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aerogels supporting Pt\/TiO2 nanoparticles were fabricated using a one-pot supercritical CO2 gelling and drying method, followed by mild reduction under a N2 atmosphere. Electron microscopy images and N2 adsorption\/desorption isotherms indicate the formation of 3D monolithic aerogels with a meso\/macroporous morphology. A comprehensive evaluation of the synthesized photocatalyst was carried out with a focus on the target application: the photocatalytic production of H2 from methanol in aqueous media. The reaction conditions (water\/methanol ratio, catalyst concentration), together with the aerogel composition (Pt\/TiO2\/rGO ratio) and architecture (size of the aerogel pieces), were the factors that varied in optimizing the process. These experimental parameters influenced the diffusion of the reactants\/products inside the aerogel, the permeability of the porous structure, and the light-harvesting properties, all determined in this study towards maximizing H2 production. Using methanol as the sacrificial agent, the measured H2 production rate for the optimized system (18,800 \u00b5molH2h\u22121gNPs\u22121) was remarkably higher than the values found in the literature for similar Pt\/TiO2\/rGO catalysts and reaction media (2000\u201310,000 \u00b5molH2h\u22121gNPs\u22121).<\/jats:p>","DOI":"10.3390\/gels8110719","type":"journal-article","created":{"date-parts":[[2022,11,8]],"date-time":"2022-11-08T10:47:34Z","timestamp":1667904454000},"page":"719","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":13,"title":["Photocatalytic Hydrogen Production Using Porous 3D Graphene-Based Aerogels Supporting Pt\/TiO2 Nanoparticles"],"prefix":"10.3390","volume":"8","author":[{"given":"M\u00e1rta","family":"Kubovics","sequence":"first","affiliation":[{"name":"Instituto de Ciencia de Materiales de Barcelona, CSIC, Campus UAB s\/n, 8193 Bellaterra, Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6469-4871","authenticated-orcid":false,"given":"Cl\u00e1udia G.","family":"Silva","sequence":"additional","affiliation":[{"name":"LSRE-LCM-Laboratory of Separation and Reaction Engineering\u2013Laboratory of Catalysis and Materials, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal"},{"name":"ALiCE-Associate Laboratory in Chemical Engineering, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3777-3205","authenticated-orcid":false,"given":"Ana M.","family":"L\u00f3pez-Periago","sequence":"additional","affiliation":[{"name":"Instituto de Ciencia de Materiales de Barcelona, CSIC, Campus UAB s\/n, 8193 Bellaterra, Spain"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6531-3978","authenticated-orcid":false,"given":"Joaquim L.","family":"Faria","sequence":"additional","affiliation":[{"name":"LSRE-LCM-Laboratory of Separation and Reaction Engineering\u2013Laboratory of Catalysis and Materials, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal"},{"name":"ALiCE-Associate Laboratory in Chemical Engineering, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal"}]},{"given":"Concepci\u00f3n","family":"Domingo","sequence":"additional","affiliation":[{"name":"Instituto de Ciencia de Materiales de Barcelona, CSIC, Campus UAB s\/n, 8193 Bellaterra, Spain"}]}],"member":"1968","published-online":{"date-parts":[[2022,11,7]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"9324","DOI":"10.1016\/j.ijhydene.2020.12.089","article-title":"Current progress on 3D graphene-based photocatalysts: From synthesis to photocatalytic hydrogen production","volume":"46","author":"Wong","year":"2021","journal-title":"Int. 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