Preparation method of nano-particle@minisize metal organic frame material

A technology of metal-organic frameworks and nanoparticles, which is applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., to achieve good versatility, strong applicability, and the effect of preventing agglomeration

Inactive Publication Date: 2017-11-17
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the composite materials of MOFs and nanoparticles synthesized by traditional methods are all in the range of hundreds to several microns, which limits its application in many aspects. Therefore, it is very important to develop a composite material of small-sized MOFs and nanoparticles.

Method used

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  • Preparation method of nano-particle@minisize metal organic frame material
  • Preparation method of nano-particle@minisize metal organic frame material
  • Preparation method of nano-particle@minisize metal organic frame material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Synthesis of Pt nanoparticles

[0029] Aqueous solution of chloroplatinic acid (6mM, 20ml) and polyvinylpyrrolidone (0.018mmol) were mixed, then methanol was added and the volume was adjusted to 200 ml, after the polyvinylpyrrolidone was stirred and dissolved, the mixed solution was transferred to a 250 ml round-bottomed flask, and placed Reflux and react in an oil bath at 70°C for 3 hours, spin-evaporate the obtained product, precipitate and centrifuge with acetone, and finally wash with chloroform and n-hexane for 10 times, disperse in methanol for later use, and the particle size is about 3nm.

[0030] 2) Synthesis of Pt@nano-UiO-66 using a small molecule acetic acid regulator

[0031] 0.005mmol of Pt nanoparticles modified by polyvinylpyrrolidone synthesized in step 1), 0.14mmol of zirconium tetrachloride, 0.14mmol of terephthalic acid and 0.4ml of acetic acid were mixed, and N, N dimethylformamide was added to constant volume. 10ml, ultrasonic 1min fully dissol...

Embodiment 2

[0034] 1) The synthesis of Pt nanoparticles modified by polyvinylpyrrolidone is the same as in Example 1.

[0035] 2) Synthesis of Pt@nano-UiO-66-NH using a small molecule acetic acid regulator 2

[0036] Mix 0.005 mmol of Pt nanoparticles modified with polyvinylpyrrolidone, 0.14 mmol of zirconium tetrachloride, 0.14 mmol of aminoterephthalic acid and 0.5 ml of acetic acid, and add N,N dimethylformamide to make the total volume 10 ml , sonicated for 1 min and fully dissolved, transferred to a 20 ml isotope bottle and placed in a 120 °C oven for solvothermal reaction for 36 h, the obtained product was centrifuged, washed three times with N, N dimethylformamide and ethanol, and dried , that is, Pt@nano-UiO-66-NH 2 , the resulting size is about 25 nm.

[0037] The characterization diagram of the product is shown in 5-6, Figure 5 It is the TEM image of Pt@nano-UiO-66-NH2, Figure 6 It is the powder diffraction pattern of Pt@nano-UiO-66-NH2.

Embodiment 3

[0039] 1) The synthesis of Pt nanoparticles modified by polyvinylpyrrolidone is the same as in Example 1.

[0040] 2) Synthesis of Pt@nano-801 using acetic acid regulator

[0041] Mix 0.005 mmol of Pt nanoparticles modified with polyvinylpyrrolidone, 0.14 mmol of zirconium tetrachloride, 0.14 mmol of fumaric acid and 0.5 ml of acetic acid, and add N, N dimethylformamide to make the total volume 10 ml , sonicated for 1min and fully dissolved, transferred to a 20ml isotope bottle and placed in a 120°C oven for solvothermal reaction for 24h, the obtained product was centrifuged, washed three times with N,N dimethylformamide and ethanol, and dried , that is, Pt@nano-801, the resulting size is about 30nm.

[0042] The characterization diagram of the product is shown in 7-8, Figure 7 It is the transmission electron microscope picture of Pt@nano-801, Figure 8 It is the powder diffraction pattern of Pt@nano-801.

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Abstract

The invention relates to a preparation method of a nano-particle@minisize metal organic frame material. The preparation method comprises the following steps of 1, preparing nano-particles modified by polyvinylpyrrolidone; 2, adding the obtained nano-particles into an MOF growth reaction solution, the addition amount of an adjusting agent is controlled, and the nano-particle@minisize metal organic frame material is obtained. The method is simple and easy to implement, mild in condition and high in applicability, and the prepared nano-particle@minisize metal organic frame material can effectively prevent nano-particle aggregation, meanwhile has the advantages of being good in size selectivity, and short in diffusion range between the surface of the metal organic framework and the active center of nano-particles, and has the wide application prospect in the fields of catalysis, biological imaging and the like.

Description

technical field [0001] The invention relates to the technical field of composite nanomaterials, and in particular, discloses a method for preparing nanoparticle@small-sized metal-organic framework materials. Background technique [0002] Metal–Organic Frameworks (MOFs) are a class of porous materials assembled by metal ions / metal atom clusters and organic ligands. Due to its structural characteristics such as high specific surface area, adjustable pore size and window size, and easy modification of ligands, it has a wide range of applications in gas adsorption and separation, catalysis, and drug sustained release. In recent years, composites prepared by coating nanoparticles with metal-organic frameworks (MOFs) have attracted extensive attention from researchers as heterogeneous catalysts. Using MOF as a carrier to coat highly active nanoparticles can achieve properties that cannot be achieved by a single component. However, the composite materials of MOFs and nanoparticle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B82Y30/00B82Y40/00
CPCB01J31/1691B01J31/1815B01J31/2213B01J35/006B01J35/0073B01J35/023B01J2531/26B01J2531/49B82Y30/00B82Y40/00
Inventor 刘军枫王兵庆
Owner BEIJING UNIV OF CHEM TECH
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