Photocatalytic CO2 conversion: sol-gel and aerosolization synthesis of CuxO-modified TiO2 over 3D printed supports

Autores
Pascual, Julián Ramiro; Altieri, Tamara; Lombardo, María Verónica; Montesinos, Victor Nahuel; Quici, Natalia
Año de publicación
2023
Idioma
inglés
Tipo de recurso
documento de conferencia
Estado
versión publicada
Descripción
CuxO-modified TiO2 photocatalysts are powerful materials for conversion of CO2 in methane. However, it is necessary to develop scalable synthesis routes that led to photocatalysts with improved conversion efficiency, elevated photocatalytic activity and low environmental impact. 3D printing facilitates the construction of precise geometrically-controlled reactors in short production times that can speed up the thinking-designing-production cycle of reactors minimizing waste generation. In this work we synthesized CuxO-modified TiO2 photocatalysts following two different routes: (1 ) modification of commercial TiO2 by surface precipitation of Cu2+ (CuxO-TiO2) and (2) one-pot aerosolization of TiO2 and CuxO precursors (CuxO@AerTiO2). The solids were characterized by diffuse reflectance spectroscopy, SEM and XRD. Exploratory experiments for impregnation of photocatalysts in PET monoliths were undertaken. The modification of commercial TiO2 (Aeroxide P25 or Hombikat UV100) was carried out by dropwise addition of 62.9 mL of a 0.05 M Cu2+ solution to 400 mL of a 12.5 g/L of TiO2 suspension in NaOH 0.25 M under continuous stirring. After 4 h, the solid was filtered, washed, dried at 80 °C overnight and, finally, calcinated at 400 °C for 2 h. The effect of copper salt (CuCl2 vs. CuNO3) and Cu loading (0.28, 1 and 5 Cu/Ti At%) was studied. XRD patterns clearly showed the presence of CuO in all cases over the P25 samples, in addition to the anatase and rutile typical signals for the base photocatalyst. When CuCl2 was used as CuxO precursor, well defined nanoparticles of 80 nm where obtained. The synthesis with CuNO3 gave a smooth homogeneous aspect to the solid surface with no distinguishable nanoparticles. The synthesis through aerosolization was based on the one described in the work of Zelcer et al. [1]. Briefly, a solution containing 1.39 g acetylacetone, 1.39 g of glacial acetyc acid, 0.34 g of Ti-iPrOH, 0.0145 g of Cu(NO3)2.3H2O and 0.2 g of Pluronics F127 in 43 mL of MilliQ water was continuously fed to a Büchi B-290 spray drier with a peristaltic pump at a flow rate of 3 mL/min. The liquid was atomized at 220 °C in a two-fluid nozzle with a secondary air-flow of 473 L/h. After collection of the material from the cyclone of the spray drier, the solid was calcined at 440 °C for 4 h. The band-gaps of the synthetized photocatalysts were calculated by the Tauc method being 3.13 eV, 3.17 eV and 3.15 eV for the CuxO-P25, CuxO-UV100 and CuxO@AerTiO2 powders, respectively. Square-based monolith of 3  1.5  3 cm with 15% of PET loading were impregnated by dip-coating in suspensions of 1 – 20 g/L of P25. Once dried at 50°C overnight, all of them were irradiated from one side with a 365 nm UV-LED and the UV-light intensity was measured before and after passing through the impregnated monolith by a 365 nm radiometer. The use of 1 g/L of TiO2 was found as the best option as it absorbs 90% of the UV-light, against the 92.3% absorbed by the monolith impregnated in the 20 g/L suspension. In all cases, the diffuse reflectance spectrum obtained for the Cumodified TiO2 impregnated supports matched the spectrum of the respective powders. The solids synthesized presented promising structural and optical properties and, currently, XRD and SEM analysis are being completed, together with porosimetry for all solids to have broader and comparative information.
