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通过调控DMSO/DMF/H2O混合溶剂中溶剂成分的物质的量比和反应温度,合成出3种基于1,3,5-三(4′-羧甲基苯基)苯(H3BTB)和氯化钴的钴簇基金属-有机框架化合物(NH2Me2)2[Co3O(BTB)2(H2O)].2H2O.4.5DMF.7.5DMSO(1),(NH2Me2)2[Co4O(BTB)8/3].6H2O.13DMSO(2)和(NH2Me2)2[Co6O3(BTB)8/3(H2O)4].5H2O.5DMF.13DMSO(3),它们分别含有三核Co3O簇、四核Co4O簇和六核Co6O3簇。这种六核簇为我们首次发现。研究表明,相对中等的温度105℃和较多DMF的使用有利于三核簇的形成;125℃高温和溶剂DMSO有利于四核簇的构建;与形成1的条件相比,较低的温度95℃和更多水的存在则有利于六核簇的生成。2和3虽然由不同的金属簇构成,但具有相同的框架结构,Schlfli符号为(43)8(48.64.812.104)3。此外,还研究了2和3抽出溶剂后产物的气体吸附性质,它们均具有较高的氢气吸附焓。
Three compounds based on 1,3,5-tris (4’-carboxymethylphenyl) benzene (H3BTB) and chlorination were synthesized by controlling the molar ratio of the solvent components in DMSO / DMF / H2O mixed solvent and the reaction temperature. Cobalt cobalt cluster-based metal-organic framework compound (NH2Me2) 2 [Co3O (BTB) 2 (H2O)] 2H2O.4.5DMF.7.5DMSO (1), (NH2Me2) 2 [Co4O (BTB) 8/3]. 6H2O.13DMSO (2) and (NH2Me2) 2 [Co6O3 (BTB) 8/3 (H2O) 4] .5H2O.5DMF.13DMSO (3) which respectively contain trinuclear Co3O clusters, tetranuclear Co4O clusters and hexanuclear Co6O3 cluster. This six-core cluster was first discovered by us. The results show that the relatively moderate temperature of 105 ℃ and the use of more DMF are beneficial to the formation of tri-nucleus clusters; the high temperature of 125 ℃ and the solvent DMSO favor the construction of tetranuclear clusters; compared with the formation of 1, the lower temperature of 95 The existence of ℃ and more water is conducive to the formation of six-core clusters. 2 and 3, although composed of different metal clusters, have the same framework structure and the Schlfli symbol is (43) 8 (48.64.812.104) 3. In addition, the gas adsorption properties of the products after 2 and 3 solvent extraction were also studied, both of which have higher enthalpy of hydrogen adsorption.