Aluminophosphate and -phosphonate Xerogels by Non-Hydrolytic
Sol-Gel Reactions

a 2019

Aluminophosphate and -phosphonate Xerogels by Non-Hydrolytic Sol-Gel Reactions

PINKAS, Jiří, Petr MACHÁČ, Ján PODHORSKÝ, Zdeněk MORAVEC, Aleš STÝSKALÍK et. al.

Základní údaje

Originální název

Aluminophosphate and -phosphonate Xerogels by Non-Hydrolytic Sol-Gel Reactions

Autoři

PINKAS, Jiří, Petr MACHÁČ, Ján PODHORSKÝ, Zdeněk MORAVEC a Aleš STÝSKALÍK

Vydání

20th International Sol-Gel Conference, Sankt Peterburg, Russia, 2019

Další údaje

Jazyk

angličtina

Typ výsledku

Konferenční abstrakt

Obor

10402 Inorganic and nuclear chemistry

Stát vydavatele

Rusko

Utajení

není předmětem státního či obchodního tajemství

Organizační jednotka

Přírodovědecká fakulta

Klíčová slova anglicky

aluminophosphates; Aluminophosphonates; non-hydrolytic sol-gel reactions

Příznaky

Mezinárodní význam, Recenzováno

Změněno: 9. 8. 2019 21:53, prof. RNDr. Jiří Pinkas, Ph.D.

Anotace

V originále

We have investigated the preparation of high-surface area mesoporous aluminophosphates and aluminophosphonates by non-hydrolytic sol-gel reactions. The first synthetic method is based on reactions of EtAlCl2 with trialkylesters of phosphoric acid (OP(OR)3, R = Me, Et, iPr, nBu, in dry organic solvents. The condensations proceed by alkylchloride elimination. Various reaction and calcination conditions were examined. Porosity is obtained after calcination by removal of organic residual groups. This thermal processing at 300 °C of as-synthesized precursor gels leads to amorphous aluminophosphate xerogels with surface areas of 400–500 m2 g–1 provided by small mesopores (2–8 nm). Changes in coordination environment of aluminium from six- to four-coordinate are evidenced by shift of 27Al MAS NMR resonances. The second method involves reaction of Al(NMe2)3 with trimethylsilylated phosphate, phosphonate, and bis-phosphonate esters in dry toluene. The reactions proceed by silylamine elimination and provide organic-inorganic hybrid xerogels with properties influenced by organic substituents and the Al:P ratio of the precursors. Dried xerogels exhibit large surface areas (up to 1000 m2 g-1) and Al–O–P networks stay stable under medium high thermal conditions. 27Al, 13C, and 29Si MAS NMR was employed to characterize aluminum coordination and residual amido and trimethylsilyl groups. The amount of residual groups was determined by gravimetric measurements and by thermal TG-DSC analysis. These unreacted groups have the potential to be used in post-synthetic grafting of catalytically active metal centers.

Návaznosti

LM2015043, projekt VaV

Název: Česká infrastruktura pro integrativní strukturní biologii (Akronym: CIISB)

Investor: Ministerstvo školství, mládeže a tělovýchovy ČR, Czech Infrastructure for Integrative Structural Biology

LQ1601, projekt VaV

Název: CEITEC 2020 (Akronym: CEITEC2020)

Investor: Ministerstvo školství, mládeže a tělovýchovy ČR, CEITEC 2020

Citovat

PINKAS, Jiří, Petr MACHÁČ, Ján PODHORSKÝ, Zdeněk MORAVEC a Aleš STÝSKALÍK. Aluminophosphate and -phosphonate Xerogels by Non-Hydrolytic Sol-Gel Reactions. In 20th International Sol-Gel Conference, Sankt Peterburg, Russia. 2019.

@proceedings{1548907,
   author = {Pinkas, Jiří and Macháč, Petr and Podhorský, Ján and Moravec, Zdeněk and Stýskalík, Aleš},
   booktitle = {20th International Sol-Gel Conference, Sankt Peterburg, Russia},
   keywords = {aluminophosphates; Aluminophosphonates; non-hydrolytic sol-gel reactions},
   language = {eng},
   title = {Aluminophosphate and -phosphonate Xerogels by Non-Hydrolytic Sol-Gel Reactions},
   year = {2019}
}

TY  - CONF
ID  - 1548907
AU  - Pinkas, Jiří - Macháč, Petr - Podhorský, Ján - Moravec, Zdeněk - Stýskalík, Aleš
PY  - 2019
TI  - Aluminophosphate and -phosphonate Xerogels by Non-Hydrolytic Sol-Gel Reactions
KW  - aluminophosphates
KW  - Aluminophosphonates
KW  - non-hydrolytic sol-gel reactions
N2  - We have investigated the preparation of high-surface area mesoporous aluminophosphates and aluminophosphonates by non-hydrolytic sol-gel reactions. The first synthetic method is based on reactions of EtAlCl2 with trialkylesters of phosphoric acid (OP(OR)3, R = Me, Et, iPr, nBu, in dry organic solvents. The condensations proceed by alkylchloride elimination. Various reaction and calcination conditions were examined. Porosity is obtained after calcination by removal of organic residual groups. This thermal processing at 300 °C of as-synthesized precursor gels leads to amorphous aluminophosphate xerogels with surface areas of 400–500 m2 g–1 provided by small mesopores (2–8 nm). Changes in coordination environment of aluminium from six- to four-coordinate are evidenced by shift of 27Al MAS NMR resonances. The second method involves reaction of Al(NMe2)3 with trimethylsilylated phosphate, phosphonate, and bis-phosphonate esters in dry toluene. The reactions proceed by silylamine elimination and provide organic-inorganic hybrid xerogels with properties influenced by organic substituents and the Al:P ratio of the precursors. Dried xerogels exhibit large surface areas (up to 1000 m2 g-1) and Al–O–P networks stay stable under medium high thermal conditions. 27Al, 13C, and 29Si MAS NMR was employed to characterize aluminum coordination and residual amido and trimethylsilyl groups. The amount of residual groups was determined by gravimetric measurements and by thermal TG-DSC analysis. These unreacted groups have the potential to be used in post-synthetic grafting of catalytically active metal centers.
ER  -

PINKAS, Jiří, Petr MACHÁČ, Ján PODHORSKÝ, Zdeněk MORAVEC a Aleš STÝSKALÍK. Aluminophosphate and -phosphonate Xerogels by Non-Hydrolytic Sol-Gel Reactions. In \textit{20th International Sol-Gel Conference, Sankt Peterburg, Russia}. 2019.

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