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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Mixed-linker MOFs with CAU-10 structure: Synthesis and gas sorption characteristics
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Mixed-linker MOFs with CAU-10 structure: Synthesis and gas sorption characteristics

机译：具有CAU-10结构的混合接头MOF：合成和气体吸附特性

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摘要

The metal-organic framework compound [Al(OH)(BDC-Br)] (1) (BDC-Br _2- = 5-bromo-1,3-benzenedicarboxylate) denoted CAU-10-Br was synthesised under solvothermal reaction conditions. Its structure was successfully refined by Rietveld methods. The framework is based on the connection of infinite helical chains of cis-corner-sharing AlO 6-polyhedra via BDC-Br~2- ions. Thus non-intersecting parallel channels are formed, each periodically varying in diameter between 1.1 and 6.6 ?. Nevertheless 1 adsorbs CO2 at 298 K, while it is non-porous towards H2 and N2 at 77 K. Employing high-throughput (HT) methods we identified synthesis conditions that lead to the formation of mixed-linker MOFs with CAU-10 topology. Starting with a molar ratio H2B:H2BDC-Br = 3:1 we established a synthesis procedure for the partially bromo-functionalised mixed-linker-MOF [Al(OH)(BDC)0.8(BDC-Br)0.2] (2) denoted as CAU-10-H/Br. Starting with a molar ratio H2BDC-NH2:H 2BDC-NO2 = 1:1 the partially NO2- and NH 2-functionalised mixed-linker MOF [Al(OH)(BDC-NO2)0. 55(BDC-NH2)0.23(BDC-NHCHO)0.22] (3) denoted as CAU-10-NO2NH2 was synthesised, in which the NH 2-groups were found to be partially formylated. The partial bromo-functionalisation in CAU-10-H/Br (2) leads to a lower sorption capacity in comparison with the parent structure CAU-10-H, while the pore accessibility is comparable. The incorporation of NO2-, NH2- and NHCHO-groups in CAU-10-NO2/NH2 (3) does not only affect the accessibility of the pores for N2, but results also in an increased capacity for H2 and CO2 in comparison with the parent structure CAU-10-NO2. The reproducibility of the synthesis procedures was tested regarding the composition of the MOFs and the resulting gas sorption properties. In 2 a molar fraction of (BDC)2- = 80 ± 2% is found, while in 3 a molar fraction of (BDC-NO2) 2- = 55 ± 2% is observed. Starting from the molar ratio H 2BDC:H2BDC-CH3 = 1:1 mixed linker MOFs denoted as CAU-10-H/CH3 (4) were also obtained. In contrast to 2 and 3 the molar ratios of BDC2-/BDC-CH3 2- and especially the sorption properties differ substantially for every batch. The compounds were further characterised by X-ray powder diffraction, thermogravimetric/elemental analysis, NMR/Vis/IR-spectroscopy, and gas sorption measurements.
机译：在溶剂热反应条件下合成了表示为CAU-10-Br的金属-有机骨架化合物[Al（OH）（BDC-Br）]（1）（BDC-Br _2- = 5-溴-1,3-苯二甲酸）。其结构已通过Rietveld方法成功地完善。该框架基于通过BDC-Br〜2-离子连接顺角共享AlO 6-多面体的无限螺旋链。这样就形成了不相交的平行通道，每个通道的直径在1.1和6.6之间周期性变化。然而，1在298 K时会吸附CO2，而在77 K时则对H2和N2无孔。使用高通量（HT）方法，我们确定了导致形成具有CAU-10拓扑结构的混合连接MOF的合成条件。从摩尔比H2B：H2BDC-Br = 3：1开始，我们建立了部分溴官能化的混合连接基MOF [Al（OH）（BDC）0.8（BDC-Br）0.2]（2）的合成程序作为CAU-10-H / Br。从摩尔比H2BDC-NH2：H 2BDC-NO2 = 1：1开始，部分NO2-和NH 2官能化的混合连接基MOF [Al（OH）（BDC-NO2）0。合成了表示为CAU-10-NO2NH2的55（BDC-NH2）0.23（BDC-NHCHO）0.22]（3），其中发现NH 2-基团部分被甲酰化。与母体结构CAU-10-H相比，CAU-10-H / Br（2）中的部分溴官能化导致较低的吸附能力，而孔可达性却相当。在CAU-10-NO2 / NH2中掺入NO2-，NH2-和NHCHO基团（3）不仅影响孔对N2的可及性，而且与H2和CO2相比，还增加了H2和CO2的容量。母体结构CAU-10-NO2。关于MOF的组成和所得的气体吸附性能，测试了合成方法的可再现性。在2中发现（BDC）2- = 80±2％的摩尔分数，而在3中发现（BDC-NO2）2- = 55±2％的摩尔分数。从摩尔比H 2BDC：H2BDC-CH3 = 1：1开始，还获得了表示为CAU-10-H / CH3的混合连接基MOF（4）。与2和3相反，BDC 2-/ BDC-CH 3 2-的摩尔比，尤其是吸附性质对于每批基本上不同。通过X射线粉末衍射，热重/元素分析，NMR / Vis / IR光谱和气体吸收测量进一步表征化合物。

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