UTN
FONCyT
CONICET
Fil: Pascual, Julián Ramiro. Centro Tecnologías Químicas – Dpto. de Ingeniería Química, FRBA, UTN, Medrano 951, CABA, Argentina
Fil: Altieri, Tamara. Gerencia de Química - INN – CNEA, CONICET, Av. Gral. Paz 1499, Villa Maipú, Argentina,
Fil: Lombardo, María Verónica. Gerencia de Química - INN – CNEA, CONICET, Av. Gral. Paz 1499, Villa Maipú, Argentina,
Fil: Montesinos, Victor Nahuel. Centro Tecnologías Químicas – Dpto. de Ingeniería Química, FRBA, UTN, Medrano 951, CABA, Argentina. Gerencia de Química – CNEA, Av. Gral. Paz 1499, Villa Maipú, Argentina.
Fil: Quici, Natalia. Centro Tecnologías Químicas – Dpto. de Ingeniería Química, FRBA, UTN, Medrano 951, CABA, Argentina. Gerencia de Química – CNEA, Av. Gral. Paz 1499, Villa Maipú, Argentina.
Materia
3D printing
TiO2
NOx
heterogeneous photocatalysis
Nivel de accesibilidad
acceso abierto
Condiciones de uso
2024-03-27T17:14:07Z
Repositorio
Repositorio Institucional Abierto (UTN)
Institución
Universidad Tecnológica Nacional
OAI Identificador
oai:ria.utn.edu.ar:20.500.12272/10196
Acceder
id RIAUTN_efb235168d500670fff7baf57137df8b
oai_identifier_str oai:ria.utn.edu.ar:20.500.12272/10196
network_acronym_str RIAUTN
repository_id_str a
network_name_str Repositorio Institucional Abierto (UTN)
spelling Photocatalytic CO2 conversion: sol-gel and aerosolization synthesis of CuxO-modified TiO2 over 3D printed supportsPascual, Julián RamiroAltieri, TamaraLombardo, María VerónicaMontesinos, Victor NahuelQuici, Natalia3D printingTiO2NOxheterogeneous photocatalysisCuxO-modified TiO2 photocatalysts are powerful materials for conversion of CO2 in methane. However, it is necessary to develop scalable synthesis routes that led to photocatalysts with improved conversion efficiency, elevated photocatalytic activity and low environmental impact. 3D printing facilitates the construction of precise geometrically-controlled reactors in short production times that can speed up the thinking-designing-production cycle of reactors minimizing waste generation. In this work we synthesized CuxO-modified TiO2 photocatalysts following two different routes: (1 ) modification of commercial TiO2 by surface precipitation of Cu2+ (CuxO-TiO2) and (2) one-pot aerosolization of TiO2 and CuxO precursors (CuxO@AerTiO2). The solids were characterized by diffuse reflectance spectroscopy, SEM and XRD. Exploratory experiments for impregnation of photocatalysts in PET monoliths were undertaken. The modification of commercial TiO2 (Aeroxide P25 or Hombikat UV100) was carried out by dropwise addition of 62.9 mL of a 0.05 M Cu2+ solution to 400 mL of a 12.5 g/L of TiO2 suspension in NaOH 0.25 M under continuous stirring. After 4 h, the solid was filtered, washed, dried at 80 °C overnight and, finally, calcinated at 400 °C for 2 h. The effect of copper salt (CuCl2 vs. CuNO3) and Cu loading (0.28, 1 and 5 Cu/Ti At%) was studied. XRD patterns clearly showed the presence of CuO in all cases over the P25 samples, in addition to the anatase and rutile typical signals for the base photocatalyst. When CuCl2 was used as CuxO precursor, well defined nanoparticles of 80 nm where obtained. The synthesis with CuNO3 gave a smooth homogeneous aspect to the solid surface with no distinguishable nanoparticles. The synthesis through aerosolization was based on the one described in the work of Zelcer et al. [1]. Briefly, a solution containing 1.39 g acetylacetone, 1.39 g of glacial acetyc acid, 0.34 g of Ti-iPrOH, 0.0145 g of Cu(NO3)2.3H2O