A kind of homogeneous metal organic framework material and its preparation method and application
A metal-organic framework and organic ligand technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of unobserved application prospects and high production costs, and achieve low reuse costs, low costs, and low isothermal adsorption enthalpy. Effect
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Embodiment 1
[0031] This example relates to a preparation method of N,N'-bis(3,5-dicarboxybenzene)-1,4,5,8-naphthalene diimide organic ligand, which specifically includes the following steps:
[0032] Add 1.81g of 5-amino-isophthalic acid and 1.34g of 1,4,5,8-naphthalene tetracarboxylic anhydride to 25mL of glacial acetic acid solution, react at 120°C for 15 hours, and after cooling down to room temperature, Filtrate, collect the precipitate, wash with distilled water until the pH value of the washing solution is neutral, and dry in vacuum at 80°C for 12 hours to obtain N,N'-bis(3,5-dicarboxybenzene)-1,4,5, 8-naphthalene diimide organic ligand 2.4g, yield 77%.
Embodiment 2
[0034] This embodiment relates to a method for preparing a homogeneous Cu-organic framework, which specifically includes the following steps:
[0035] 30 mg of N,N'-di(3,5-dicarboxybenzene)-1,4,5,8-naphthalene diimide obtained in Example 1 and 36 mg of Cu(NO 3 ) 2 ·3H 2 O dissolved in N,N'-dimethylformamide (DMF) / dioxane / H 2 O (5mL, volume ratio: 3:1:1) mixed solvent, then add 80μL of concentrated HCl, put it in a 20mL seed bottle, seal it and put it in an oven at 80°C for 72h, take it out and wash it repeatedly with DMF , the optical microscope showed a square green crystal, which is the prepared Cu-organic framework material. Its structure was determined by Agilent Technologies SuperNova single crystal diffractometer test, the test results show that: the crystal structure is [Cu 2 (C 30 h 10 N 2 o 12 )(H 2 O) 2 ](C 3 h 7 NO) 5 (H 2 O) 3 , belonging to the tetragonal crystal system, the space group is P42 1 2. The unit cell parameters are α=β=γ=90°, the unit...
Embodiment 3
[0050] This embodiment relates to a method for preparing a homogeneous Co-organic framework, which specifically includes the following steps:
[0051] 30 mg of N,N'-di(3,5-dicarboxybenzene)-1,4,5,8-naphthalene diimide obtained in Example 1 and 45 mg of Co(NO 3 ) 2 ·6H 2 O dissolved in N,N'-diethylformamide (DEF) / methanol / H 2 O (5mL, volume ratio: 3:1:1) mixed solvent, then add 80μL of concentrated HCl, put it in a 20mL strain bottle, seal it and put it in an oven at 80°C to react for 72, take it out and wash it repeatedly with DEF , to obtain metal-organic framework materials.
[0052] The metal-organic framework material obtained in this example is solvent-exchanged with anhydrous acetone, and the solvent is exchanged every half hour, at least ten times, and then activated under vacuum and 25°C for 12 hours, and then activated at 100°C After 12 hours, a metal-organic framework material with unsaturated metal sites and open pores was obtained. Micromeritics ASAP 2020 spec...
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