Preparation method of MOF-metal nanoparticle-COF-based composite material

A technology of metal nanoparticles and composite materials, which is applied in the field of preparation based on MOF@metal nanoparticles@COF composite materials, to achieve high dispersion, simple preparation method, stable and firm combination of electrostatic interaction

Inactive Publication Date: 2020-06-26
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are some reports on MOF@COF core-shell composite materials, but the preparation method of MOF@metal nanoparticles@COF composite materials combining MOF, metal nanoparticles and COF is still rarely reported.

Method used

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  • Preparation method of MOF-metal nanoparticle-COF-based composite material
  • Preparation method of MOF-metal nanoparticle-COF-based composite material
  • Preparation method of MOF-metal nanoparticle-COF-based composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Dissolve 1mmol of titanium tetraisopropoxide and 3mmol of 2-aminoterephthalic acid into a mixed solution containing 9ml of DMF solution and 1ml of methanol, stir evenly with a magnetic force and place in a 50ml polytetrafluoroethylene high-temperature reaction kettle In 150°C high temperature reaction for 72h, wash and centrifuge with DMF and methanol solution successively, then vacuum dry at 80°C for 12h to obtain MIL-125(Ti)-NH 2 Material;

[0029] 2) 0.4g prepared MIL-125(Ti)-NH 2 The material was dispersed in 10ml of solvent deionized water, and 0.8ml of chloroauric acid solution (Au 3+ content of 5 mg / ml), stirred at room temperature for 4 hours, added 30 mg of sodium borohydride, stirred at room temperature for 4 hours, centrifuged, washed with deionized water three times, and dried in an oven at 80°C to obtain MIL-125(Ti)-NH 2 @AuComposite;

[0030] 3) 0.2g prepared MIL-125(Ti)-NH 2 After the @Au composite material was activated at 80°C for 12 hours, it wa...

Embodiment 2

[0034]1) Mix 4mmol of ferric nitrate, 1mmol of 2-aminoterephthalic acid and 10ml of DMF solution evenly and place it in a 50ml polytetrafluoroethylene high-temperature reaction kettle, react at 150°C for 6 hours, and then wash with DMF and methanol solution in turn Centrifuge, then vacuum dry at 80°C to obtain amino-modified MIL-53(Fe)-NH 2 Material;

[0035] 2) 0.3g prepared MIL-53(Fe)-NH 2 The material was dispersed in a mixed solution of 30ml ethanol and water (the volume ratio of ethanol: water was 4:1), and 1mL potassium chloroplatinate (Pt 2+ The concentration is 3mg / ml) aqueous solution, and then the above solution is stirred under the ultraviolet light for 3 hours at low temperature by the ultraviolet light reduction method, and finally centrifuged, washed with deionized water for 3 times, and dried at 80°C to obtain MIL-53(Fe)-NH 2 @PtComposite;

[0036] 3) 0.1g of prepared MIL-53(Fe)-NH 2 After @Pt material was activated at 100°C for 10 hours, it was dispersed in...

Embodiment 3

[0040] 1) Mix 0.675g of ferric chloride, 0.225g of 2-aminoterephthalic acid and 15ml of DMF solution evenly and place them in a 100ml polytetrafluoroethylene high-temperature reactor. Wash and centrifuge with methanol solution, then vacuum dry at 80°C to obtain amino-modified MIL-101(Fe)-NH 2 Material;

[0041] 2) 0.2g prepared MIL-101(Fe)-NH 2 The material was dispersed in 20ml of n-hexane, and 0.6ml of chloroauric acid solution (Au 3+ Concentration is 5mg / ml), after stirring at room temperature for 2h, let it stand, take out n-hexane, dry at room temperature and then in a tube furnace in 5%H 2 / Ar atmosphere and reduction treatment at 200°C for 2h, after cooling to obtain MIL-101(Fe)-NH 2 @AuComposite;

[0042] 3) 0.2g of prepared MIL-101(Fe)-NH 2 The @Au material was activated at 120°C for 12 hours and dispersed in 15ml of a mixed solution of 1,4-dioxane and mesitylene with a volume ratio of 2:1, and then added 0.06mmol of 2,2'-bipyridine- 5,5'-diformaldehyde was ultr...

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Abstract

The invention discloses a preparation method of the MOF-metal nanoparticle-COF composite material. The method comprises the following steps: dispersing MOF into a solution containing a metal ion precursor, adding a sodium borohydride solution or performing illumination reduction, or performing hydrogen reduction after centrifugation to obtain the MOF-metal nanoparticle composite material. Activating at a high temperature of 120-150 DEG C and then dispersing in 1, 3-butanediol; the method comprises the following steps: adding 1, 4-dioxane and mesitylene into a mixed solvent of 1, 4-dioxane andmesitylene; then adding a small amount of aldehyde group organic ligand and ultrasonically and uniformly mixing; subsequent addition of acetic acid, adding a corresponding amount of amino organic ligand, and continuously stirring for a period of time to obtain an MOF-metal nanoparticle-COF seed crystal compound; and adding an aldehyde group organic ligand and an amino group organic ligand, uniformly stirring and mixing, adding a corresponding amount of acetic acid, and continuously stirring, heating and preserving heat to obtain the MOF-metal nanoparticle-COF compound. Covalent binding of thetwo materials is achieved through a Schiff base reaction between aldehyde groups on the surfaces of the seed crystals and amino groups on the surfaces of the MOF materials, the binding force is stableand firm, the preparation method is simple, the method can be used for mass production, and traditional high-temperature and high-pressure reaction conditions are not needed in the compounding process.

Description

technical field [0001] The invention belongs to the technical field of preparation of advanced nanocomposite materials, in particular to a preparation method based on MOF@metal nanoparticle@COF composite materials. Background technique [0002] Metal-Organic Framework (MOF for short) is a porous crystalline material formed by metal ions and organic ligands or clusters through coordination bonds. Covalent Organic Framework (COF for short) is a class of porous crystalline polymers constructed from organic units through covalent bonds. Due to the advantages of high specific surface area, adjustable pore structure, and good topology, the two types of materials have great application prospects in catalysis, gas adsorption, and separation. In recent years, both MOF and COF hybrid materials have been reported, such as hybridizing MOF and metal nanoparticles, polymers or other MOFs, or hybridizing COF and metal nanoparticles (such as Au). Professor Zhang Hua's research group repor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C08K3/08C08L87/00
CPCC08G83/008C08K3/08C08K2003/0831C08L87/00C08L2205/025
Inventor 黄秀兵席作帅王戈路桂隆
Owner UNIV OF SCI & TECH BEIJING
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