Skip to main content
U.S. Department of Energy
Office of Scientific and Technical Information

Mesoporous Crystalline Niobium Oxide with a High Surface Area: A Solid Acid Catalyst for Alkyne Hydration

Journal Article · · ACS Applied Materials and Interfaces
A mesoporous crystalline niobium oxide with tunable pore sizes was synthesized via the sol–gel-based inverse micelle method. The material shows a surface area of 127 m2/g, which is the highest surface area reported so far for crystalline niobium oxide synthesized by soft template methods. The material also has a monomodal pore size distribution with an average pore diameter of 5.6 nm. A comprehensive characterization of niobium oxide was performed using powder X-ray diffraction, Brunauer–Emmett–Teller, thermogravimetric analysis, scanning electron microscopy, transmission electron microscopy, UV–vis, and X-ray photoelectron spectroscopy. The material acts as an environmentally friendly, solid acid catalyst toward hydration of alkynes under with excellent catalytic activity (99% conversion, 99% selectivity, and 4.39 h–1 TOF). Brønsted acid sites present in the catalyst were found to be responsible for the high catalytic activity. Lastly, the catalyst was reusable up to five cycles without a significant loss of the activity.
Research Organization:
Univ. of Connecticut, Storrs, CT (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences & Biosciences Division
Grant/Contract Number:
FG02-86ER13622
OSTI ID:
1776504
Alternate ID(s):
OSTI ID: 1838012
Journal Information:
ACS Applied Materials and Interfaces, Journal Name: ACS Applied Materials and Interfaces Journal Issue: 42 Vol. 12; ISSN 1944-8244
Publisher:
American Chemical Society (ACS)Copyright Statement
Country of Publication:
United States
Language:
English

References (57)

