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A kind of preparation method of metal organic framework/noble metal simple substance nanocomposite material

A technology of nanocomposite materials and metal organic frameworks, which is applied in the field of preparation of metal organic frameworks/noble metal nanocomposites, and can solve the problems of large particle size, cumbersome preparation steps, uneven distribution of noble metal nanoparticle or clusters, etc. , to achieve the effect of uniform dispersion, uniform size, stable and firm combination

Active Publication Date: 2021-09-21
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, there have been some reports on MOFs / noble metal nanocomposites, such as loading noble metal nanoparticles or clusters on the surface of MOFs by sol-gel method, or immobilizing noble metal ions in the pores of MOFs by impregnation method or dual solvent method. Then the precious metal simple substance nanoparticles or clusters are obtained by sodium borohydride or hydrogen reduction. The preparation steps of MOFs / noble metal simple substance nanocomposites by the two-step method are cumbersome, and the noble metal simple substance nanoparticles or clusters have uneven distribution and small particle size. Large and insufficient
There are few reports on the preparation of MOFs / noble metal nanocomposites with uniform distribution of noble metal by in situ reduction method

Method used

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  • A kind of preparation method of metal organic framework/noble metal simple substance nanocomposite material
  • A kind of preparation method of metal organic framework/noble metal simple substance nanocomposite material
  • A kind of preparation method of metal organic framework/noble metal simple substance nanocomposite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Dissolve 1.7mmol of zirconium tetrachloride and 1.7mmol of 2-aminoterephthalic acid in a mixed solution containing 2.85ml of glacial acetic acid and 95ml of DMF solution, mix them uniformly with ultrasound, and place them at 120°C for 24 hours of high temperature reaction Wash and centrifuge with DMF and methanol solution successively, and then vacuum-dry at 80°C to obtain amino-modified UiO-66(Zr)-NH 2 Material;

[0024] 2) 1g of prepared UiO-66(Zr)-NH 2 The material was dispersed in 50ml of a mixed solvent of formaldehyde, ethanol and water with a volume ratio of 5:20:25, then stirred and mixed evenly at 40°C for 120min, and then the solid was separated and vacuum-dried at 80°C for 12h to obtain the modified UiO-66(Zr )-NH 2 Material;

[0025] 3) Take 0.2g modified UiO-66(Zr)-NH 2 The material was dispersed in 20ml of n-hexane, and 0.2ml of HAuCl was added 4 4H 2 O precious metal solution (wherein Au 3+ The mass is 4 mg, and the solvent is a mixed solution o...

Embodiment 2

[0027] 1) Dissolve 1.7mmol of zirconium tetrachloride and 1.7mmol of 2-aminoterephthalic acid in a mixed solution containing 2.85ml of glacial acetic acid and 95ml of DMF solution, mix them uniformly with ultrasound, and place them at 120°C for 24 hours of high temperature reaction Wash and centrifuge with DMF and methanol solution successively, and then vacuum-dry at 80°C to obtain amino-modified UiO-66(Zr)-NH 2 Material;

[0028] 2) 0.5g prepared UiO-66(Zr)-NH 2 The material was dispersed in 30ml of a mixed solvent of formaldehyde, ethanol and water with a volume ratio of 10:20:20, then stirred and mixed evenly at 50°C for 120min, and then the solid was separated and vacuum-dried at 90°C for 20h to obtain the modified UiO-66(Zr )-NH 2 Material;

[0029] 3) Take 0.3g modified UiO-66(Zr)-NH 2 The material was dispersed in 30ml of n-hexane, and 0.3ml of H 2 PtCI 6 ·6H 2 O precious metal solution (wherein Pt 4+ The mass is 4 mg, and the solvent is a mixed solution of ace...

Embodiment 3

[0031] 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 After reacting at high temperature at 150°C for 72 hours, washing and centrifuging with DMF and methanol solution successively, and then vacuum drying at 80°C, the amino-modified MIL-125(Ti)-NH 2 Material;

[0032] 2) 1g of prepared MIL-125(Ti)-NH 2 The material was dispersed in 40ml of a mixed solvent of formaldehyde, ethanol and water with a volume ratio of 5:20:20, then stirred and mixed evenly at 40°C for 120min, and then the solid was separated and vacuum-dried at 80°C for 12h to obtain the modified MIL-125(Ti )-NH 2 Material;

[0033] 3) Take 0.4g of modified MIL-125(Ti)-NH 2 The material was dispersed in 40ml of n-hexane, and 0.4ml of HAuCl was added 4 4H 2 O precious metal solution (wherein...

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Abstract

A preparation method of metal-organic framework / precious metal elemental nanocomposite material. First prepare MOFs modified with amino groups, then disperse the MOFs modified with amino groups in a mixed solution of formaldehyde, ethanol and water. Formaldehyde will react with the amino groups on the surface of the pores of MOFs. of MOFs. Take an appropriate amount of MOFs with reducing functional groups and uniformly disperse them in a hydrophobic solvent. After adding a noble metal ion aqueous solution, the reducing functional groups can in situ reduce the noble metal ions to noble metal nano-particles or clusters. After stirring, separation and vacuum drying, MOFs are obtained. / Noble metal elemental nanocomposites. The in-situ reduction method can make the loading distribution of noble metal nano-particles or clusters in the pores of MOFs more uniform and the size more uniform. By changing the concentration of noble metal ions, the loading of noble metal elemental nanoparticles or clusters can be regulated. The method of the invention is simple, can be used for mass production, and the compounding process does not need the traditional reaction conditions of high temperature and high pressure.

Description

technical field [0001] The invention belongs to the technical field of preparation of advanced nanocomposite materials, and in particular relates to a method for preparing a metal organic framework / noble metal simple substance nanocomposite material by using an in-situ reduction method. Background technique [0002] Metal-organic frameworks (MOFs for short) are porous crystalline materials formed by metal ions and organic ligands or clusters through coordination bonds. Due to the characteristics of high specific surface area, adjustable pore structure, good topology, functional modification and multifunctionality of MOFs materials, as well as the advantages of high catalytic activity and many surface active sites of noble metal single substance nanoparticles or clusters, the two The combined MOFs / noble metal single substance nanocomposites have aroused widespread interest of researchers, and have great application prospects in catalysis, gas adsorption and separation. In re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
CPCC08K3/08C08K2003/0806C08K2003/0831C08K2201/011C08L87/00
Inventor 黄秀兵席作帅路桂隆王戈
Owner UNIV OF SCI & TECH BEIJING