Journal
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
Volume 56, Issue 30, Pages 8874-8878Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/anie.201704044
Keywords
carbon dioxide; hysteresis; metal-organic frameworks; solvent exchange; sorption cycles
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Funding
- Department of Science and Technology
- National Research Foundation (South Africa)
- French Embassy in South Africa
- Labex CSC within the Investissement d'Avenir program [ANR-10-LABX-0026 CSC, ANR-10-IDEX-0002-02]
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A non-interpenetrated metal-organic framework with a paddle-wheel secondary building unit has been activated by direct thermal evacuation, guest exchange with a volatile solvent, and supercritical CO2 drying. Conventional thermal activation yields a mixture of crystalline phases and some amorphous content. Exchange with a volatile solvent prior to vacuum activation produces a pure breathing phase with high sorption capacity, selectivity for CO2 over N-2 and CH4, and substantial hysteresis. Supercritical drying can be used to access a guest-free open phase. Pressure-resolved differential scanning calorimetry was used to confirm and investigate a systematic loss of sorption capacity by the breathing phase as a function of successive cycles of sorption and desorption. A corresponding loss of sample integrity was not detectable by powder X-ray diffraction analysis. This may be an important factor to consider in cases where flexible MOFs are earmarked for industrial applications.
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