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Optimisation of synthesis conditions for UiO-66-CO2H towards scale-up and its vapour sorption properties
Reaction Chemistry & Engineering ( IF 3.4 ) Pub Date : 2018-04-18 00:00:00 , DOI: 10.1039/c7re00214a
Helge Reinsch 1, 2, 3, 4, 5 , Dominik Fröhlich 3, 6, 7 , Steve Waitschat 1, 2, 3 , Sachin Chavan 8, 9, 10, 11, 12 , Karl-Petter Lillerud 8, 9, 10, 11, 12 , Stefan Henninger 3, 6, 7 , Norbert Stock 1, 2, 3, 8, 9
Affiliation  

Based on the preferences of an industrial process for the production of MOFs we herein present a facile procedure for the synthesis of the zirconium based MOF UiO-66-CO2H with the composition [Zr6O4(OH)4(O2C–C4H3CO2H–CO2)6nH2O. The synthesis utilises Zr(SO4)2·4H2O and trimellitic acid (1,2,4-benzenetricarboxylic acid) in water as solvent. The product is already obtained after one hour under reflux with yields of 90% and extrapolated space–time yields up to 2000 kg m−3 d−1 can be achieved. The reaction is carried out at ambient pressure which is particularly beneficial for the potential production of the MOF at industrial scale. The vapour sorption properties and stabilities of UiO-66-CO2H were furthermore characterised in detail utilising methanol and water as fluids, respectively. While the harsh conditions for thermal water vapour cycling between 40 °C and 140 °C led to a rapid decline of sorption capacity, repeated cycling with methanol vapour did have a beneficial repairing effect on the framework's crystallinity.

中文翻译:

UiO-66-CO 2 H的大规模合成条件优化及其蒸气吸附性能

基于生产MOF的工业方法的偏爱,我们在这里提出了一种合成锆基MOF UiO-66-CO 2 H的简便方法,其组成为[Zr 6 O 4(OH)4(O 2 C -C 4 ħ 3 CO 2 H-CO 26ñ ħ 2 O的合成利用的Zr(SO 42 ·4H 2O和偏苯三酸(1,2,4-苯三甲酸)在水中作为溶剂。在回流下一小时后,已经获得了该产物,产率为90%,外推时空产率可以达到2000 kg m -3 d -1。该反应在环境压力下进行,这对于工业规模的MOF的潜在生产特别有利。UiO-66-CO 2的蒸气吸附特性和稳定性此外,分别利用甲醇和水作为流体对H进行了详细表征。尽管热水蒸气在40°C至140°C之间循环的苛刻条件导致吸附能力迅速下降,但用甲醇蒸气反复循环确实对骨架的结晶性产生了有益的修复作用。
更新日期:2018-04-18
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