and 0.2 g of Pluronics F127 in 43 mL of MilliQ water was continuously fed to a Büchi B-290 spray drier with a peristaltic pump at a flow rate of 3 mL/min. The liquid was atomized at 220 °C in a two-fluid nozzle with a secondary air-flow of 473 L/h. After collection of the material from the cyclone of the spray drier, the solid was calcined at 440 °C for 4 h. The band-gaps of the synthetized photocatalysts were calculated by the Tauc method being 3.13 eV, 3.17 eV and 3.15 eV for the CuxO-P25, CuxO-UV100 and CuxO@AerTiO2 powders, respectively. Square-based monolith of 3  1.5  3 cm with 15% of PET loading were impregnated by dip-coating in suspensions of 1 – 20 g/L of P25. Once dried at 50°C overnight, all of them were irradiated from one side with a 365 nm UV-LED and the UV-light intensity was measured before and after passing through the impregnated monolith by a 365 nm radiometer. The use of 1 g/L of TiO2 was found as the best option as it absorbs 90% of the UV-light, against the 92.3% absorbed by the monolith impregnated in the 20 g/L suspension. In all cases, the diffuse reflectance spectrum obtained for the Cumodified TiO2 impregnated supports matched the spectrum of the respective powders. The solids synthesized presented promising structural and optical properties and, currently, XRD and SEM analysis are being completed, together with porosimetry for all solids to have broader and comparative information.UTNFONCyTCONICETFil: Pascual, Julián Ramiro. Centro Tecnologías Químicas – Dpto. de Ingeniería Química, FRBA, UTN, Medrano 951, CABA, ArgentinaFil: Altieri, Tamara. Gerencia de Química - INN – CNEA, CONICET, Av. Gral. Paz 1499, Villa Maipú, Argentina,Fil: Lombardo, María Verónica. Gerencia de Química - INN – CNEA, CONICET, Av. Gral. Paz 1499, Villa Maipú, Argentina,Fil: Montesinos, Victor Nahuel. Centro Tecnologías Químicas – Dpto. de Ingeniería Química, FRBA, UTN, Medrano 951, CABA, Argentina. Gerencia de Química – CNEA, Av. Gral. Paz 1499, Villa Maipú, Argentina.Fil: Quici, Natalia. Centro Tecnologías Químicas – Dpto. de Ingeniería Química, FRBA, UTN, Medrano 951, CABA, Argentina. Gerencia de Química – CNEA, Av. Gral. Paz 1499, Villa Maipú, Argentina.2024-03-27T17:14:07Z2024-03-27T17:14:07Z2023info:eu-repo/semantics/conferenceObjectinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_5794info:ar-repo/semantics/documentoDeConferenciapdfapplication/pdfhttps://www.wcce11.org/wc/template/Proceedings-Abstracts_WCCE11.pdf?http://hdl.handle.net/20.500.12272/10196enginfo:eu-repo/semantics/openAccess2024-03-27T17:14:07Zhttp://creativecommons.org/licenses/by-nc-nd/4.0/Attribution-NonCommercial-NoDerivatives 4.0 InternacionalAtribuciónreponame:Repositorio Institucional Abierto (UTN)instname:Universidad Tecnológica Nacional2026-10-01T12:01:05Zoai:ria.utn.edu.ar:20.500.12272/10196instacron:UTNInstitucionalhttp://ria.utn.edu.ar/Universidad públicaNo correspondehttp://ria.utn.edu.ar/oaigestionria@rec.utn.edu.ar; fsuarez@rec.utn.edu.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:a2026-10-01 12:01:06.059Repositorio Institucional Abierto (UTN) - Universidad Tecnológica Nacionalfalse
dc.title.none.fl_str_mv Photocatalytic CO2 conversion: sol-gel and aerosolization synthesis of CuxO-modified TiO2 over 3D printed supports
title Photocatalytic CO2 conversion: sol-gel and aerosolization synthesis of CuxO-modified TiO2 over 3D printed supports
spellingShingle Photocatalytic CO2 conversion: sol-gel and aerosolization synthesis of CuxO-modified TiO2 over 3D printed supports
