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High-yield, fluoride-free and large-scale synthesis of MIL-101(Cr)

: Zhao, T.; Jeremias, F.; Boldog, I.; Nguyen, B.; Henninger, S.K.; Janiak, C.

Fulltext ()

Dalton transactions 44 (2015), No.38, pp.16791-16801
ISSN: 1477-9226
ISSN: 2209-2386
ISSN: 1477-9234
Bundesministerium für Wirtschaft und Technologie BMWi
Journal Article, Electronic Publication
Fraunhofer ISE ()
adsorption; adsorption chiller; heat pump; MOF; scale up; Energieeffiziente Gebäude; Speichertechnologie; Servicebereiche; Energiekonzepte für Gebäude; Elektrische und thermische Wärmepumpen; Wärmeübertragung in gebäudetechnischen Anlagen; Latentwärmespeicher; ServiceLab Thermochemical and Porous Materials

MIL-101(Cr), one of the most important prototypical MOFs, is well investigated and widely used in many scientific fields. With regard to MOF synthesis in general, the addition of a modifier is commonly used to improve the properties of the products. The effect of inorganic (mineral) and organic acid modifiers was thoroughly investigated in the synthesis of MIL-101(Cr) and HNO3 could increase the yield to over 80% of a product with average S-BET > 3200 m(2) g(-1) in repeated experiments (from an average of 50% in most published syntheses) in small-scale laboratory synthesis. The large-scale synthesis could use the finding of HNO3 addition and produce MIL-101(Cr) in >100 g quantities with yields near 70% and BET-surface areas near 4000 m(2) g(-1). The addition of acetic acid (CH3COOH) together with seeding could decrease the reaction temperature, the lowest being 160 degrees C (from typically 220 degrees C in published procedures), with still relatively good yield and BET surface area of the product. The use of other strong inorganic or weak carboxylic acids as modulators typically caused a decrease in yield and porosity.