Synthesis and characterization of sulfated TiO 2 nanorods and ZrO 2/TiO 2 nanocomposites for the esterification of biobased organic acid

Zhonglai Li, Renata Wnetrzak, Witold Kwapinski, James J. Leahy

Research output: Contribution to journalArticlepeer-review

Abstract

TiO 2 nanorods and ZrO 2-modified TiO 2 nanocomposites have been prepared by hydrothermal synthesis and the deposition-precipitation method. Their sulfated products were tested as solid superacid catalysts for the esterification of levulinic acid which was used as a model bio-oil molecule. SEM and TEM characterization showed that TiO 2 nanorods with diameters ranging from 20 to 200 nm and with lengths of up to 5 μm were synthesized by a hydrothermal method at 180 °C. ZrO 2 nanoparticles with the diameters ranging from 10 to 20 nm were evenly deposited on TiO 2 nanorods. IR and XPS results suggested that sulfated ZrO 2/TiO 2 nanocomposite has higher content of sulfate groups on the surface with a S/(Zr+Ti) ratio of 13.6% than sulfated TiO 2 nanorods with a S/Ti ratio of 4.9%. The HPLC results showed that sulfated ZrO 2/TiO 2 nanocomposite have enhanced catalytic activity for esterification reaction between levulinic acid and ethanol compared to sulfated TiO 2 nanorods. The conversion of levulinic acid to ethyl levulinate can reach to 90.4% at the reaction temperature of 105 °C after 180 min.

Original languageEnglish
Pages (from-to)4499-4505
Number of pages7
JournalACS Applied Materials and Interfaces
Volume4
Issue number9
DOIs
Publication statusPublished - 26 Sep 2012

Keywords

  • bio-oil
  • levulinic acid
  • nanocomposite
  • sulfate
  • TiO
  • ZrO

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