Pascual, Julián Ramiro
3D printing
TiO2
NOx
heterogeneous photocatalysis
title_short Photocatalytic CO2 conversion: sol-gel and aerosolization synthesis of CuxO-modified TiO2 over 3D printed supports
title_full Photocatalytic CO2 conversion: sol-gel and aerosolization synthesis of CuxO-modified TiO2 over 3D printed supports
title_fullStr Photocatalytic CO2 conversion: sol-gel and aerosolization synthesis of CuxO-modified TiO2 over 3D printed supports
title_full_unstemmed Photocatalytic CO2 conversion: sol-gel and aerosolization synthesis of CuxO-modified TiO2 over 3D printed supports
title_sort Photocatalytic CO2 conversion: sol-gel and aerosolization synthesis of CuxO-modified TiO2 over 3D printed supports
dc.creator.none.fl_str_mv Pascual, Julián Ramiro
Altieri, Tamara
Lombardo, María Verónica
Montesinos, Victor Nahuel
Quici, Natalia
author Pascual, Julián Ramiro
author_facet Pascual, Julián Ramiro
Altieri, Tamara
Lombardo, María Verónica
Montesinos, Victor Nahuel
Quici, Natalia
author_role author
author2 Altieri, Tamara
Lombardo, María Verónica
Montesinos, Victor Nahuel
Quici, Natalia
author2_role author
author
author
author
dc.subject.none.fl_str_mv 3D printing
TiO2
NOx
heterogeneous photocatalysis
topic 3D printing
TiO2
NOx
heterogeneous photocatalysis
dc.description.none.fl_txt_mv CuxO-modified TiO2 photocatalysts are powerful materials for conversion of CO2 in methane. However, it is necessary to develop scalable synthesis routes that led to photocatalysts with improved conversion efficiency, elevated photocatalytic activity and low environmental impact. 3D printing facilitates the construction of precise geometrically-controlled reactors in short production times that can speed up the thinking-designing-production cycle of reactors minimizing waste generation. In this work we synthesized CuxO-modified TiO2 photocatalysts following two different routes: (1 ) modification of commercial TiO2 by surface precipitation of Cu2+ (CuxO-TiO2) and (2) one-pot aerosolization of TiO2 and CuxO precursors (CuxO@AerTiO2). The solids were characterized by diffuse reflectance spectroscopy, SEM and XRD. Exploratory experiments for impregnation of photocatalysts in PET monoliths were undertaken. The modification of commercial TiO2 (Aeroxide P25 or Hombikat UV100) was carried out by dropwise addition of 62.9 mL of a 0.05 M Cu2+ solution to 400 mL of a 12.5 g/L of TiO2 suspension in NaOH 0.25 M under continuous stirring. After 4 h, the solid was filtered, washed, dried at 80 °C overnight and, finally, calcinated at 400 °C for 2 h. The effect of copper salt (CuCl2 vs. CuNO3) and Cu loading (0.28, 1 and 5 Cu/Ti At%) was studied. XRD patterns clearly showed the presence of CuO in all cases over the P25 samples, in addition to the anatase and rutile typical signals for the base photocatalyst. When CuCl2 was used as CuxO precursor, well defined nanoparticles of 80 nm where obtained. The synthesis with CuNO3 gave a smooth homogeneous aspect to the solid surface with no distinguishable nanoparticles. The synthesis through aerosolization was based on the one described in the work of Zelcer et al. [1]. Briefly, a solution containing 1.39 g acetylacetone, 1.39 g of glacial acetyc acid, 0.34 g of Ti-iPrOH, 0.0145 g of Cu(NO3)2.3H2O and 0.2 g of Pluronics F127 in 43 mL of MilliQ water was continuously fed to a Büchi B-290 spray drier with a peristaltic pump at a flow rate of 3 mL/min. The liquid was atomized at 220 °C