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Cd(II)metal organic framework based on imidazole radicals nicotinoylhydrazones-containing organic ligand as well as preparation method and application thereof
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A metal-organic framework and organic ligand technology, applied in the fields of organic chemistry, separation methods, cadmium organic compounds, etc., can solve the problems of high space volume, decreased porosity, etc., and achieve the effect of good adsorption capacity
Active Publication Date: 2017-03-22
SHANDONG NORMAL UNIV
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Current MOFs can be divided into positively charged MOFs, neutrally charged MOFs, and negatively charged MOFs. Both positively charged MOFs and negatively charged MOFs contain counter ions, which lead to a sharp decrease in porosity.
The neutral MOF has a relatively high space volume, and has always been an ideal adsorption and separation material for small gas molecules and small organic molecules. Although many neutral MOFs are currently being studied, the pyridine acylhydrazone There are no reports on organic-like ligands and their use in self-assembly with Cd(II) inorganic salts
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preparation example Construction
[0043] Preparation of intermediate 5-imidazolyl nicotinic acid:
[0044]
[0045] N 2 Under protection, 5-bromonicotinic acid (3.0g, 15mmol), imidazole (1.4g, 21mmol), cesium carbonate (14.5g, 45mmol), cuprous iodide (0.6g, 3mmol) were added to a 150mL three-necked flask, 15mL of DMF was used as a solvent and heated in an oil bath at 120°C for 24h. After the reaction, pour it into 250mL of water, let it stand, and filter it with suction, adjust the pH of the filtrate to 5-6 with hydrochloric acid, filter it with suction, steam the filtrate to 1 / 3 to precipitate a solid, filter it with suction, and dry it in the air to obtain 1.6 g of a white solid. rate 56%. IR(v,cm -1 ):3436(w), 3126(w), 3100(w), 2402(w), 1693(m), 1604(s), 1511(m), 1437(w), 1339(s), 1287(m ),1121(w),1068(s),858(w),774(m),724(w),691(w),648(w),552(w). 1 H NMR (300MHz, CDCl 3 ,25℃,TMS,ppm):δ=9.15(s,1H,–C 5 h 3 N),9.01(s,1H,–C 5 h 3 N),8.46(s,1H,–C 5 h 3 N),8.44(s,1H,–C 3 h 3 N 2 ), 7.93-7.95 (d...
Embodiment 1
[0057] The organic ligand L (3mg, 0.01mmol), CdBr 2 (8.16mg, 0.03mmol) was dissolved in 2mL N,N-dimethylformamide (DMF), kept at 90°C for 72 hours, and cooled to room temperature to obtain CdBr-MOF. The infrared spectrum is as follows image 3 As shown, the TGA spectrum is as Figure 4 As shown, the PXRD spectrum is shown in 7. The crystal data of Example 1 are shown in Attached Table 1.
Embodiment 2
[0059] The preparation of organic ligand L is the same as in Example 1;
[0060] The organic ligand L (3mg, 0.01mmol), CdCl 2 (5.50mg, 0.03mmol) was dissolved in 2mL N,N-dimethylformamide (DMF), kept at 90°C for 72 hours, and cooled to room temperature to obtain CdCl-MOF. The PXRD characterization of the product is as follows Figure 7 shown.
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Abstract
The invention discloses a Cd(II)metal organic framework based on an imidazole radicals nicotinoylhydrazones-containing organic ligand as well as a preparation method and an application thereof. A structural formula is CdmLnXa, wherein, m equals n or a, and m, n and a are natural numbers, X is NO3<->, Cl<->, Br<-> and I<->, L is an organic ligand L, a structural formula of the organic ligand is shown as a specification, the organic ligand L and CdX2 are added into a solvent, the materials are uniformly mixed, then heated, and the Cd(II)metal organic framework is obtained after the reaction. The metal organic framework has good adsorption capability on gas molecules under room temperature.
Description
technical field [0001] The invention belongs to the technical field of preparation of inorganic-organic nanometer materials, and in particular relates to an organic ligand containing imidazolyl nicotinyl hydrazone, a metal-organic framework based on the organic ligand and Cd(II) ions, and a preparation method thereof. Background technique [0002] Metal-organic Framework (MOF) is a research hotspot in recent years. Compared with traditional porous materials, MOF has the characteristics of porosity, larger specific surface area and pore volume in the framework. MOFs are efficient materials for gas adsorption due to their high specific surface area, high porosity, and high stability. Since MOFs materials have adjustable pore sizes, designing MOFs materials with suitable pore sizes for CO 2 Specific adsorption separation is a way to reduce greenhouse gases. [0003] At present, metal-organic framework compounds with large porosity and large-sized tunnels are research hotspots...
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