四种多重穿插结构MOFs的合成及在气相色谱上分离香料的应用
发布时间：2019-06-02 20:28
【摘要】：金属-有机骨架材料(Metal-Organic Frameworks,MOFs)作为一种新型的功能材料,因具有高的比表面积、丰富的拓扑结构、持久性的孔道结构以及可修饰的孔道表面等特点,在气体储存、催化剂、吸附分离、传感等许多领域具有广阔的应用前景。多重穿插结构的MOFs是金属-有机骨架材料的重要分支,由于具有穿插结构增强了结构稳定性,同时具有高的热稳定性等特点引起人们广泛关注。目前,将穿插结构的MOFs用于色谱固定相分离的例子很少。本文合成四种穿插结构的MOFs,制备成毛细管柱作为固定相用于气相色谱分离肉桂、薄荷等香料。1通过溶剂热法成功合成一种新型四重穿插金属-有机骨架材料[Ni(pybz)2]·DMF(1),这是一个四重穿插、具有金刚石拓扑结构的MOF,在c方向有一个尺寸为7.6?′7.6?的一维通道。采用动态涂覆法将其制备成毛细管气相色谱柱,在气相色谱上成功分离了包含醇、醛、酮、酸、酯、醚等的六组香料,对分离机理进行探讨并模拟计算MOF与香料间的范德华力大小。结果显示:这种固定相对这些香料具有很好分离能力,模拟计算结果与色谱分离结果吻合。这是第一例将四重穿插的MOF做固定相在气相色谱上分离香料。2通过水热法成功合成出两种四重穿插结构的金属-有机骨架材料,[Zn(D.Cam)(tmdpy)]·H_2O(2)和[Cd(D.Cam)(tmdpy)](3),它们有相同的手性金刚石拓扑结构。这两个MOFs都是由一个可伸缩的手性“Z”桥连链状配体tmdpy形成3D结构,再自组装成四重穿插的3D手性MOFs。将它制备成毛细管柱在气相色谱上成功分离了六组香料。实验结果表明:这两种固定相都能将六组香料较好的分离开,但3涂覆的毛细管柱的分离能力比2好。3通过水热法成功合成出了三重穿插结构的金属-有机骨架材料[Ni(D.Cam)(tmdpy)](4),它具有一种罕见的4-连接双层的单元,它与相邻的配体tmdpy连接形成三重穿插的三维超分子结构。采用动态涂覆法将它制备成毛细管柱在气相色谱上成功分离了五组香料。实验结果表明,该MOF涂覆的毛细管柱对五组不同官能团(R-OH,H-C(R)=O,C(RR’)=O,HO-(R)C=O,R-O-(R’)C=O,R-O-R’)取代的直链、芳香结构化合物以及环烷烃具有良好的分离能力。
[Abstract]:Metal-organic skeleton material (Metal-Organic Frameworks,MOFs), as a new functional material, is stored in gas because of its high specific surface area, rich topological structure, persistent pore structure and modifiable pore surface. Catalysts, adsorption separation, sensing and many other fields have broad application prospects. MOFs with multiple interlaced structures is an important branch of metal-organic skeleton materials. Because of its interlaced structure, it enhances the structural stability and has high thermal stability. At present, there are few examples of using interlaced MOFs for chromatographic stationary phase separation. In this paper, four kinds of interlaced MOFs, were synthesized to prepare capillary column as stationary phase for the separation of cinnamon by gas chromatography. A new type of metal-organic skeleton material [Ni (pybz) 2] DMF (1) was successfully synthesized by solvothermal method, which is a quadruple intercalated MOF, with diamond topological structure. 1. A new type of metal-organic skeleton material [DMF 2] DMF (1) has been successfully synthesized by solvothermal method. There is a size of 7.6 鈮，
本文编号：2491406
[Abstract]:Metal-organic skeleton material (Metal-Organic Frameworks,MOFs), as a new functional material, is stored in gas because of its high specific surface area, rich topological structure, persistent pore structure and modifiable pore surface. Catalysts, adsorption separation, sensing and many other fields have broad application prospects. MOFs with multiple interlaced structures is an important branch of metal-organic skeleton materials. Because of its interlaced structure, it enhances the structural stability and has high thermal stability. At present, there are few examples of using interlaced MOFs for chromatographic stationary phase separation. In this paper, four kinds of interlaced MOFs, were synthesized to prepare capillary column as stationary phase for the separation of cinnamon by gas chromatography. A new type of metal-organic skeleton material [Ni (pybz) 2] DMF (1) was successfully synthesized by solvothermal method, which is a quadruple intercalated MOF, with diamond topological structure. 1. A new type of metal-organic skeleton material [DMF 2] DMF (1) has been successfully synthesized by solvothermal method. There is a size of 7.6 鈮，
本文编号：2491406
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