Spiky-shaped niobium pentoxide nano-architecture: highly stable and recoverable Lewis acid catalyst

Abstract

Niobium pentoxide particles with a complex three-dimensional (3D) nanostructure consisting of a spiky structure have been developed as recyclable and recoverable Lewis acid catalysts. The morphology of the niobium pentoxide was successfully controlled from 1D to 3D via a bridging-ligand-assisted hydrothermal treatment, without changing the crystal structure. Compared with dispersed one-dimensional (1D) niobium pentoxide nanorods with a major-axis length and minor-axis length of 20 nm and 5–8 nm, respectively, the spiky-shaped niobium pentoxide composed of 300 nm spherical cores and nanorods with a minor-axis length of 5 nm maintained its surface nanostructure even after calcination at 400 °C in air. The 400 °C-calcined spiky particles exhibited the highest production rate of 2-((4-methoxyphenyl)amino)-2-phenylacetonitrile (0.115 mmol m−2) in a Strecker reaction, resulting in a nanoscale and ordered surface structure of spiky particles that simultaneously exhibit high specific reactivity and high structural stability. Acid site analysis and Raman spectroscopy revealed that stable nanorods that grew in the (001) orientation functioned as Lewis acid catalysts and that the origin of the acidity was a flexible Nb–O polyhedral structure in the single-nanoscale (<10 nm) niobium oxide rods. This study proposes that the spiky-shaped niobium pentoxide exhibits sintering resistivity and high activity and has potential applications as a recoverable and recyclable solid acid catalyst.