4.6 Article

Mixing nitrogen-containing compounds for synthesis of porous boron nitride for improved porosity, surface functionality, and solid base catalytic activity

Journal

APPLIED CATALYSIS A-GENERAL
Volume 638, Issue -, Pages -

Publisher

ELSEVIER
DOI: 10.1016/j.apcata.2022.118635

Keywords

Boron nitride; Porous materials; Solid base catalyst; 11 B MAS NMR; B K-edge XAFS

Funding

  1. JSPS, Japan [21K18853]
  2. ESPEC Foundation for Global Environment Research and Technology (Charitable Trust) (ESPEC Prize for the Encouragement of Environmental Studies)
  3. Yashima Environment Technology Foundation
  4. AIST Nanocharacterization Facility (ANCF) platform as a program of the Nanotechnology Platform of the Ministry of Education, Culture, Sports, Science and Technology (MEXT), Japan [JPMX09A21AT0045]
  5. KEK-IMSS-PF [2021G518]
  6. Grants-in-Aid for Scientific Research [21K18853] Funding Source: KAKEN

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Porous boron nitride was synthesized using boric acid with urea and/or hexamethylenetetramine (HMTA) via pyrolysis method. The synthesized boron nitride has a turbostratic structure with both amino and hydroxyl groups on the surface. The mixture of two nitrogen-containing precursors not only significantly increases the porosity, but also improves the surface functionality.
Porous boron nitride was synthesized using boric acid with urea and/or hexamethylenetetramine (HMTA) via pyrolysis method. X-ray diffraction and Fourier transform infrared measurements indicated that the synthesized boron nitride has a turbostratic structure with both amino and hydroxyl group on the surface. The synthesis using a mixture of two nitrogen-containing precursors was found to not only significantly increase the porosity, but also improve the surface functionality. X-ray photoelectron spectroscopy and B K-edge and O K-edge X-ray absorption fine structure measurements revealed that the proportion of amino and hydroxyl groups on the surface increased with increasing concentration of HMTA during synthesis. Solid-state 11B nuclear magnetic resonance spectroscopy indicated that all samples contained trigonal B-N, trigonal B-O and tetrahedral B-O sites, and that samples prepared with high concentrations of HMTA had less tetrahedral B-O sites, suppressing the formation of BOx species as byproducts. Solid base catalytic activity was evaluated through Knoevenagel condensation, and the catalytic performance was significantly improved by synthesizing boron nitride catalyst using a mixture of the two nitrogen-containing precursors. The enhancement of the activity was influenced by the development of the pore structure as well as the emergence of functional groups on the surface.

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