Layered Orthorhombic Nb 2 O 5 @Nb 4 C 3 T x and TiO 2 @Ti 3 C 2 T x Hierarchical Composites for High Performance Li-ion Batteries journal May 2016
In-Plane Assembled Orthorhombic Nb 2 O 5 Nanorod Films with High-Rate Li + Intercalation for High-Performance Flexible Li-Ion Capacitors journal November 2017
Enhancement of Photocatalytic and Electrochromic Properties of Electrochemically Fabricated Mesoporous WO3 Thin Films journal August 2003
Recent Progress in the Synthesis of Porous Carbon Materials journal August 2006
A New Metastable Phase of Crystallized V2O4·0.25H2O Nanowires: Synthesis and Electrochemical Measurements journal December 2005
Monodispersed Particles: Monodispersed Nb 2 O 5 Microspheres: Facile Synthesis, Air/Water Interfacial Self-Assembly, Nb 2 O 5 -Based Composite Films, and Their Selective NO 2 Sensing (Adv. Mater. Interfaces 11/2015) journal July 2015
Graphene Oxide: A Convenient Carbocatalyst for Facilitating Oxidation and Hydration Reactions journal August 2010
Fluorine-Enabled Cationic Gold Catalysis: Functionalized Hydration of Alkynes journal August 2010
Shape-Dependent Acidity and Photocatalytic Activity of Nb2O5 Nanocrystals with an Active TT (001) Surface journal February 2012
Hard Templating of Nanocrystalline Titanium Dioxide with Chiral Nematic Ordering journal May 2012
Heterogeneously Catalyzed Efficient Hydration of Alkynes to Ketones by Tin-Tungsten Mixed Oxides journal December 2010
Surface-controlled Nb2O5 nanoparticle networks for fast Li transport and storage journal October 2018
Crystallite-size dependency of the pressure and temperature response in nanoparticles of magnesia journal July 2017
Optical and electrochemical characteristics of niobium oxide films prepared by sol-gel process and magnetron sputtering A comparison journal August 1996
Pulsed laser deposition of mesoporous niobium oxide thin films and application as chemical sensors journal March 1999
Electrochemistry and biosensing reactivity of heme proteins adsorbed on the structure-tailored mesoporous Nb2O5 matrix journal August 2004
Solvent-free hydration of alkynes over Hβ zeolite journal September 2015
A green and efficient hydration of alkynes catalyzed by hierarchically porous poly(ionic liquid)s solid strong acids journal August 2018
Synthesis of Nb2O5 nanoparticles through the oxidant peroxide method applied to organic pollutant photodegradation: A mechanistic study journal January 2014
Superior photocatalytic disinfection effect of Ag-3D ordered mesoporous CeO2 under visible light journal May 2018
Enhanced activity of mesoporous Nb2O5 for photocatalytic hydrogen production journal August 2007
Facile synthesis of Nb2O5 nanorod array films and their electrochemical properties journal September 2011
Investigation of thermal treatment effect on physicochemical and photocatalytic H2 production properties of mesoporous-assembled Nb2O5 nanoparticles synthesized via a surfactant-modified sol–gel method journal January 2013
High-silica Hβ zeolites for catalytic hydration of hydrophobic epoxides and alkynes in water journal December 2018
Easy access to highly crystalline mesoporous transition-metal oxides with controllable uniform large pores by using block copolymers synthesized via atom transfer radical polymerization journal August 2011
Mesoporous Molybdenum–Tungsten Mixed Metal Oxide: A Solid Acid Catalyst for Green, Highly Efficient sp 3 –sp 2 C–C Coupling Reactions journal January 2020
Metal Support Interaction in Pt Nanoparticles Partially Confined in the Mesopores of Microsized Mesoporous CeO 2 for Highly Efficient Purification of Volatile Organic Compounds journal December 2015
Structure and Acid Catalysis of Mesoporous Nb 2 O 5 · n H 2 O journal June 2010
Niobium Compounds:  Preparation, Characterization, and Application in Heterogeneous Catalysis journal December 1999
Selective Amine Oxidation Using Nb 2 O 5 Photocatalyst and O 2 journal August 2011
Au-NHC@Porous Organic Polymers: Synthetic Control and Its Catalytic Application in Alkyne Hydration Reactions journal December 2013
Crystallographically Oriented Mesoporous WO3 Films:  Synthesis, Characterization, and Applications
  • Santato, Clara; Odziemkowski, Marek; Ulmann, Martine
  • Journal of the American Chemical Society, Vol. 123, Issue 43, p. 10639-10649 https://doi.org/10.1021/ja011315x
journal October 2001
Three-Dimensionally Ordered Mesoporous Niobium Oxide journal September 2002
Hydration of Terminal Alkynes Catalyzed by Water-Soluble Cobalt Porphyrin Complexes journal December 2012
Mesoporous TiO 2 Nanocrystals Grown in Situ on Graphene Aerogels for High Photocatalysis and Lithium-Ion Batteries journal April 2014
Dye-Sensitized Solar Cells Based on Oriented TiO 2 Nanotube Arrays: Transport, Trapping, and Transfer of Electrons journal October 2008
[(NHC)Au I ]-Catalyzed Acid-Free Alkyne Hydration at Part-per-Million Catalyst Loadings journal December 2008
Dispersed NbO x Catalytic Phases in Silica Matrixes: Influence of Niobium Concentration and Preparative Route journal August 2008
Nanostructured Nb 2 O 5 Polymorphs by Electrospinning for Rechargeable Lithium Batteries journal November 2009
Synthesis of Highly Ordered Carbon Molecular Sieves via Template-Mediated Structural Transformation journal September 1999
2,6-Dimethylpyridine as a probe of the strength of Brønsted acid sites: study on zeolites. Application to alumina journal January 2005
Mild chemo-selective hydration of terminal alkynes catalysed by AgSbF 6 journal January 2012
Efficient hydration of alkynes through acid-assisted Brønsted acid catalysis journal January 2015
Synthesis, acid properties and catalysis by niobium oxide nanostructured materials journal January 2014
Hydrothermal synthesis of octahedra-based layered niobium oxide and its catalytic activity as a solid acid journal January 2014
Hydration of alkynes at room temperature catalyzed by gold( i ) isocyanide compounds journal January 2015
Facile preparation of hierarchical Nb 2 O 5 microspheres with photocatalytic activities and electrochemical properties journal January 2014
Comparison of amorphous, pseudohexagonal and orthorhombic Nb 2 O 5 for high-rate lithium ion insertion journal January 2016
Upgrading of oxygenated compounds present in aqueous biomass-derived feedstocks over NbO x -based catalysts journal January 2017
The surface acidity of solid oxides and its characterization by IR spectroscopic methods. An attempt at systematization journal January 1999
Solvent-free hydration of alkynes over a heterogeneous silver exchanged silicotungstic acid catalyst journal January 2012
Catalytic Hydration of Alkynes and Its Application in Synthesis journal April 2007
Versatile Methodology to Hydrate Alkynes, in the Presence of a Wide Variety of Functional Groups, with Mercury(II) p -Toluensulfonamidate, Under Catalytic, Mild, and Neutral Conditions journal April 2013
Optical Properties of Sol-Gel Nb 2 O 5 Films with Tunable Porosity for Sensing Applications journal January 2015
Physisorption of gases, with special reference to the evaluation of surface area and pore size distribution (IUPAC Technical Report) journal October 2015
Synthesis and Structural Properties of Niobium Pentoxide Powders: A Comparative Study of the Growth Process journal October 2016
A Porous Polymer-Based Solid Acid Catalyst with Excellent Amphiphilicity: An Active and Environmentally Friendly Catalyst for the Hydration of Alkynes journal December 2019