Preparation method of nanometer-to-micrometer scale zeolitic imidazolate frameworks (ZIFs)

A technology of zeolite imidazole framework and structural material, which is applied in the directions of cobalt organic compounds, zinc organic compounds, etc., can solve the problems of restricting the large-scale industrial production of zeolite imidazole framework materials, difficult to control the crystal size, harsh reaction conditions, etc., and achieve controllable size. Wide range, reduced ligand dosage, good morphology

Active Publication Date: 2012-10-17
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] So far, most of the reported ZIFs have been synthesized using traditional solvothermal synthesis methods. For example, US Patent Publication US 2007/0202038A discloses a production method of a functional zeolite structure, using N,N-dimethylformamide or butanol as Solvent, heated to 120-150°C, and reacted for 24-72 hours to prepare ZIFs. The reaction conditions of this method are harsh, the reaction time is long, and the preparation process is complicated
Some other methods for preparing zeolite imidazole structures reported in the literature are such as ball milling (references Patrick J.Beldon, LászlóFábián, Robin S.Stein, A.Thirumurugan, Anthony K.Cheetham, Tomislav Angewandte Chemie International Edition, 2010,49,9640-9643), preparation method is simple but preparation kind is limited; Water vapor assisted synthesis method (reference literature Qi Shi, Zhaofeng Chen, Zhengwei Song, Jinping Li, Jinxiang Dong, Angewandte Chemie International Edition , 2011,50,

Method used

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  • Preparation method of nanometer-to-micrometer scale zeolitic imidazolate frameworks (ZIFs)
  • Preparation method of nanometer-to-micrometer scale zeolitic imidazolate frameworks (ZIFs)
  • Preparation method of nanometer-to-micrometer scale zeolitic imidazolate frameworks (ZIFs)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The synthetic method of zeolite imidazole framework material ZIF-8 is as follows: under room temperature, dissolve mIm (2-methylimidazole) in 20ml water, make its concentration be 0.2M, add ammonia water and adjust its pH to be 11.00, add nitric acid while stirring The zinc solid particles were adjusted to a concentration of 0.1M, stirred for 15 minutes, the obtained precipitate was washed with water and centrifuged, and the supernatant was discarded. Repeat the washing and centrifuging operation 3 times, then heat and dry at 60°C for 10 hours. Carry out XRD characterization to sample, as shown in the figure, can find out that synthesized product and ZIF-8 standard XRD spectrogram (K.Park, Z.Ni, A.Cote, J.Choi, R, Huang, F.Uribe-Romo , H.Chae, M.O'Keeffe, O.Yaghi, Prov.Natl.Acad.Sci.U.S.A., 2006, 103, 10189-10191.) coincide, the cleanliness of the surface sample is good, and the sample is pure. Some samples were taken and characterized by SEM. It can be seen that the o...

Embodiment 2

[0019] Check the impact of adding alkaline substances on the prepared product: under room temperature, dissolve mIm (2-methylimidazole) in 20ml water, make its concentration 0.1M, measure the pH value of the solution to 10.21, add zinc nitrate solid while stirring The pellet was brought to a concentration of 0.1 M and stirred for 15 minutes, the resulting precipitate was washed with water and centrifuged, and the supernatant was discarded. Repeat the washing and centrifuging operation at least 3 times, and heat and dry at 60°C for 10 hours. Some samples were taken for XRD characterization. As shown in the figure, it can be seen that the synthesized product does not match the standard XRD spectrum of ZIF-8 and the difference is very large, indicating that the prepared product is not the target product. Under the synthesis conditions, no alkaline Substance cannot synthesize ZIF-8.

Embodiment 3

[0021] Check and adjust the pH value of the solution to affect the prepared product. At room temperature, dissolve mIm (2-methylimidazole) in 20ml water to make its concentration 0.1M. Add ammonia water to adjust the pH to 11.50, and add zinc nitrate solid particles while stirring. , so that the concentration was 0.1M, stirred for 15 minutes, the obtained precipitate was washed with water and centrifuged, and the supernatant was discarded. Repeat the washing and centrifuging operation at least 3 times, and heat and dry at 60°C for 10 hours. Some samples were taken for XRD characterization, as shown in the figure, it can be seen that the synthesized product is consistent with the ZIF-8 standard XRD spectrum, indicating that the sample is pure. Compared with Example 1, the crystallinity of the sample is improved. Some samples were taken and characterized by SEM. It can be seen that the obtained ZIF-8 material is a polyhedron with a particle size of about 100-200nm. Compared wi...

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Abstract

The invention which belongs to the technical field of new materials relates to a synthetic method of ZIFs, and concretely discloses a method for synthesizing nanometer/micrometer scale ZIFs based on imidazole and its derivatives at room temperature in a concise, efficient and green manner. The method comprises the following steps: dissolving a single imidazole ligand or a mixture of two imidazole ligands in water or an organic liquid to form a solution, adding an alkaline substance to adjust the pH value of the solution, adding a metal salt to form a reaction system, and reacting to obtain the nanometer or micrometer scale ZIFs. The method which allows routine reactants to be utilized and the alkaline substance to be added to adjust the pH value of the system has the advantages of ligand application amount reduction, controllable product size, and high purity of the nanometer/micrometer scale ZIFs. The synthetic method has the characteristics of cheap and easily available raw materials and solvent, and no pollution, and has important meanings to the production and the application of the ZIFs.

Description

technical field [0001] The invention belongs to the technical field of new materials, and relates to a method for synthesizing zeolite imidazole framework materials (ZIFs). Background technique [0002] Zeolitic imidazole frameworks (ZIFs) are a class of nitrogen-containing heterocyclic metal-organic frameworks (MOFs) with organic imidazolates as linking ligands, which are similar in structure to traditional zeolite molecular sieves, with transition metal ions such as Zn or Co substituted The Si element and Al element in the traditional zeolite molecular sieve, imidazole or imidazole derivatives replace the bridging oxygen in the traditional zeolite molecular sieve, and form a coordination polymer through the assembly of the N atom on the imidazole ring and the transition metal. In addition to the large specific surface area and porous properties of conventional MOFs, ZIFs also have high thermal stability (>673K), chemical stability and moisture resistance due to the stro...

Claims

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Application Information

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IPC IPC(8): C07F3/06C07F15/06
Inventor 柴永明刘杜鹏刘晨光徐彪郭海玲戴昉纳
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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