Mesoporous hybrid inorganic-organic phosphosilicates by
non-hydrolytic sol-gel reactions

a 2014

Mesoporous hybrid inorganic-organic phosphosilicates by non-hydrolytic sol-gel reactions

PINKAS, Jiří, Aleš STÝSKALÍK, David ŠKODA, Zdeněk MORAVEC, Craig E. BARNES et. al.

Základní údaje

Originální název

Mesoporous hybrid inorganic-organic phosphosilicates by non-hydrolytic sol-gel reactions

Autoři

PINKAS, Jiří (203 Česká republika, garant, domácí), Aleš STÝSKALÍK (203 Česká republika, domácí), David ŠKODA (203 Česká republika, domácí), Zdeněk MORAVEC (840 Spojené státy, domácí) a Craig E. BARNES (840 Spojené státy)

Vydání

248th American Chemical Society National Meeting & Exposition, San Francisco, California, USA, 2014

Další údaje

Jazyk

angličtina

Typ výsledku

Konferenční abstrakt

Obor

10402 Inorganic and nuclear chemistry

Stát vydavatele

Spojené státy

Utajení

není předmětem státního či obchodního tajemství

Odkazy

URL

Impakt faktor

Impact factor: 0.269

Kód RIV

RIV/00216224:14740/14:00077575

Organizační jednotka

Středoevropský technologický institut

ISSN

Klíčová slova anglicky

Mesoporous; hybrid; phosphosilicates; sol-gel; nonhydrolytic

Příznaky

Mezinárodní význam, Recenzováno

Změněno: 20. 5. 2015 20:25, Mgr. Zdeněk Moravec, Ph.D.

Anotace

V originále

Non-hydrolytic sol-gel reactions based on condensation of two functional groups are studied as an alternative to aqueous techniques for the synthesis of multimetallic oxides and inorganic-organic hybrid materials in the form of xerogels, nanoparticles, and thin films. We developed a non-hydrolytic sol-gel route based on acetic acid ester elimination providing parent phosphosilicate and its hybrid inorganic-organic derivatives. The polycondensation reactions between Si(OAc)4 and OP(OSiMe3)3 provides microporous phosphosilicate xerogels with surface areas up to 570 m2 g-1. Substitution reactions of residual acetoxy and trimethylsiloxy groups on the surface with a variety of reagents, such as SiCl4, RSiCl3, POCl3, AlX3, ROH, and Me3SiOSiMe3, show versatility of the synthesized phosphosilicate xerogels in tuning their properties, such as Bronsted and Lewis acidity. The consecutive substitution of Si and P precursors by acetoxysilanes 1RxSi(OC(O)CH3)4-x (1R = Me, Ph; x = 1-2) and trimethylsilylesters of phosphonic acid 2RP(O)(OSiMe3)2 (2R = c-Hex, Ph) caused the decrease of surface areas and increase of average pore sizes because of the lower cross-linking ability of the substituted precursors. To avoid a significant decrease of surface areas of hybrid xerogels we used as precursors acetoxysilanes and phosphonic acid esters with bridging alkyl or aryl groups, such as (AcO)3Si-(CH2)x-Si(OAc)3 (x = 1-3, 6) and (Me3SiO)2P(O)-3R-P(O)(OSiMe3)2 (3R = C2H4, C6H4). We were able to tune the pore size of resulting xerogels to the mesoporous range. The prepared xerogels were characterized by elemental analyses, solid-state 13C, 29Si, 31P NMR spectroscopy, IR spectroscopy, surface area analysis, thermal analysis TG/DSC, and XRD measurements.