in a two-fluid nozzle with a secondary air-flow of 473 L/h. After collection of the material from the cyclone of the spray drier, the solid was calcined at 440 °C for 4 h. The band-gaps of the synthetized photocatalysts were calculated by the Tauc method being 3.13 eV, 3.17 eV and 3.15 eV for the CuxO-P25, CuxO-UV100 and CuxO@AerTiO2 powders, respectively. Square-based monolith of 3  1.5  3 cm with 15% of PET loading were impregnated by dip-coating in suspensions of 1 – 20 g/L of P25. Once dried at 50°C overnight, all of them were irradiated from one side with a 365 nm UV-LED and the UV-light intensity was measured before and after passing through the impregnated monolith by a 365 nm radiometer. The use of 1 g/L of TiO2 was found as the best option as it absorbs 90% of the UV-light, against the 92.3% absorbed by the monolith impregnated in the 20 g/L suspension. In all cases, the diffuse reflectance spectrum obtained for the Cumodified TiO2 impregnated supports matched the spectrum of the respective powders. The solids synthesized presented promising structural and optical properties and, currently, XRD and SEM analysis are being completed, together with porosimetry for all solids to have broader and comparative information.
UTN
FONCyT
CONICET
Fil: Pascual, Julián Ramiro. Centro Tecnologías Químicas – Dpto. de Ingeniería Química, FRBA, UTN, Medrano 951, CABA, Argentina
Fil: Altieri, Tamara. Gerencia de Química - INN – CNEA, CONICET, Av. Gral. Paz 1499, Villa Maipú, Argentina,
Fil: Lombardo, María Verónica. Gerencia de Química - INN – CNEA, CONICET, Av. Gral. Paz 1499, Villa Maipú, Argentina,
Fil: Montesinos, Victor Nahuel. Centro Tecnologías Químicas – Dpto. de Ingeniería Química, FRBA, UTN, Medrano 951, CABA, Argentina. Gerencia de Química – CNEA, Av. Gral. Paz 1499, Villa Maipú, Argentina.
Fil: Quici, Natalia. Centro Tecnologías Químicas – Dpto. de Ingeniería Química, FRBA, UTN, Medrano 951, CABA, Argentina. Gerencia de Química – CNEA, Av. Gral. Paz 1499, Villa Maipú, Argentina.
description CuxO-modified TiO2 photocatalysts are powerful materials for conversion of CO2 in methane. However, it is necessary to develop scalable synthesis routes that led to photocatalysts with improved conversion efficiency, elevated photocatalytic activity and low environmental impact. 3D printing facilitates the construction of precise geometrically-controlled reactors in short production times that can speed up the thinking-designing-production cycle of reactors minimizing waste generation. In this work we synthesized CuxO-modified TiO2 photocatalysts following two different routes: (1 ) modification of commercial TiO2 by surface precipitation of Cu2+ (CuxO-TiO2) and (2) one-pot aerosolization of TiO2 and CuxO precursors (CuxO@AerTiO2). The solids were characterized by diffuse reflectance spectroscopy, SEM and XRD. Exploratory experiments for impregnation of photocatalysts in PET monoliths were undertaken. The modification of commercial TiO2 (Aeroxide P25 or Hombikat UV100) was carried out by dropwise addition of 62.9 mL of a 0.05 M Cu2+ solution to 400 mL of a 12.5 g/L of TiO2 suspension in NaOH 0.25 M under continuous stirring. After 4 h, the solid was filtered, washed, dried at 80 °C overnight and, finally, calcinated at 400 °C for 2 h. The effect of copper salt (CuCl2 vs. CuNO3) and Cu loading (0.28, 1 and 5 Cu/Ti At%) was studied. XRD patterns clearly showed the presence of CuO in all cases over the P25 samples, in addition to the anatase and