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Bifunctional mesoporous hybrid sol-gel prepared silicas for CO2 adsorption

  • Original Paper: Sol-gel and hybrid materials for energy, environment and building applications
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Abstract

Bifunctionalized mesoporous silica materials were prepared by sol–gel method applying newly proposed sequence of addition of the used silanols in the systems tetraethylortosilicate (TEOS): Tris[3-(trimethoxysilyl)propyl] isocyanurate (ISC): bis[(3- trimethoxysilyl)propyl]amine (BTPA), TEOS: ISC: (3-mercaptopropyl)trimethoxysilane (MPTMS) (TEOS: ISC: MPTMS) and TEOS: BTPA: MPTMS. The bi-functionalized hybrid silicas were synthesized by co-condensation reaction between TEOS and silsesquioxane precursors in acidic media. Soft template approach for pore formation was applied with structural directing agent Pluronic P123. Mesitylene and KCl were used for improving the materials' texture. New sequences of addition of the silanol precursors into the reaction mixture were applied in order to achieve better distribution of the functional groups on the materials surface and for prevention of entrapment of the functional groups in the pore walls. The synthesized bi-functional hybrid mesoporous silicas were investigated by FTIR, N2-physisorption, DTA/TG-MS, SEM, XPS and XRD techniques. CO2 adsorption properties of the synthesized bi-functionalized hybrids were investigated. I was found that the sequence of addition of silanol precursors, the type of the silsesquioxane precursors and the presence of isocyanurate groups have significant influence on the materials texture, morphology and CO2 sorption properties. The presence of isocyanurate groups in the hybrid silica framework significantly improves the textural characteristics and CO2 sorption capacities. The determined heats of adsorption evidenced CO2 physisorption on the active sites of the hybrid materials.

Original scheme for preparation of bifunctional mesoporous silica in the system TEOS: BTPA: ISC.

Highlights

  • Bifunctionalized silicas are prepared by TEOS, ISC, BTPA and/or MPTMS in presence of Pluronic P123.

  • Sequence of silanol addition influences texture, morphology and distribution of surface functional groups.

  • Materials with pore size in the range 3.8–4.4 nm and lack of long-range pore order were prepared.

  • Heats of adsorption evidence CO2 physisorption on the active sites of the hybrids.

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Funding

This work was supported by KAKENHI (18F18768), Grant-in-Aid for JSPS Fellows. Research equipment of distributed research infrastructure INFRAMAT (part of Bulgarian National roadmap for research infrastructures) supported by Bulgarian Ministry of Education and Science under contract D01-155/28.08.2018 and project “Center of Excellence: National center of mechatronics and clean technologies” - BG05M2OP001-1.001-0008 were used in this investigation.

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  1. JSPS International Research Fellow, Graduate School of Science and Technology, Gunma University, Kiryu, 376-8515, Japan

    Nina Velikova

  2. Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., bl. 11, Sofia 1113, Bulgaria, Bulgaria

    Nina Velikova & Ivanka Spassova

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  1. Nina Velikova
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Correspondence to Nina Velikova.

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Velikova, N., Spassova, I. Bifunctional mesoporous hybrid sol-gel prepared silicas for CO2 adsorption. J Sol-Gel Sci Technol 100, 326–340 (2021). https://doi.org/10.1007/s10971-021-05641-8

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