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

Inactive Publication Date: 2011-10-19
DALIAN UNIV OF TECH
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Problems solved by technology

[0005] The object of the present invention is to solve the difficult technical problem that metal-organic framework material (ZIFs) nano crystal is not easy to prepare, provides a kind of simple and easy, and the preparation method of ZIFs crystal that product crystal par

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  • Nano zeolitic imidazolate frameworks crystal preparation method through dynamic crystallization
  • Nano zeolitic imidazolate frameworks crystal preparation method through dynamic crystallization
  • Nano zeolitic imidazolate frameworks crystal preparation method through dynamic crystallization

Examples

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Example Embodiment

[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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Abstract

A nano zeolitic imidazolate frameworks crystal preparation method through dynamic crystallization. The method comprises the following steps: dissolving a metal precursor and an organic ligand in solvents respectively to prepare a metal precursor solution A and an organic ligand solution B; mixing the solution A and the solution B and placing the mixture in a reaction vessel with a stirring device; reacting at 30 DEG C-180 DEG C for 10min-96h, then cooling for crystal growth, and carrying out centrifugal separation and washing to obtain a target product. The method provided by the invention has simple synthesis conditions, is easy to operate and can effectively reduce crystal dimensions. Therefore, the method with a wide universality is suitable for various ZIFs crystal preparation.

Description

technical field [0001] The invention belongs to the technical field of new materials, and relates to a method for preparing zeolitic imidazolate framework compound (Zeolitic Imidazolate Frameworks, ZIFs) material nanocrystals under simple conditions, and expands the application range of ZIFs to the nanometer field. Background technique [0002] Nanocrystals refer to crystalline materials in the nanometer size range, or nanoparticles with a crystalline structure. Nanocrystals have always been a research hotspot for many researchers and have important research value. The electrical and thermodynamic properties of nano-sized crystals show strong size dependence, so the properties of nanoparticles can be controlled by adjusting the preparation process. Nanocrystals can also provide the crystal structure of the monomer. The study of the crystal structure of the monomer can provide information for explaining the behavior of macroscopic samples of similar materials, and also provid...

Claims

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Application Information

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IPC IPC(8): C30B7/14C30B28/04C07F19/00
Inventor 杨建华刘娟王金渠鲁金明谢忠殷慧敏张艳殷德宏
Owner DALIAN UNIV OF TECH
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