Non-Hydrolytic Synthesis of Titanosilicate Xerogels by
Acetamide Elimination and their Use as Epoxidation Catalysts

J 2012

Non-Hydrolytic Synthesis of Titanosilicate Xerogels by Acetamide Elimination and their Use as Epoxidation Catalysts

STÝSKALÍK, Aleš, David ŠKODA, Jiří PINKAS and Sanjay MATHUR

Basic information

Original name

Non-Hydrolytic Synthesis of Titanosilicate Xerogels by Acetamide Elimination and their Use as Epoxidation Catalysts

Authors

STÝSKALÍK, Aleš (203 Czech Republic, belonging to the institution), David ŠKODA (203 Czech Republic, belonging to the institution), Jiří PINKAS (203 Czech Republic, guarantor, belonging to the institution) and Sanjay MATHUR (276 Germany)

Edition

Journal of Sol-Gel Science and Technology, Dordrecht, Springer Science + Business Media, 2012, 0928-0707

Other information

Language

English

Type of outcome

Článek v odborném periodiku

Field of Study

10402 Inorganic and nuclear chemistry

Country of publisher

Netherlands

Confidentiality degree

není předmětem státního či obchodního tajemství

References:

URL

Impact factor

Impact factor: 1.660

RIV identification code

RIV/00216224:14740/12:00057761

Organization unit

Central European Institute of Technology

DOI

http://dx.doi.org/10.1007/s10971-012-2808-5

UT WoS

000310162700020

Keywords in English

Non-hydrolytic; amide elimination; titanosilicate; epoxidation; catalysis

Abstract

V originále

Novel non-hydrolytic syntheses of titanosilicate xerogels by polycondensation of silicon acetate, Si(OAc)4, with titanium (IV) dimethylamide or diethylamide, Ti(NR2)4 (R = Me, Et), are presented. The reactions are based on acetamide elimination and yield gels with a high content of Si-O-Ti bonds in comparison with the ester elimination route. Although a ligand exchange was observed, it was interestingly not followed by homo-condensation and during the synthesis the phase separation to SiO2 and TiO2 was avoided. The degree of condensation reached up to 68 %. The xerogels prepared for a comparison by ester elimination from Si(OAc)4 and titanium (IV) isopropoxide featured a significantly lower content of the Si-O-Ti bonds. The initial tests in the epoxidation of cyclohexene by cumyl hydroperoxide (CHP) indicated a high selectivity and moderate activity of the xerogels. The catalytic properties were significantly improved by combining non-hydrolytic and hydrolytic methods yielding mesoporous and homogeneous Si/Ti mixed oxides. The catalysts prepared by these methods provided a complete epoxidation of cyclohexene in 2 h at 65 oC.

Links

ED1.1.00/02.0068, research and development project

Name: CEITEC - central european institute of technology

Files attached

SiOTi_nonhydrolSG_JSGST_2012_463-472.pdf

Request the author's version of the file

Citovat

STÝSKALÍK, Aleš, David ŠKODA, Jiří PINKAS and Sanjay MATHUR. Non-Hydrolytic Synthesis of Titanosilicate Xerogels by Acetamide Elimination and their Use as Epoxidation Catalysts. Journal of Sol-Gel Science and Technology. Dordrecht: Springer Science + Business Media, 2012, vol. 63, No 3, p. 463-472. ISSN 0928-0707. Available from: https://dx.doi.org/10.1007/s10971-012-2808-5.

@article{1071242,
   author = {Stýskalík, Aleš and Škoda, David and Pinkas, Jiří and Mathur, Sanjay},
   article_location = {Dordrecht},
   article_number = {3},
   doi = {http://dx.doi.org/10.1007/s10971-012-2808-5},
   keywords = {Non-hydrolytic; amide elimination; titanosilicate; epoxidation; catalysis},
   language = {eng},
   issn = {0928-0707},
   journal = {Journal of Sol-Gel Science and Technology},
   title = {Non-Hydrolytic Synthesis of Titanosilicate Xerogels by Acetamide Elimination and their Use as Epoxidation Catalysts},
   url = {http://link.springer.com/article/10.1007%2Fs10971-012-2808-5},
   volume = {63},
   year = {2012}
}

TY  - JOUR
ID  - 1071242
AU  - Stýskalík, Aleš - Škoda, David - Pinkas, Jiří - Mathur, Sanjay
PY  - 2012
TI  - Non-Hydrolytic Synthesis of Titanosilicate Xerogels by Acetamide Elimination and their Use as Epoxidation Catalysts
JF  - Journal of Sol-Gel Science and Technology
VL  - 63
IS  - 3
SP  - 463-472
EP  - 463-472
PB  - Springer Science + Business Media
SN  - 09280707
KW  - Non-hydrolytic
KW  - amide elimination
KW  - titanosilicate
KW  - epoxidation
KW  - catalysis
UR  - http://link.springer.com/article/10.1007%2Fs10971-012-2808-5
L2  - http://link.springer.com/article/10.1007%2Fs10971-012-2808-5
N2  - Novel non-hydrolytic syntheses of titanosilicate xerogels by polycondensation of silicon acetate, Si(OAc)4, with titanium (IV) dimethylamide or diethylamide, Ti(NR2)4 (R = Me, Et), are presented. The reactions are based on acetamide elimination and yield gels with a high content of Si-O-Ti bonds in comparison with the ester elimination route. Although a ligand exchange was observed, it was interestingly not followed by homo-condensation and during the synthesis the phase separation to SiO2 and TiO2 was avoided. The degree of condensation reached up to 68 %. The xerogels prepared for a comparison by ester elimination from Si(OAc)4 and titanium (IV) isopropoxide featured a significantly lower content of the Si-O-Ti bonds. The initial tests in the epoxidation of cyclohexene by cumyl hydroperoxide (CHP) indicated a high selectivity and moderate activity of the xerogels. The catalytic properties were significantly improved by combining non-hydrolytic and hydrolytic methods yielding mesoporous and homogeneous Si/Ti mixed oxides. The catalysts prepared by these methods provided a complete epoxidation of cyclohexene in 2 h at 65 oC.
ER  -

STÝSKALÍK, Aleš, David ŠKODA, Jiří PINKAS and Sanjay MATHUR. Non-Hydrolytic Synthesis of Titanosilicate Xerogels by Acetamide Elimination and their Use as Epoxidation Catalysts. \textit{Journal of Sol-Gel Science and Technology}. Dordrecht: Springer Science + Business Media, 2012, vol.~63, No~3, p.~463-472. ISSN~0928-0707. Available from: https://dx.doi.org/10.1007/s10971-012-2808-5.

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