Non-aqueous template-assisted synthesis of mesoporous
nanocrystalline silicon orthophosphate

J 2015

Non-aqueous template-assisted synthesis of mesoporous nanocrystalline silicon orthophosphate

STÝSKALÍK, Aleš, David ŠKODA, Zdeněk MORAVEC, Pavla ROUPCOVÁ, Craig E. BARNES et. al.

Basic information

Original name

Non-aqueous template-assisted synthesis of mesoporous nanocrystalline silicon orthophosphate

Authors

STÝSKALÍK, Aleš (203 Czech Republic, belonging to the institution), David ŠKODA (203 Czech Republic, belonging to the institution), Zdeněk MORAVEC (203 Czech Republic, belonging to the institution), Pavla ROUPCOVÁ (203 Czech Republic), Craig E. BARNES (840 United States of America) and Jiří PINKAS (203 Czech Republic, guarantor, belonging to the institution)

Edition

RSC Advances, Cambridge, Royal Society of Chemistry, 2015, 2046-2069

Other information

Language

English

Type of outcome

Článek v odborném periodiku

Field of Study

10402 Inorganic and nuclear chemistry

Country of publisher

United Kingdom of Great Britain and Northern Ireland

Confidentiality degree

není předmětem státního či obchodního tajemství

Impact factor

Impact factor: 3.289

RIV identification code

RIV/00216224:14740/15:00084631

Organization unit

Central European Institute of Technology

DOI

http://dx.doi.org/10.1039/c5ra10982e

UT WoS

000360860500038

Keywords in English

PHOSPHORIC-ACID CATALYST; ORGANIC-INORGANIC HYBRID; SOL-GEL SYNTHESIS; PHOSPHOSILICATE GELS; AMBIENT CONDITIONS; CRYSTAL-STRUCTURE; MOLECULAR-SIEVES; SURFACE-AREA; MAS NMR; GLASSES

Abstract

V originále

The first synthesis of mesoporous nanocrystalline silicon orthophosphate Si5P6O25 is presented. The synthetic procedure is based on the non-hydrolytic sol-gel reaction in the presence of Pluronic P123 template and subsequent calcination in air. The condensation of silicon acetate, Si(OAc)(4), and tris(trimethylsilyl) phosphate, OP(OSiMe3)(3) (TTP), in non-aqueous solvents driven by elimination of trimethylsilyl acetate provides a homogeneous network with a high content of Si-O-P bonds and SiO6 moieties. After burning out the template, mesoporous silicon orthophosphate was obtained with surface areas up to 128 m(2) g(-1) and pore sizes around 20 nm. The nanocrystalline Si5P6O25 phase forms relatively easily (500 degrees C, 4 h) in comparison with other synthetic routes. All samples were characterized by SEM, TEM, elemental analysis, TGA, nitrogen adsorption, SAXS, H-1, C-13, Si-29, and P-31 solid-state NMR spectroscopy, and powder XRD. These xerogels showed superior catalytic activity and selectivity in methylstyrene dimerization.

Links

ED1.1.00/02.0068, research and development project

Name: CEITEC - central european institute of technology

LH11028, research and development project

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

Investor: Ministry of Education, Youth and Sports of the CR

Citovat

STÝSKALÍK, Aleš, David ŠKODA, Zdeněk MORAVEC, Pavla ROUPCOVÁ, Craig E. BARNES and Jiří PINKAS. Non-aqueous template-assisted synthesis of mesoporous nanocrystalline silicon orthophosphate. RSC Advances. Cambridge: Royal Society of Chemistry, 2015, vol. 5, No 90, p. 73670-73676. ISSN 2046-2069. Available from: https://dx.doi.org/10.1039/c5ra10982e.

@article{1316862,
   author = {Stýskalík, Aleš and Škoda, David and Moravec, Zdeněk and Roupcová, Pavla and Barnes, Craig E. and Pinkas, Jiří},
   article_location = {Cambridge},
   article_number = {90},
   doi = {http://dx.doi.org/10.1039/c5ra10982e},
   keywords = {PHOSPHORIC-ACID CATALYST; ORGANIC-INORGANIC HYBRID; SOL-GEL SYNTHESIS; PHOSPHOSILICATE GELS; AMBIENT CONDITIONS; CRYSTAL-STRUCTURE; MOLECULAR-SIEVES; SURFACE-AREA; MAS NMR; GLASSES},
   language = {eng},
   issn = {2046-2069},
   journal = {RSC Advances},
   title = {Non-aqueous template-assisted synthesis of mesoporous nanocrystalline silicon orthophosphate},
   volume = {5},
   year = {2015}
}

TY  - JOUR
ID  - 1316862
AU  - Stýskalík, Aleš - Škoda, David - Moravec, Zdeněk - Roupcová, Pavla - Barnes, Craig E. - Pinkas, Jiří
PY  - 2015
TI  - Non-aqueous template-assisted synthesis of mesoporous nanocrystalline silicon orthophosphate
JF  - RSC Advances
VL  - 5
IS  - 90
SP  - 73670-73676
EP  - 73670-73676
PB  - Royal Society of Chemistry
SN  - 20462069
KW  - PHOSPHORIC-ACID CATALYST
KW  - ORGANIC-INORGANIC HYBRID
KW  - SOL-GEL SYNTHESIS
KW  - PHOSPHOSILICATE GELS
KW  - AMBIENT CONDITIONS
KW  - CRYSTAL-STRUCTURE
KW  - MOLECULAR-SIEVES
KW  - SURFACE-AREA
KW  - MAS NMR
KW  - GLASSES
N2  - The first synthesis of mesoporous nanocrystalline silicon orthophosphate Si5P6O25 is presented. The synthetic procedure is based on the non-hydrolytic sol-gel reaction in the presence of Pluronic P123 template and subsequent calcination in air. The condensation of silicon acetate, Si(OAc)(4), and tris(trimethylsilyl) phosphate, OP(OSiMe3)(3) (TTP), in non-aqueous solvents driven by elimination of trimethylsilyl acetate provides a homogeneous network with a high content of Si-O-P bonds and SiO6 moieties. After burning out the template, mesoporous silicon orthophosphate was obtained with surface areas up to 128 m(2) g(-1) and pore sizes around 20 nm. The nanocrystalline Si5P6O25 phase forms relatively easily (500 degrees C, 4 h) in comparison with other synthetic routes. All samples were characterized by SEM, TEM, elemental analysis, TGA, nitrogen adsorption, SAXS, H-1, C-13, Si-29, and P-31 solid-state NMR spectroscopy, and powder XRD. These xerogels showed superior catalytic activity and selectivity in methylstyrene dimerization.
ER  -

STÝSKALÍK, Aleš, David ŠKODA, Zdeněk MORAVEC, Pavla ROUPCOVÁ, Craig E. BARNES and Jiří PINKAS. Non-aqueous template-assisted synthesis of mesoporous nanocrystalline silicon orthophosphate. \textit{RSC Advances}. Cambridge: Royal Society of Chemistry, 2015, vol.~5, No~90, p.~73670-73676. ISSN~2046-2069. Available from: https://dx.doi.org/10.1039/c5ra10982e.

Detailed Information on Publication Record