Microporous metal-organic framework material as well as preparation method and application thereof

An organic framework and metal technology, applied in the field of microporous metal-organic framework materials and their preparation, can solve the problems of reducing application value and structural stability

Inactive Publication Date: 2011-11-23
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The loss of guest molecules will greatly reduce the stability of the o

Method used

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  • Microporous metal-organic framework material as well as preparation method and application thereof
  • Microporous metal-organic framework material as well as preparation method and application thereof
  • Microporous metal-organic framework material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1 Preparation of Zn(pybdc) microporous metal-organic framework material.

[0018] Weigh Zn(AcO) 2 2H 2 O 0.025 g (0.1 mmol), H 2 pybdc 0.02 g (0.1 mmol), dissolved in 8 mL of deionized water and 2 mL of absolute ethanol, stirred at room temperature for 2 hours, and transferred the suspension to a 15 mL stainless steel reactor with a Teflon liner , crystallized at 140° for 72 hours, cooled to room temperature, brown transparent needle-like crystal Zn (pybdc) was precipitated, filtered, washed, and dried to obtain 25 mg. Yield 55.5%. The X-ray diffraction pattern of the product and the simulated X-ray diffraction pattern of a single crystal are shown in figure 2 .

Embodiment 2

[0019] Example 2 Structural characterization of Zn(pybdc) microporous metal-organic framework materials.

[0020] The single crystal X-ray diffraction data were measured on Bruker's SMART APEX CCD single crystal diffractometer, and the diffraction data were collected by Mo / Ka rays (λ= 0.71073 ?) and ω scanning. The unit cell parameters and orientation matrix are corrected by the least square method, and the crystal structure is analyzed by the direct method or the Patterson method to obtain the initial structure, and then the coordinates of all non-hydrogen atoms and organic groups are obtained by least square correction and difference Fourier method. The hydrogen atoms on the water were obtained by theoretical hydrogenation, and the hydrogen atoms on the water were determined by the difference Fourier method. And corrected by full-matrix least [84] squares, all non-hydrogen atoms were refined using anisotropic thermal parameters. Using the corrected precise atomic coordinate...

Embodiment 3

[0023] Example 3 The thermal stability of the microporous metal-organic framework material Zn(pybdc) obtained in Example 1 was characterized.

[0024] The thermal stability of the microporous metal-organic framework material Zn(pybdc) is analyzed by thermogravimetry, and the thermogravimetric curve is shown in image 3 .

[0025] Example 4 Characterization of gas adsorption properties of the microporous metal-organic framework material obtained in Example 1.

[0026] We carried out hydrogen adsorption at 77 K and CO adsorption at 273 K using samples of Zn(pybdc) 2 Adsorption studies. At 77K, the adsorption amount of hydrogen on the Zn(pybdc) sample showed a rapid increase in the low pressure region, and then increased linearly with the increase of pressure, and the adsorption amount reached 17 cm at 800 mmHg pressure. 3 / g. And at 273K, CO 2 The adsorption amount on the Zn(pybdc) sample showed a linear increase in the whole pressure range. Its adsorption isotherm diagram...

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Abstract

The invention belongs to the technical field of a microporous metal-organic framework material and particularly relates to a microporous metal-organic framework material based on isophthalic acid derivatives as well as a preparation method and an application thereof. The chemical formula of the microporous metal-organic framework material provided by the invention has a chemical formula of Zn(pybdc), wherein pybdc<2-> is deprotonated 5-(1-pyrrolidyl)-1,3-phthalic acid and n represents an infinite link of the structural unit. The metal-organic framework material provided by the invention is crystallized in a trigonal system and the space group is R-3m; the metal Zn<2+> is located in the center of a tetrahedron and is tetrachordinate. The microporous metal-organic framework material provided by the invention has a one-dimensional porous channel structure along the direction of axis c and a methylene group of a pentary pyrrole ring stretches into the porous channel; the window of the porous channel is about 4 angstroms and the porosity is 18.6%. The structure of the material provided by the invention has the porous channel, so that the material can be used for safely storing gas or solvent molecules.

Description

technical field [0001] The invention belongs to the technical field of microporous metal-organic framework materials, and in particular relates to a microporous metal-organic framework material based on isophthalic acid derivatives and its preparation method and application. Background technique [0002] In the past decade, microporous metal-organic frameworks (MOFs) have attracted much attention due to their rich topologies and applications in gas storage or separation, ion exchange, catalysis, and even chemical sensors. [0003] In the process of building these structures, organic ligands play a pivotal role. Carboxylic acid coordination polymer materials have attracted widespread attention because of their structural stability, diversity, and applications in gas adsorption, especially in hydrogen storage. The diversity of dihedral angles between the carboxyl plane and the benzene ring plane of polycarboxylate ligands gives them significant advantages in anchoring metal c...

Claims

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Application Information

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IPC IPC(8): C07F3/06B01J20/22B01J20/30B01D53/04
Inventor 凌云杨淼贾瑜陈珍霞邓名莉刘小锋杨永泰周亚明
Owner FUDAN UNIV
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