Thermal post-synthetic modification of Al-MIL-53–COOH : systematic investigation of the decarboxylation and condensation reaction

doi:10.1039/c2ce06649a

Thermal post-synthetic modification of Al-MIL-53–COOH ...

Bibliographic description

punktacja MNiSW [2012 A]: 35

title:	Thermal post-synthetic modification of Al-MIL-53–COOH : systematic investigation of the decarboxylation and condensation reaction
author:	Reimer Nele, Gil Barbara , Marszałek Bartosz , Stock Norbert
Journal title:	CrystEngComm
volume:	14
issue:	12
date of publication:	2012
pages:	4119-4125
eISSN:	1466-8033
DOI:	10.1039/c2ce06649a
language:	English
Journal language:	English
abstract in english:	Aluminium trimellitate [Al(OH)(BDC–COOH)] ? 0.9H 2 O( 1 ), the Al-MIL-53–COOH derivative, was discovered under solvothermal conditions using a high-throughput set-up suitable for microwave (MW)-assisted heating. The compound shows high structural flexibility. The large-pore (lp) form of the framework is obtained under large excess of H 2 O or after solvothermal treatment with N , N -dimethylformamide upon which [Al(OH)(BDC–COOH)] ? 0.7DMF ( 2 ) is obtained. Exposure of the water rich lp form of 1 to ambient conditions leads to the transformation to the narrow-pore (np) form. Thermal activation of both compounds results in the formation of the empty lp form and the activation of 1 was studied in detail by in situ IR-spectroscopy. Depending on the activation temperature and time two post-synthetic modification (PSM) processes are observed: the partial decarboxylation and the formation of acid anhydride groups. Thus at high temperatures and long activation times [Al(OH)(BDC–OCOCO–BDC) x /2 (BDC) y ]( x + y = 1) is formed. Upon cooling in air the anhydride functionality still remains intact, but the np form is obtained in air due to the adsorption of H 2 O molecules. Sorption measurements of 1 confirm a preference for polar gases like H 2 O and CO 2 in comparison to N 2 ,H 2 , and CH 4 . The N 2 capacity depends strongly on the degree of decarboxylation.
departmental parameterization:	35
affiliation:	Wydział Chemii : Zakład Chemii Nieorganicznej
type:	journal article
subtype:	academic paper