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Porous fluid as well as preparation method and application thereof

A fluid, ionic liquid technology, applied in the field of porous fluid and its preparation, can solve the problems of poor universality, difficult characterization and modification of pores, unstable colloidal dispersion system, etc., to achieve high colloidal stability, enhanced solvation, mechanical Properties that can be tunable

Pending Publication Date: 2021-11-26
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If a small molecule solvent is used as a medium, it will lead to a decrease in the porosity of the MOF material
[0004] The currently reported porous fluids are as follows, 1) porous fluids based on crown ether imine cages, 15-crown-5 as a solvent, macromolecular solvents cannot enter the crown ether imine cages, effectively retaining porosity, but due to the organic porous The structure is soft and amorphous, and the pores are difficult to characterize and modify; 2) Porous fluids based on porous silicon spheres and porous carbon spheres have a single pore structure and cannot be selectively adsorbed; 3) Porous fluids obtained by directly dispersing MOF in ordinary ionic liquids , the ionic liquid is small, and it is easy to enter the pores of some MOFs with larger pore diameters, resulting in a decrease in porosity, and there is no interaction between the ionic liquid and the MOF surface, resulting in an unstable colloidal dispersion system, easy aggregation, and poor universality

Method used

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  • Porous fluid as well as preparation method and application thereof
  • Porous fluid as well as preparation method and application thereof
  • Porous fluid as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] The preparation method of the porous fluid of the present embodiment is as follows:

[0057] 1) Synthesis of cationic part (substance A): 2-methylimidazole (116.43mg, 0.0011mol) and N-(3-azide)-N,N-dioctyl-N-methylammonium bromide (339.58mg, 0.001mol) was dissolved in a round bottom flask of 5mlDMF, under the protection of inert gas (nitrogen or argon), add CuBr (43.635mg, 0.0003mol) and PMDETA (109.98mg, 0.0006mol), stirred at room temperature Overnight, the crude product was obtained; the crude product was dissolved in ethyl acetate after removing DMF, and washed three times (purification) with NaOH aqueous solution of EDTA; the ethyl acetate layer was washed with anhydrous NaOH 2 SO 4 After drying, the excess solution was removed by rotary evaporation to obtain the cationic fraction (substance A).

[0058] 2) Synthesis of ionic liquid: put cationic part and PEGS of equal amount in a flask, add 5 times the volume (that is, 5 times the volume of cationic part and PEG...

Embodiment 2

[0068] The preparation method of the porous fluid of the present embodiment is as follows:

[0069] 1) Synthesis of cationic part (substance A): 2-methylimidazole (116.43mg, 0.0011mol) and N-(3-azide)-N,N-dioctyl-N-methylammonium bromide (339.58mg, 0.001mol) was dissolved in a 5ml DMF round bottom flask, under the protection of an inert gas, CuBr (43.635mg, 0.0003mol) and PMDETA (109.98mg, 0.0006mol) were added, stirred overnight at room temperature to obtain a crude product; The crude product was dissolved in ethyl acetate after removing DMF, washed three times with EDTA NaOH aqueous solution; the ethyl acetate layer was washed with anhydrous NaOH 2 SO 4 After drying, the excess solution was removed by rotary evaporation to obtain the cationic fraction (substance A).

[0070] 2) Synthesis of ionic liquids: put cationic moieties and PEGS in equal amounts in a flask, add 5 times the volume of a 1:1 mixed solution of water and ethanol, react overnight at 70°C, and dialyze the ...

Embodiment 3

[0074] The preparation method of the porous fluid of the present embodiment is as follows:

[0075] 1) Synthesis of cationic part (substance A): 2-methylimidazole (116.43mg, 0.0011mol) and N-(3-azide)-N,N-dioctyl-N-methylammonium bromide (339.58mg, 0.001mol) was dissolved in a 5ml DMF round bottom flask, under the protection of an inert gas, CuBr (43.635mg, 0.0003mol) and PMDETA (109.98mg, 0.0006mol) were added, stirred overnight at room temperature to obtain a crude product; The crude product was dissolved in ethyl acetate after removing DMF, washed three times with EDTA NaOH aqueous solution; the ethyl acetate layer was washed with anhydrous NaOH 2 SO 4 After drying, the excess solution was removed by rotary evaporation to obtain the cationic fraction (substance A).

[0076] 2) Synthesis of ionic liquids: put cationic moieties and PEGS in equal amounts in a flask, add 5 times the volume of a 1:1 mixed solution of water and ethanol, react overnight at 70°C, and dialyze the ...

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Abstract

The invention provides a porous fluid as well as a preparation method and application thereof. The preparation method comprises the steps that: 2-methylimidazole and N-(3-azide)-N, N-dioctyl-N-methyl ammonium bromide are dissolved in an organic solvent, under the protection of inert gas, COR and PMDETA are added, stirring is conducted for 8-14 h at the room temperature, and a crude product A is obtained; the crude product A is purified and dried to obtain a substance A; the substance A, PEGS and an ethanol solution are mixed, a reaction is performed at 60-80 DEG C for 8-14 hours, and dialyzing is performed for 60-80 hours to obtain an ionic liquid for later use; and nano-scale MOFs are dispersed in an ethanol solution, then the ionic liquid obtained in S2 is added, uniform mixing is performed, shaking is performed for 8-14 hours, the solvent is removed, and drying is performed to obtain the porous fluid. The porous fluid provided by the invention has both flowability and porosity, and has a wide application prospect.

Description

technical field [0001] The invention relates to a porous fluid and its preparation method and application. Background technique [0002] Metal-organic frameworks (MOFs): Metal ions or metal clusters (ie: SBU, secondary building units) and organic ligands are linked together through metal-organic ligand bonds. The properties of materials are determined by their structures. The basic building blocks of MOFs are central metal ions and organic ligands. Therefore, the design and synthesis of open-frame coordination polymers can be achieved at the molecular level by selecting appropriate metal ions and steric ligands with extended effects. Self-assembly is carried out on the surface, and the structure of the complex is regulated by appropriate means to obtain MOFs materials with novel structures and special properties. Due to their high porosity, good chemical stability, reproducibility, simple synthesis process and equipment, and their exquisite framework structure, MOFs have at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28C07D403/06C02F1/28C02F101/30
CPCB01J20/226B01J20/28054C07D403/06C02F1/285C02F2101/308
Inventor 邢航谢敏肖跃谢莎莎
Owner HUNAN UNIV
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