Synthetic method of metal organic framework

A technology of metal-organic framework and synthesis method, which is applied in the field of preparation of metal-organic framework materials, can solve the problems of small specific surface area, low porosity, and poor stability of MOFs materials, and achieve improved mass transfer efficiency, simplified synthesis steps, and easy interaction. The effect of contact

Pending Publication Date: 2021-12-28
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The MOFs materials obtained in this application still have problems such as small specific surface area, low porosity and poor stability.

Method used

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  • Synthetic method of metal organic framework
  • Synthetic method of metal organic framework
  • Synthetic method of metal organic framework

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 0.23mmol of ZrCl 4 and 2.3mmol terephthalic acid were added to 2.3mmol N,N-dimethylformamide, stirred at room temperature until the solids were completely dissolved, then added 2.3mmol acetic acid, stirred evenly, added 0.23mmol water and 0.023mmol p-xylene; The above mixed solution was moved to a reaction kettle lined with polytetrafluoroethylene, and the reaction kettle was sealed, and the reaction temperature was controlled to be 100°C, and the reaction time was 10h; after the reaction was completed, the target product 1 was obtained by centrifugation, washing and drying, and its scanning Electron microscope image and nitrogen adsorption-desorption isotherm as shown in figure 1 , Figure 8 shown.

Embodiment 2

[0049] Add 0.46mmol of ZrOCl2 8H2O and 0.23mmol of terephthalic acid to 920mmol of N,N-dimethylacetamide, stir at room temperature until all the solids are dissolved, add 92mmol of formic acid, add 23mmol of water and 0.23mmol of tris Toluene, stirred evenly at room temperature; move the above mixed solution to a reaction kettle lined with polytetrafluoroethylene, seal the reaction kettle, control the reaction temperature to 120°C, and the reaction time to 12h; after the reaction, centrifuge, wash and Dried to obtain the target product 2, its scanning electron microscope picture and nitrogen adsorption-desorption isotherm are as follows figure 2 , Figure 9 shown.

Embodiment 3

[0051]Add 0.23mmol of zirconyl nitrate and 0.46mmol of terephthalic acid to 115mmol of acetonitrile, stir at room temperature until the solids are completely dissolved, add 11.5mmol of benzoic acid and stir evenly, add 11.5mmol of water and 2.3mmol of durene; then Move the above mixed solution to a reaction kettle lined with polytetrafluoroethylene, seal the reaction kettle, control the reaction temperature to 150°C, and the reaction time to 24h; after the reaction, centrifuge, wash and dry to obtain the target product 3, which Scanning electron microscope image and nitrogen adsorption-desorption isotherm as shown in image 3 , Figure 10 shown.

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Abstract

The invention relates to a metal organic framework material, in particular to a preparation method of the metal organic framework material, which comprises the following steps: (1) adding a metal zirconium salt and a dicarboxylic acid organic ligand into an aprotic polar solvent, and stirring the solution at room temperature until the solid is completely dissolved to obtain a solution I; (2) adding monocarboxyl organic acid into the solution I, and uniformly stirring the solution I to obtain a solution II; (3) adding water into the solution II to obtain a solution III; (4) adding a regulator into the solution III to obtain a solution IV, the regulator being one of xylene, trimethylbenzene or tetramethylbenzene; (5) controlling the temperature range of the solution IV to be 25-300 DEG C, and carrying out hydrothermal reaction; (6) after the reaction is finished, carrying out centrifugal separation, washing and drying to obtain a target product. Herein, the small-grain zirconium-based MOFs material can be successfully obtained by controlling the nucleation and crystallization rate of the metal ions and the organic ligands, so that the mass transfer efficiency of the microporous material is improved.

Description

technical field [0001] The invention relates to metal organic framework materials, in particular to a preparation method of metal organic framework materials. Background technique [0002] Metal-organic frameworks (MOFs) refer to polymer materials with one-dimensional, two-dimensional or three-dimensional materials self-assembled by metal centers (metalsites) and organic ligands (organic ligands) through coordination bonds. Compared with traditional porous materials such as molecular sieves and activated carbons, they have ultra-high specific surfaces (7000m 2 / g) and porosity (up to 0.9cm 3 / g), at the same time, MOFs materials are ever-changing through different ligand types and coordination forms, and their pore structure and surface properties can also be regulated and designed, so MOFs are widely used in gas storage, adsorption separation, catalytic reactions, biomedicine , smart materials and other fields. [0003] The pore size distribution of most of the reported ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 刘宗健刘建新杨爱武尹淑华任珉汪洋王保正周启慧朱庆奋
Owner CHINA PETROLEUM & CHEM CORP
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