafts reactions (alkylation of toluene with benzyl alcohol, acylation of anisole with acetic anhydride) and the dimerization of α-methylstyrene. Milling conditions (stainless steel or polystyrene apparatus, milling time), loading of the active components, and the type of support were found to have profound effects on the physical characteristics and catalytic performance of the samples. Ball-milled HPW-SiO2 samples prepared under appropriately selected conditions exhibit catalytic properties similar to catalysts made by impregnation. HPW in ball-milled samples, in turn, proved to be more resistant to extraction with polar solvents (hot methanol) and these catalysts display higher stability in recycling studies. Supported Nafion-H samples prepared by ball-milling show high activities in test reactions. The best catalyst exceeds SAC-13 in the selective synthesis of 1,1,3-trimethyl-3-phenylindane in the dimerization of 2-phenylpropene. Catalysts with high catalytic performance require the use of optimal milling time, because particle coalescence and the resulting decrease in BET surface area hinder the accessibility of the active sites.

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