Nano zeolitic imidazolate frameworks crystal preparation method through dynamic crystallization
A metal-organic framework and dynamic crystallization technology, which is applied in organic chemistry, chemical instruments and methods, and crystal growth, can solve the problems of difficult preparation of nanocrystals and reduce the grain size of ZIFs materials, so as to shorten the nucleation time, Avoid the formation of large-sized crystals and reduce the effect of crystal size
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[0021] Example 1 Preparation of ZIF-7 nanocrystals
[0022] The configuration of ZIF-7 crystal synthesis mother liquor: 0.132g Zn(NO 3 ) 2 ·6H 2 O was fully dissolved in 20ml DMF to form solution A, and 0.432g benzimidazole (BIM) was dissolved in 20ml DMF to form solution B in another 50ml beaker. The solutions A and B are slowly mixed in an Erlenmeyer flask to form a crystal synthesis mother liquor.
[0023] Heating, stirring and crystallization process: immediately put the mixed crystal synthesis mother liquor in an oil bath that has been heated to 130°C, and at the same time turn on the magnetic stirrer to make all parts of the solution uniformly stirred, and the reaction is completed after 2 hours of dynamic crystallization. Quickly cool with cold water to terminate the crystal growth process, quickly centrifuge the product, wash and separate the solid phase with methanol, then place the solid phase in a vacuum oven and dry it at 30°C and 0.1Mpa vacuum.
[0024] Finally, the dri...
Example Embodiment
[0025] Example 2 Preparation of ZIF-9 nanocrystals
[0026] The configuration of ZIF-9 crystal synthesis mother liquor: 0.128g Co(NO 3 ) 2 ·6H 2 O was fully dissolved in 20ml DMF to form solution A, and 0.432g benzimidazole (BIM) was dissolved in 20ml DMF to form solution B in another 50ml beaker. The solutions A and B are slowly mixed in an Erlenmeyer flask to form a crystal synthesis mother liquor.
[0027] Heating, stirring and crystallization process: immediately place the mixed crystal synthesis mother liquor in an oil bath heated to 180°C, and turn on the magnetic stirrer at the same time to make each part of the solution be uniformly stirred, and the reaction ends after 1.5h of dynamic crystallization ,Quickly cool with cold water to end the crystal growth process, quickly centrifuge the product, and wash and separate the solid phase with methanol, and then place the solid phase in a vacuum oven at 30°C and a vacuum of 0.1Mpa to dry.
[0028] Finally, the dried product was di...
Example Embodiment
[0029] Example 3 Preparation of ZIF-8 nanocrystals
[0030] The configuration of ZIF-8 crystal synthesis mother liquor: 1.184g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 50 ml of water to form a solution A, 2.6 g of 2-methylimidazole (Hmim) was dissolved in another 50 ml of water to form a solution B, and solution A and solution B were slowly mixed to obtain a crystal synthesis mother liquor.
[0031] Heating, stirring and crystallization process: immediately put the mixed crystal synthesis mother liquor in a water bath heated to 40°C, and turn on the magnetic stirrer at the same time to make each part of the solution be uniformly stirred. The reaction is finished after 24 hours of dynamic crystallization. The cold water is rapidly cooled to end the crystal growth process, the product is quickly centrifuged, and the solid phase is washed with methanol and separated, and then the solid phase is placed in a vacuum oven at 30°C and a vacuum degree of 0.1Mpa for drying.
[0032] Finally, the d...
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