Non-hydrolytic sol-gel synthesis of zirconium phosphonates with controlled mesoporosity

Result code in IS VaVaI

<a href="https://www.isvavai.cz/riv?ss=detail&h=RIV%2F00216224%3A14310%2F23%3A00131672" target="_blank" >RIV/00216224:14310/23:00131672 - isvavai.cz</a>

Result on the web

<a href="https://doi.org/10.1016/j.micromeso.2023.112787" target="_blank" >https://doi.org/10.1016/j.micromeso.2023.112787</a>

DOI - Digital Object Identifier

<a href="http://dx.doi.org/10.1016/j.micromeso.2023.112787" target="_blank" >10.1016/j.micromeso.2023.112787</a>

Result language

angličtina

Original language name

Non-hydrolytic sol-gel synthesis of zirconium phosphonates with controlled mesoporosity

Original language description

We disclose the preparation of high-surface-area mesoporous zirconium phosphonates by the non-hydrolytic sol-gel reactions (NHSG) of Zr(NEt2)4 with trimethylsilylated phosphonates RP(O)(OSiMe3)2 (R = Me, tBu, Ph, OSiMe3), and bis-phosphonates (Me3SiO)2(O)P–X–P(O)(OSiMe3)2 (X = CH2, C6H4, CH2(C6H4)CH2, and CH2(C6H4)2CH2) in dry toluene under ambient pressure. Zirconium phosphonate xerogels are prepared by condensation reaction with the elimination of silylamine Me3SiNEt2. This irreversible reaction provides the amorphous xerogels and drives the formation of the porous structure. The influence of organic moieties bonded to phosphorus atoms on porosity was examined in this study. The final surface area of dried xerogels reached 720 m2 g−1 without any extra templating agent. Xerogels were characterized by 13C, 29Si, and 31P solid-state NMR to define atomic homogeneity and evidence the presence of organic phosphonate substituents and residual amido and trimethylsilyl groups. The amount of residual reactive groups was determined by gravimetric measurements and the thermal analysis (TG-DSC) method. These groups may be applied in post-synthetic surface modification, such as controlling the hydrophobic/hydrophilic properties. The catalytic properties of NHSG-prepared xerogels were tested on a model reaction of aminolysis of styrene oxide in a batch mode employing relatively bulky molecules. Products were identified and quantified by the 1H NMR spectroscopy. Catalyst performance parameters, such as selectivity, conversion, turnover frequency, and others, were exceeded compared to benchmark microporous layered zirconium phosphonate catalysts.

Czech name

—

Czech description

—

Type

J_imp - Article in a specialist periodical, which is included in the Web of Science database

CEP classification

—

OECD FORD branch

10402 - Inorganic and nuclear chemistry

Project

Result was created during the realization of more than one project. More information in the Projects tab.

Continuities

P - Projekt vyzkumu a vyvoje financovany z verejnych zdroju (s odkazem do CEP)<br>S - Specificky vyzkum na vysokych skolach

Publication year

2023

Confidentiality

S - Úplné a pravdivé údaje o projektu nepodléhají ochraně podle zvláštních právních předpisů

Name of the periodical

Microporous and Mesoporous Materials

ISSN

1387-1811

e-ISSN

1873-3093

Volume of the periodical

362

Issue of the periodical within the volume

December

Country of publishing house

NL - THE KINGDOM OF THE NETHERLANDS

Number of pages

10

Pages from-to

1-10

UT code for WoS article

001074508200001

EID of the result in the Scopus database

2-s2.0-85169571692