Hybrid organosilicate materials by non-hydrolytic sol-gel
synthesis

a 2013

Hybrid organosilicate materials by non-hydrolytic sol-gel synthesis

PINKAS, Jiří, Martin KEJÍK, Zdeněk MORAVEC and Craig BARNES

Basic information

Original name

Hybrid organosilicate materials by non-hydrolytic sol-gel synthesis

Authors

PINKAS, Jiří (203 Czech Republic, guarantor, belonging to the institution), Martin KEJÍK (203 Czech Republic, belonging to the institution), Zdeněk MORAVEC (203 Czech Republic, belonging to the institution) and Craig BARNES (840 United States of America)

Edition

3rd International Conference on Multifunctional, Hybrid and Nanomaterials, Sorrento, Italy, 2013

Other information

Language

English

Type of outcome

Konferenční abstrakt

Field of Study

10402 Inorganic and nuclear chemistry

Country of publisher

Italy

Confidentiality degree

není předmětem státního či obchodního tajemství

RIV identification code

RIV/00216224:14740/13:00069401

Organization unit

Central European Institute of Technology

Keywords in English

Organosilicate; Hybrid Materials; Non-Hydrolytic; Sol-Gel

Abstract

V originále

A non-hydrolytic sol-gel synthesis of new hybrid organosilicate materials containing various phenolic and bisphenolic structural motifs was developed. Mesoporous gels are formed in polycondensation reactions of multifunctional phenols, such as hydroquinone, 4,4-dihydroxybiphenyl, bisphenol A, and phloroglucinol with silicon(IV) acetate in polar ether solvent. Acetic acid was identified as an elimination reaction byproduct. Xerogels were obtained upon drying in vacuo and the produced materials contain residual acetoxy and phenolic hydroxyl groups allowing for later grafting and surface modification. An impact of employed spacer molecule and reaction conditions on the degree of condensation and xerogel porosity was studied. Condensation degree was established by gravimetric techniques and appears to be independent of reaction temperature but strongly depends on the nature of the spacer molecule. Hydroquinone provided gels with the highest value of 91%. Surface area of xerogels depends both on reaction temperature and the phenol ligand. A higher reaction temperature leads to a larger surface area; phloroglucinol providing gel with up to 790 m2/g of surface. Additionally a study of grafting organic groups on the gel surface by the reactions with alcohols and phenols and anchoring of aluminum species by treating the gels with compounds such as AlR3 and AlX3 was performed. All the prepared xerogels and modified materials were characterized by elemental analyses, solid-state 13C, 27Al, and 29Si NMR, IR spectroscopy, surface area analysis, thermal analysis TG/DSC, and XRD.

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

PINKAS, Jiří, Martin KEJÍK, Zdeněk MORAVEC and Craig BARNES. Hybrid organosilicate materials by non-hydrolytic sol-gel synthesis. In 3rd International Conference on Multifunctional, Hybrid and Nanomaterials, Sorrento, Italy. 2013.

@proceedings{1122956,
   author = {Pinkas, Jiří and Kejík, Martin and Moravec, Zdeněk and Barnes, Craig},
   booktitle = {3rd International Conference on Multifunctional, Hybrid and Nanomaterials, Sorrento, Italy},
   keywords = {Organosilicate; Hybrid Materials; Non-Hydrolytic; Sol-Gel},
   language = {eng},
   title = {Hybrid organosilicate materials by non-hydrolytic sol-gel synthesis},
   year = {2013}
}

TY  - CONF
ID  - 1122956
AU  - Pinkas, Jiří - Kejík, Martin - Moravec, Zdeněk - Barnes, Craig
PY  - 2013
TI  - Hybrid organosilicate materials by non-hydrolytic sol-gel synthesis
KW  - Organosilicate
KW  - Hybrid Materials
KW  - Non-Hydrolytic
KW  - Sol-Gel
N2  - A non-hydrolytic sol-gel synthesis of new hybrid organosilicate materials containing various phenolic and bisphenolic structural motifs was developed. Mesoporous gels are formed in polycondensation reactions of multifunctional phenols, such as hydroquinone, 4,4-dihydroxybiphenyl, bisphenol A, and phloroglucinol with silicon(IV) acetate in polar ether solvent. Acetic acid was identified as an elimination reaction byproduct. Xerogels were obtained upon drying in vacuo and the produced materials contain residual acetoxy and phenolic hydroxyl groups allowing for later grafting and surface modification. An impact of employed spacer molecule and reaction conditions on the degree of condensation and xerogel porosity was studied. Condensation degree was established by gravimetric techniques and appears to be independent of reaction temperature but strongly depends on the nature of the spacer molecule. Hydroquinone provided gels with the highest value of 91%. Surface area of xerogels depends both on reaction temperature and the phenol ligand. A higher reaction temperature leads to a larger surface area; phloroglucinol providing gel with up to 790 m2/g of surface. Additionally a study of grafting organic groups on the gel surface by the reactions with alcohols and phenols and anchoring of aluminum species by treating the gels with compounds such as AlR3 and AlX3 was performed. All the prepared xerogels and modified materials were characterized by elemental analyses, solid-state 13C, 27Al, and 29Si NMR, IR spectroscopy, surface area analysis, thermal analysis TG/DSC, and XRD.
ER  -

PINKAS, Jiří, Martin KEJÍK, Zdeněk MORAVEC and Craig BARNES. Hybrid organosilicate materials by non-hydrolytic sol-gel synthesis. In \textit{3rd International Conference on Multifunctional, Hybrid and Nanomaterials, Sorrento, Italy}. 2013.

Detailed Information on Publication Record