Preparation of α-MoO3 from H3PMo12O40 precursor: synthesis of 1,2-cyclohexanediol from cyclohexene over α-MoO3-TiO2 catalyst

A series of α -MoO _3 -TiO _2 mixed oxides were prepared by calcining a mixture of the heteropolyacid H _3 PMo _12 O _40 and TiO _2 at temperatures ranging from 350 °C to 600 °C. The mixed oxides thus prepared were characterized and tested for the oxidation of cyclohexene by the oxidizing mixture H...

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Main Authors: Tahani Saad AlGarni, Naaser A Y Abduh, Abdullah Al Kahtani, Ahmed Aouissi
Format: Article
Language:English
Published: IOP Publishing 2022-01-01
Series:Materials Research Express
Subjects:
Online Access:https://doi.org/10.1088/2053-1591/ac8a3d
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author Tahani Saad AlGarni
Naaser A Y Abduh
Abdullah Al Kahtani
Ahmed Aouissi
author_facet Tahani Saad AlGarni
Naaser A Y Abduh
Abdullah Al Kahtani
Ahmed Aouissi
author_sort Tahani Saad AlGarni
collection DOAJ
description A series of α -MoO _3 -TiO _2 mixed oxides were prepared by calcining a mixture of the heteropolyacid H _3 PMo _12 O _40 and TiO _2 at temperatures ranging from 350 °C to 600 °C. The mixed oxides thus prepared were characterized and tested for the oxidation of cyclohexene by the oxidizing mixture H _2 O _2 /CO _2 . FTIR and XRD characterizations showed that the Keggin structure of H _3 PMo _12 O _40 was preserved for calcination temperatures below 400 °C. Above 450 °C, Keggin’s structure collapses. XRD analysis revealed that as the calcination temperature increased, more orthorhombic α -MoO _3 was formed. Analysis of the reaction mixture by GC-MS showed that oxidation by the H _2 O _2 /CO _2 mixture leads to 1,2-cyclohexanediol as the main product and to 2-cyclohexene-1-one and 2-cyclohexene-1-ol as minor products. Oxidation by H _2 O _2 /CO _2 mixture proved to be more effective than H _2 O _2 alone and CO _2 alone. The conversion (69.4%) and the 1,2-cyclohexanediol selectivity (93.2%) obtained over α -MoO _3 -TiO _2 mixed oxides, higher than that obtained with TiO _2 monoxide and α -MoO _3 monoxide, suggest a synergistic effect between TiO _2 and α -MoO _3 . This efficient and stable catalyst after reuse can be developed for the synthesis of diols.
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spelling doaj.art-d5c6214050d5452bb50518c0a55e3c6a2023-08-09T16:16:20ZengIOP PublishingMaterials Research Express2053-15912022-01-019808500310.1088/2053-1591/ac8a3dPreparation of α-MoO3 from H3PMo12O40 precursor: synthesis of 1,2-cyclohexanediol from cyclohexene over α-MoO3-TiO2 catalystTahani Saad AlGarni0Naaser A Y Abduh1Abdullah Al Kahtani2Ahmed Aouissi3https://orcid.org/0000-0001-9035-8660Chemistry Department, College of Science, King Saud University , Riyadh, Saudi ArabiaChemistry Department, College of Science, King Saud University , Riyadh, Saudi ArabiaChemistry Department, College of Science, King Saud University , Riyadh, Saudi ArabiaChemistry Department, College of Science, King Saud University , Riyadh, Saudi ArabiaA series of α -MoO _3 -TiO _2 mixed oxides were prepared by calcining a mixture of the heteropolyacid H _3 PMo _12 O _40 and TiO _2 at temperatures ranging from 350 °C to 600 °C. The mixed oxides thus prepared were characterized and tested for the oxidation of cyclohexene by the oxidizing mixture H _2 O _2 /CO _2 . FTIR and XRD characterizations showed that the Keggin structure of H _3 PMo _12 O _40 was preserved for calcination temperatures below 400 °C. Above 450 °C, Keggin’s structure collapses. XRD analysis revealed that as the calcination temperature increased, more orthorhombic α -MoO _3 was formed. Analysis of the reaction mixture by GC-MS showed that oxidation by the H _2 O _2 /CO _2 mixture leads to 1,2-cyclohexanediol as the main product and to 2-cyclohexene-1-one and 2-cyclohexene-1-ol as minor products. Oxidation by H _2 O _2 /CO _2 mixture proved to be more effective than H _2 O _2 alone and CO _2 alone. The conversion (69.4%) and the 1,2-cyclohexanediol selectivity (93.2%) obtained over α -MoO _3 -TiO _2 mixed oxides, higher than that obtained with TiO _2 monoxide and α -MoO _3 monoxide, suggest a synergistic effect between TiO _2 and α -MoO _3 . This efficient and stable catalyst after reuse can be developed for the synthesis of diols.https://doi.org/10.1088/2053-1591/ac8a3ddiolcyclohexene dihydroxylationcarbon dioxidehydrogen peroxideα-MoO3
spellingShingle Tahani Saad AlGarni
Naaser A Y Abduh
Abdullah Al Kahtani
Ahmed Aouissi
Preparation of α-MoO3 from H3PMo12O40 precursor: synthesis of 1,2-cyclohexanediol from cyclohexene over α-MoO3-TiO2 catalyst
Materials Research Express
diol
cyclohexene dihydroxylation
carbon dioxide
hydrogen peroxide
α-MoO3
title Preparation of α-MoO3 from H3PMo12O40 precursor: synthesis of 1,2-cyclohexanediol from cyclohexene over α-MoO3-TiO2 catalyst
title_full Preparation of α-MoO3 from H3PMo12O40 precursor: synthesis of 1,2-cyclohexanediol from cyclohexene over α-MoO3-TiO2 catalyst
title_fullStr Preparation of α-MoO3 from H3PMo12O40 precursor: synthesis of 1,2-cyclohexanediol from cyclohexene over α-MoO3-TiO2 catalyst
title_full_unstemmed Preparation of α-MoO3 from H3PMo12O40 precursor: synthesis of 1,2-cyclohexanediol from cyclohexene over α-MoO3-TiO2 catalyst
title_short Preparation of α-MoO3 from H3PMo12O40 precursor: synthesis of 1,2-cyclohexanediol from cyclohexene over α-MoO3-TiO2 catalyst
title_sort preparation of α moo3 from h3pmo12o40 precursor synthesis of 1 2 cyclohexanediol from cyclohexene over α moo3 tio2 catalyst
topic diol
cyclohexene dihydroxylation
carbon dioxide
hydrogen peroxide
α-MoO3
url https://doi.org/10.1088/2053-1591/ac8a3d
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