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Method for preparing nano zeolitic metal-organic frameworks crystal through dynamic crystallization

A metal-organic framework, dynamic crystallization technology, applied in organic chemistry, chemical instruments and methods, crystal growth, etc., can solve the problems of difficult preparation of nanocrystals, reduce the grain size of ZIFs materials, etc., to shorten the nucleation time, Avoid the formation of large-sized crystals, and the effect of simple synthesis conditions

Inactive Publication Date: 2013-05-15
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 particle is evenly distributed in nanoscale range, the present invention is effective Reducing the grain size of ZIFs materials also provides a certain experimental basis for the development of potential application fields of ZIFs materials and the study of growth mechanism

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  • Method for preparing nano zeolitic metal-organic frameworks crystal through dynamic crystallization
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  • Method for preparing nano zeolitic metal-organic frameworks crystal through dynamic crystallization

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Experimental program
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Effect test

Embodiment 1ZI

[0021] The preparation of embodiment 1ZIF-7 nanocrystal

[0022] The configuration of ZIF-7 crystal synthesis mother liquor: in the beaker of 50ml, 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. Slowly mix solutions A and B in a conical flask to form a mother liquor for crystal synthesis.

[0023] Heating, stirring and crystallization process: immediately put the mixed crystal synthesis mother solution in an oil bath that has been heated to 130°C, and at the same time turn on the magnetic stirrer to stir all parts of the solution evenly, and end the reaction after dynamic crystallization for 2 hours. Quench with cold water to terminate the crystal growth process, quickly centrifuge the product, wash and separate the solid phase with methanol, and then place the solid phase in a vacuum oven to dry at 30°C and 0.1Mpa vacuum.

[0024] Finally, t...

Embodiment 2ZI

[0025] The preparation of embodiment 2ZIF-9 nanocrystal

[0026] The configuration of ZIF-9 crystal synthesis mother liquor: in the beaker of 50ml, 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. Slowly mix solutions A and B in a conical flask to form a mother liquor for crystal synthesis.

[0027] Heating, stirring and crystallization process: immediately put the mixed crystal synthesis mother solution in an oil bath that has been heated to 180°C, and turn on the magnetic stirrer at the same time, so that all parts of the solution are evenly stirred, and the reaction is terminated after dynamic crystallization for 1.5 hours , quenched with cold water to end the crystal growth process, quickly centrifuged the product, washed and separated the solid phase with methanol, and then dried the solid phase in a vacuum oven at 30°C with a vacuum degree ...

Embodiment 3ZI

[0029] The preparation of embodiment 3ZIF-8 nanocrystal

[0030] The configuration of ZIF-8 crystal synthesis mother liquor: 1.184g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 50ml of water to form A solution, 2.6g of 2-methylimidazole (Hmim) was dissolved in another 50ml of water to form B solution, and solution A and solution B were slowly mixed to obtain a crystal synthesis mother solution.

[0031] Heating, stirring and crystallization process: immediately place the mixed crystal synthesis mother solution in a water bath that has been heated to 40°C, and at the same time turn on the magnetic stirrer to stir all parts of the solution evenly, and stop the reaction after 24 hours of dynamic crystallization. Quench with cold water to end the crystal growth process, quickly centrifuge the product, wash the solid phase with methanol, separate, and then place the solid phase in a vacuum oven at 30°C and dry at a vacuum of 0.1Mpa.

[0032] Finally, the dried product was dispersed in e...

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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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Patent Type & Authority Patents(China)
IPC IPC(8): C07F19/00C30B7/14C30B28/04
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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