rutile typical signals for the base photocatalyst. When CuCl2 was used as CuxO precursor, well defined nanoparticles of 80 nm where obtained. The synthesis with CuNO3 gave a smooth homogeneous aspect to the solid surface with no distinguishable nanoparticles. The synthesis through aerosolization was based on the one described in the work of Zelcer et al. [1]. Briefly, a solution containing 1.39 g acetylacetone, 1.39 g of glacial acetyc acid, 0.34 g of Ti-iPrOH, 0.0145 g of Cu(NO3)2.3H2O and 0.2 g of Pluronics F127 in 43 mL of MilliQ water was continuously fed to a Büchi B-290 spray drier with a peristaltic pump at a flow rate of 3 mL/min. The liquid was atomized at 220 °C in a two-fluid nozzle with a secondary air-flow of 473 L/h. After collection of the material from the cyclone of the spray drier, the solid was calcined at 440 °C for 4 h. The band-gaps of the synthetized photocatalysts were calculated by the Tauc method being 3.13 eV, 3.17 eV and 3.15 eV for the CuxO-P25, CuxO-UV100 and CuxO@AerTiO2 powders, respectively. Square-based monolith of 3  1.5  3 cm with 15% of PET loading were impregnated by dip-coating in suspensions of 1 – 20 g/L of P25. Once dried at 50°C overnight, all of them were irradiated from one side with a 365 nm UV-LED and the UV-light intensity was measured before and after passing through the impregnated monolith by a 365 nm radiometer. The use of 1 g/L of TiO2 was found as the best option as it absorbs 90% of the UV-light, against the 92.3% absorbed by the monolith impregnated in the 20 g/L suspension. In all cases, the diffuse reflectance spectrum obtained for the Cumodified TiO2 impregnated supports matched the spectrum of the respective powders. The solids synthesized presented promising structural and optical properties and, currently, XRD and SEM analysis are being completed, together with porosimetry for all solids to have broader and comparative information.
publishDate 2023
dc.date.none.fl_str_mv 2023
2024-03-27T17:14:07Z
2024-03-27T17:14:07Z
dc.type.none.fl_str_mv info:eu-repo/semantics/conferenceObject
info:eu-repo/semantics/publishedVersion
http://purl.org/coar/resource_type/c_5794
info:ar-repo/semantics/documentoDeConferencia
format conferenceObject
status_str publishedVersion
dc.identifier.none.fl_str_mv https://www.wcce11.org/wc/template/Proceedings-Abstracts_WCCE11.pdf?
http://hdl.handle.net/20.500.12272/10196
url https://www.wcce11.org/wc/template/Proceedings-Abstracts_WCCE11.pdf?
http://hdl.handle.net/20.500.12272/10196
dc.language.none.fl_str_mv eng
language eng
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
2024-03-27T17:14:07Z
http://creativecommons.org/licenses/by-nc-nd/4.0/
Attribution-NonCommercial-NoDerivatives 4.0 Internacional
Atribución
eu_rights_str_mv openAccess
rights_invalid_str_mv 2024-03-27T17:14:07Z
http://creativecommons.org/licenses/by-nc-nd/4.0/
Attribution-NonCommercial-NoDerivatives 4.0 Internacional
Atribución
dc.format.none.fl_str_mv pdf
application/pdf
dc.source.none.fl_str_mv reponame:Repositorio Institucional Abierto (UTN)
instname:Universidad Tecnológica Nacional
reponame_str Repositorio Institucional Abierto (UTN)
collection Repositorio Institucional Abierto (UTN)
instname_str Universidad Tecnológica Nacional
repository.name.fl_str_mv Repositorio Institucional Abierto (UTN) - Universidad Tecnológica Nacional
repository.mail.fl_str_mv gestionria@rec.utn.edu.ar; fsuarez@rec.utn.edu.ar
_version_ 1877862444751126528
score 12.853507

Publicaciones similares