Solvent-free synthesis of nanostructured TiO2 in a continuous flow spinning disc reactor for application to photocatalytic reduction of CO2

Nanostructured TiO2 catalysts were synthesised via the sol-gel method using solvent-free titanium (IV) n-butoxide and acidified water at pH 1 in a continuous flow spinning disc reactor (SDR). The influence of disc rotational speed, total flow rate of the reagents, and molar hydrolysis ratio (molar r...

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Main Authors: Abdullahi Adamu, Fernando Russo Abegão, Kamelia Boodhoo
Format: Article
Language:English
Published: Elsevier 2023-01-01
Series:Tetrahedron Green Chem
Subjects:
Online Access:http://www.sciencedirect.com/science/article/pii/S2773223123000067
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author Abdullahi Adamu
Fernando Russo Abegão
Kamelia Boodhoo
author_facet Abdullahi Adamu
Fernando Russo Abegão
Kamelia Boodhoo
author_sort Abdullahi Adamu
collection DOAJ
description Nanostructured TiO2 catalysts were synthesised via the sol-gel method using solvent-free titanium (IV) n-butoxide and acidified water at pH 1 in a continuous flow spinning disc reactor (SDR). The influence of disc rotational speed, total flow rate of the reagents, and molar hydrolysis ratio (molar ratio of the acidified water to the titanium (IV) n-butoxide) on the particle size, phase distribution, band gap energy and photocatalytic activity for CO2 reduction was studied. Increasing the disc rotational speed from 400 ​rpm to 1400 ​rpm results in highly sheared, uniformly mixed thin films where small particles (up to ca. 40 ​nm mean diameter) with narrow particle size distribution (polydispersity index of up to 0.5) are formed even at the lower molar hydrolysis ratio of 113. Increasing the molar hydrolysis ratio from 113 to 301 favours anatase phase transformation to rutile phase, thus improving photocatalytic activity. Larger TiO2 particles from the SDR are associated with an increase in their band gap energy whilst doping with copper narrows the band gap energy from 3.00 ​eV down to 2.53 ​eV.The photocatalytic performance of the TiO2 nanoparticles was evaluated for CO2 reduction in the form of bicarbonate ions using a meso-structured photocatalytic reactor at a TiO2 loading of 0.5 ​g L-1 and flow rate of 4 ​mL min-1. A formate production rate of 500 ​μmol ​g-1 ​h-1 is achieved after 2 ​h of irradiation (λ ​= ​254 ​nm) on a bare TiO2 catalyst, with no apparent trend observed with SDR operating conditions used in the production of the nanoparticles. However, for copper-doped TiO2, there is a clear correlation between the anatase to rutile ratio and formate production rate.
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spelling doaj.art-c3f4a5895f1c4a999c1f1a93804067ee2024-01-27T07:03:01ZengElsevierTetrahedron Green Chem2773-22312023-01-011100007Solvent-free synthesis of nanostructured TiO2 in a continuous flow spinning disc reactor for application to photocatalytic reduction of CO2Abdullahi Adamu0Fernando Russo Abegão1Kamelia Boodhoo2School of Engineering, Faculty of Science, Agriculture and Engineering, Newcastle University, Newcastle Upon Tyne, NE1 7RU, UKSchool of Engineering, Faculty of Science, Agriculture and Engineering, Newcastle University, Newcastle Upon Tyne, NE1 7RU, UKCorresponding author.; School of Engineering, Faculty of Science, Agriculture and Engineering, Newcastle University, Newcastle Upon Tyne, NE1 7RU, UKNanostructured TiO2 catalysts were synthesised via the sol-gel method using solvent-free titanium (IV) n-butoxide and acidified water at pH 1 in a continuous flow spinning disc reactor (SDR). The influence of disc rotational speed, total flow rate of the reagents, and molar hydrolysis ratio (molar ratio of the acidified water to the titanium (IV) n-butoxide) on the particle size, phase distribution, band gap energy and photocatalytic activity for CO2 reduction was studied. Increasing the disc rotational speed from 400 ​rpm to 1400 ​rpm results in highly sheared, uniformly mixed thin films where small particles (up to ca. 40 ​nm mean diameter) with narrow particle size distribution (polydispersity index of up to 0.5) are formed even at the lower molar hydrolysis ratio of 113. Increasing the molar hydrolysis ratio from 113 to 301 favours anatase phase transformation to rutile phase, thus improving photocatalytic activity. Larger TiO2 particles from the SDR are associated with an increase in their band gap energy whilst doping with copper narrows the band gap energy from 3.00 ​eV down to 2.53 ​eV.The photocatalytic performance of the TiO2 nanoparticles was evaluated for CO2 reduction in the form of bicarbonate ions using a meso-structured photocatalytic reactor at a TiO2 loading of 0.5 ​g L-1 and flow rate of 4 ​mL min-1. A formate production rate of 500 ​μmol ​g-1 ​h-1 is achieved after 2 ​h of irradiation (λ ​= ​254 ​nm) on a bare TiO2 catalyst, with no apparent trend observed with SDR operating conditions used in the production of the nanoparticles. However, for copper-doped TiO2, there is a clear correlation between the anatase to rutile ratio and formate production rate.http://www.sciencedirect.com/science/article/pii/S2773223123000067CO2 photocatalytic reductionSpinning disc reactorPhotocatalystNanostructured TiO2Solvent-free sol-gel synthesisProcess intensification
spellingShingle Abdullahi Adamu
Fernando Russo Abegão
Kamelia Boodhoo
Solvent-free synthesis of nanostructured TiO2 in a continuous flow spinning disc reactor for application to photocatalytic reduction of CO2
Tetrahedron Green Chem
CO2 photocatalytic reduction
Spinning disc reactor
Photocatalyst
Nanostructured TiO2
Solvent-free sol-gel synthesis
Process intensification
title Solvent-free synthesis of nanostructured TiO2 in a continuous flow spinning disc reactor for application to photocatalytic reduction of CO2
title_full Solvent-free synthesis of nanostructured TiO2 in a continuous flow spinning disc reactor for application to photocatalytic reduction of CO2
title_fullStr Solvent-free synthesis of nanostructured TiO2 in a continuous flow spinning disc reactor for application to photocatalytic reduction of CO2
title_full_unstemmed Solvent-free synthesis of nanostructured TiO2 in a continuous flow spinning disc reactor for application to photocatalytic reduction of CO2
title_short Solvent-free synthesis of nanostructured TiO2 in a continuous flow spinning disc reactor for application to photocatalytic reduction of CO2
title_sort solvent free synthesis of nanostructured tio2 in a continuous flow spinning disc reactor for application to photocatalytic reduction of co2
topic CO2 photocatalytic reduction
Spinning disc reactor
Photocatalyst
Nanostructured TiO2
Solvent-free sol-gel synthesis
Process intensification
url http://www.sciencedirect.com/science/article/pii/S2773223123000067
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AT kameliaboodhoo solventfreesynthesisofnanostructuredtio2inacontinuousflowspinningdiscreactorforapplicationtophotocatalyticreductionofco2