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Modulated Synthesis of Zr‐Based Metal–Organic Frameworks: From Nano to Single Crystals

Modulated Synthesis of Zr‐Based Metal–Organic Frameworks: From Nano to Single Crystals We present an investigation on the influence of benzoic acid, acetic acid, and water on the syntheses of the Zr‐based metal–organic frameworks Zr–bdc (UiO‐66), Zr–bdc–NH2 (UiO‐66–NH2), Zr–bpdc (UiO‐67), and Zr–tpdc–NH2 (UiO‐68–NH2) (H2bdc: terephthalic acid, H2bpdc: biphenyl‐4,4′‐dicarboxylic acid, H2tpdc: terphenyl‐4,4′′‐dicarboxylic acid). By varying the amount of benzoic or acetic acid, the synthesis of Zr–bdc can be modulated. With increasing concentration of the modulator, the products change from intergrown to individual crystals, the size of which can be tuned. Addition of benzoic acid also affects the size and morphology of Zr–bpdc and, additionally, makes the synthesis of Zr–bpdc highly reproducible. The control of crystal and particle size is proven by powder XRD, SEM and dynamic light scattering (DLS) measurements. Thermogravimetric analysis (TGA) and Ar sorption experiments show that the materials from modulated syntheses can be activated and that they exhibit high specific surface areas. Water proved to be essential for the formation of well‐ordered Zr–bdc–NH2. Zr–tpdc–NH2, a material with a structure analogous to that of Zr–bdc and Zr–bpdc, but with the longer, functionalized linker 2′‐amino‐1,1′:4′,1′′‐terphenyl‐4,4′′‐dicarboxylic acid, was obtained as single crystals. This allowed the first single‐crystal structural analysis of a Zr‐based metal–organic framework. http://www.deepdyve.com/assets/images/DeepDyve-Logo-lg.png Chemistry - A European Journal Wiley

Modulated Synthesis of Zr‐Based Metal–Organic Frameworks: From Nano to Single Crystals

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References (22)

Publisher
Wiley
Copyright
Copyright © 2011 Wiley Subscription Services, Inc., A Wiley Company
ISSN
0947-6539
eISSN
1521-3765
DOI
10.1002/chem.201003211
pmid
21547962
Publisher site
See Article on Publisher Site

Abstract

We present an investigation on the influence of benzoic acid, acetic acid, and water on the syntheses of the Zr‐based metal–organic frameworks Zr–bdc (UiO‐66), Zr–bdc–NH2 (UiO‐66–NH2), Zr–bpdc (UiO‐67), and Zr–tpdc–NH2 (UiO‐68–NH2) (H2bdc: terephthalic acid, H2bpdc: biphenyl‐4,4′‐dicarboxylic acid, H2tpdc: terphenyl‐4,4′′‐dicarboxylic acid). By varying the amount of benzoic or acetic acid, the synthesis of Zr–bdc can be modulated. With increasing concentration of the modulator, the products change from intergrown to individual crystals, the size of which can be tuned. Addition of benzoic acid also affects the size and morphology of Zr–bpdc and, additionally, makes the synthesis of Zr–bpdc highly reproducible. The control of crystal and particle size is proven by powder XRD, SEM and dynamic light scattering (DLS) measurements. Thermogravimetric analysis (TGA) and Ar sorption experiments show that the materials from modulated syntheses can be activated and that they exhibit high specific surface areas. Water proved to be essential for the formation of well‐ordered Zr–bdc–NH2. Zr–tpdc–NH2, a material with a structure analogous to that of Zr–bdc and Zr–bpdc, but with the longer, functionalized linker 2′‐amino‐1,1′:4′,1′′‐terphenyl‐4,4′′‐dicarboxylic acid, was obtained as single crystals. This allowed the first single‐crystal structural analysis of a Zr‐based metal–organic framework.

Journal

Chemistry - A European Journal – Wiley

Published: Jun 6, 2011

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