Návaznosti

ED1.1.00/02.0068, projekt VaV

Název: CEITEC - central european institute of technology

EE2.3.30.0037, projekt VaV

Název: Zaměstnáním nejlepších mladých vědců k rozvoji mezinárodní spolupráce

LH11028, projekt VaV

Název: Nehydrolytické sol-gelové reakce pro přípravu křemičitanů a fosforečnanů s řízenou porozitou a funkčními skupinami na povrchu (Akronym: NHSGKNOX)

Investor: Ministerstvo školství, mládeže a tělovýchovy ČR, Nehydrolytické sol-gelové reakce pro přípravu křemičitanů a fosforečnanů s řízenou porozitou a funkčními skupinami na povrchu

Citovat

PINKAS, Jiří, Aleš STÝSKALÍK, David ŠKODA, Zdeněk MORAVEC a Craig E. BARNES. Mesoporous hybrid inorganic-organic phosphosilicates by non-hydrolytic sol-gel reactions. In 248th American Chemical Society National Meeting & Exposition, San Francisco, California, USA. 2014. ISSN 0009-2347.

@proceedings{1210926,
   author = {Pinkas, Jiří and Stýskalík, Aleš and Škoda, David and Moravec, Zdeněk and Barnes, Craig E.},
   booktitle = {248th American Chemical Society National Meeting & Exposition, San Francisco, California, USA},
   keywords = {Mesoporous; hybrid; phosphosilicates; sol-gel; nonhydrolytic},
   language = {eng},
   title = {Mesoporous hybrid inorganic-organic phosphosilicates by non-hydrolytic sol-gel reactions},
   url = {http://sanfran2014onsite.acs.org/t/138905},
   year = {2014}
}

TY  - CONF
ID  - 1210926
AU  - Pinkas, Jiří - Stýskalík, Aleš - Škoda, David - Moravec, Zdeněk - Barnes, Craig E.
PY  - 2014
TI  - Mesoporous hybrid inorganic-organic phosphosilicates by non-hydrolytic sol-gel reactions
KW  - Mesoporous
KW  - hybrid
KW  - phosphosilicates
KW  - sol-gel
KW  - nonhydrolytic
UR  - http://sanfran2014onsite.acs.org/t/138905
N2  - Non-hydrolytic sol-gel reactions based on condensation of two functional groups are studied as an alternative to aqueous techniques for the synthesis of multimetallic oxides and inorganic-organic hybrid materials in the form of xerogels, nanoparticles, and thin films. We developed a non-hydrolytic sol-gel route based on acetic acid ester elimination providing parent phosphosilicate and its hybrid inorganic-organic derivatives. The polycondensation reactions between Si(OAc)4 and OP(OSiMe3)3 provides microporous phosphosilicate xerogels with surface areas up to 570 m2 g-1. Substitution reactions of residual acetoxy and trimethylsiloxy groups on the surface with a variety of reagents, such as SiCl4, RSiCl3, POCl3, AlX3, ROH, and Me3SiOSiMe3, show versatility of the synthesized phosphosilicate xerogels in tuning their properties, such as Bronsted and Lewis acidity. The consecutive substitution of Si and P precursors by acetoxysilanes 1RxSi(OC(O)CH3)4-x (1R = Me, Ph; x = 1-2) and trimethylsilylesters of phosphonic acid 2RP(O)(OSiMe3)2 (2R = c-Hex, Ph) caused the decrease of surface areas and increase of average pore sizes because of the lower cross-linking ability of the substituted precursors. To avoid a significant decrease of surface areas of hybrid xerogels we used as precursors acetoxysilanes and phosphonic acid esters with bridging alkyl or aryl groups, such as (AcO)3Si-(CH2)x-Si(OAc)3 (x = 1-3, 6) and (Me3SiO)2P(O)-3R-P(O)(OSiMe3)2 (3R = C2H4, C6H4). We were able to tune the pore size of resulting xerogels to the mesoporous range. The prepared xerogels were characterized by elemental analyses, solid-state 13C, 29Si, 31P NMR spectroscopy, IR spectroscopy, surface area analysis, thermal analysis TG/DSC, and XRD measurements.
ER  -

PINKAS, Jiří, Aleš STÝSKALÍK, David ŠKODA, Zdeněk MORAVEC a Craig E. BARNES. Mesoporous hybrid inorganic-organic phosphosilicates by non-hydrolytic sol-gel reactions. In \textit{248th American Chemical Society National Meeting \&{} Exposition, San Francisco, California, USA}. 2014. ISSN~0009-2347.

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