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Preparation method of metal organic framework based on ionic liquid microemulsion

A metal-organic framework, ionic liquid technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc. Large-scale preparation of MOFs and other problems, to achieve the effect of increasing solubility, reducing synthesis cost and improving yield

Active Publication Date: 2021-04-02
SOUTHEAST UNIV CHENGXIAN COLLEGE
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  • Description
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  • Application Information

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Problems solved by technology

[0007] (1) During the synthesis process, MOFs crystals are grown in aqueous droplets, which requires the use of other organic reagents for dissolution, which increases the use of organic reagents and increases the pollution to the environment
[0008] (2) It is necessary to control the morphology and size of MOFs crystals through the control of complex reaction parameters, which is not conducive to the large-scale preparation of MOFs required, which greatly limits the application range of MOFs as multifunctional materials.
[0009] (3) Failure to simultaneously control the morphology and size of MOFs during the synthesis process
[0010] (4) Failure to control the morphology and size of MOFs with different metal centers

Method used

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  • Preparation method of metal organic framework based on ionic liquid microemulsion
  • Preparation method of metal organic framework based on ionic liquid microemulsion
  • Preparation method of metal organic framework based on ionic liquid microemulsion

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[0035] An embodiment of the present invention provides a method for preparing a metal-organic framework based on an ionic liquid microemulsion, comprising the following steps:

[0036] Step 1) using water, oil phase, ionic liquid and octylphenyl polyoxyethylene ether to prepare microemulsion;

[0037] Step 2) adding the organic ligand into the microemulsion, mixing and stirring to obtain the mixed solution A;

[0038] Step 3) adding the transition metal salt into the microemulsion, mixing and stirring to obtain the mixed solution B;

[0039] Step 4) mixing and stirring the mixed solution A and the mixed solution B, reacting at a preset temperature for a preset time, centrifuging to obtain a solid reactant, and washing with a mixed solution of dichloromethane and ethanol to obtain a metal organic framework.

[0040] As a preferred example, the ionic liquid is 1-alkyl-3-methylimidazolium tetrafluoroborate, wherein the number of carbons in the alkyl group is 1-16. Hydrophilic i...

Embodiment 1

[0059] 0.57g H 4 DOBDC and 1.01g Co(NO 3 ) 2 ·6H 2 O was added to the H 2 O, n-hexane, BmimBF 4 and TX-100 (molar ratio = 1:1:2:3) in the microemulsion constituted by stirring for 30min, until completely dissolved, to obtain microemulsion A and microemulsion B, mix microemulsion A and microemulsion B, room temperature The reaction was stirred for 24 hours to obtain a dark green reaction liquid, and 3 mLH 2 O demulsification, centrifuged, washed 3 times with a mixed solution of dichloromethane: ethanol = 1:1 (volume ratio), and dried in vacuum at 65°C to obtain pink Co-MOF-74 powder crystals with a yield of 25%. .

Embodiment 2

[0061] 0.57g H 4 DOBDC and 1.01g Co(NO 3 ) 2 ·6H 2 O was added to the H 2 O, n-hexane, BmimBF 4 and TX-100 (molar ratio = 1:1:3:4) in the microemulsion constituted by stirring for 30min until completely dissolved, to obtain microemulsion A and microemulsion B, mix microemulsion A and microemulsion B, at room temperature After stirring and reacting for 24 h, a dark green reaction solution was obtained, and 3 mL H 2 O demulsification, centrifuged, washed 3 times with a mixed solution of dichloromethane: ethanol = 1:1 (volume ratio), and dried in vacuum at 65°C to obtain pink Co-MOF-74 powder crystals with a yield of 22%. .

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Abstract

The invention discloses a preparation method of a metal organic framework based on an ionic liquid microemulsion. The preparation method comprises the following steps: step 1) preparing a microemulsion from water, an oil phase, an ionic liquid and octyl phenyl polyoxyethylene ether; 2) adding an organic ligand into the microemulsion, and mixing and stirring to obtain a mixed solution A; 3) addinga transition metal salt into the microemulsion, and mixing and stirring to obtain a mixed solution B; and 4) mixing and stirring the mixed solution A and the mixed solution B, reacting for a preset time at a preset temperature, carrying out centrifugal separation to obtain a solid reactant, and washing the solid reactant with a mixed solution of dichloromethane and ethanol to obtain the metal organic framework. According to the preparation method, the metal organic framework crystals with different morphologies, different sizes and different metal centers can be controlled and synthesized by modulating the alkyl chain length, the oil phase type and the component proportion of the ionic liquid in the microemulsion.

Description

technical field [0001] The invention relates to the technical field of synthesis of metal organic framework materials, in particular to a method for preparing metal organic frameworks based on ionic liquid microemulsions. Background technique [0002] Metal-organic frameworks (MOFs) are a class of unique inorganic-organic hybrid materials formed by metal centers and organic bridging ligands, which have attracted more and more attention, especially in the field of catalysis. Research extensively. The morphology, size and crystal plane of MOFs materials have an important impact on their properties and applications. Therefore, the controlled synthesis of MOFs crystals with specific morphology, size and specific exposed crystal planes has become a research hotspot in recent years. At present, the morphology and size of MOFs are mainly controlled by controlling the reaction temperature, time, adding regulators or microwave conditions. However, these synthetic methods are still...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01J31/22
CPCC08G83/008B01J31/1691B01J2531/845B01J2531/26B01J2531/0213B01J35/23
Inventor 黄诚
Owner SOUTHEAST UNIV CHENGXIAN COLLEGE
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