Precious metal ion adsorption material based on magnetic metal organic framework and preparation method

A precious metal ion, organic framework technology, applied in alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., can solve the problems of increasing the use cost of MOFs, and achieve enhanced stability, simple recovery process, High adsorption efficiency

Inactive Publication Date: 2021-10-08
UNIV OF SCI & TECH BEIJING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since most MOFs are submicron in size, high-speed centrifugation is required to achieve solid-liquid separation, which increases the cost of using MOFs.

Method used

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  • Precious metal ion adsorption material based on magnetic metal organic framework and preparation method
  • Precious metal ion adsorption material based on magnetic metal organic framework and preparation method
  • Precious metal ion adsorption material based on magnetic metal organic framework and preparation method

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preparation example Construction

[0035] The invention provides a noble metal ion adsorption material based on a magnetic metal organic framework and a preparation method.

[0036] The central metal of the adsorption material MOFs is Zr, the organic ligand is terephthalic acid or its derivatives, and the expression is Fe 3 o 4 @SiO 2 @UiO-66 - Functional groups.

[0037] Fe in this material 3 o 4 The content is 1%~50%, and the material has magnetism, the magnetic test figure of the synthesized magnetic MOFs composite material of the present invention is as follows Figure 5 Shown; Fe 3 o 4 Coated SiO 2 , Fe 3 o 4 The particle size is 5-50nm, SiO 2 The thickness of the shell layer is 1-30 nm.

[0038] The preparation method of this adsorption material comprises steps as follows:

[0039] (1) NaHCO 3 The solution is mixed with the ferric salt solution in proportion and then reacted. After the brick-red precipitate is formed, the reducing agent solution is added dropwise to the mixture. After the bri...

Embodiment 1

[0061] 1. Magnetic Zr-based MOFs composite Fe 3 o 4 @SiO 2 The preparation steps of @UiO-66 are as follows:

[0062] (1) 0.3mol / L of FeCl 3 solution with 0.45mol / L NaHCO 3 The solution was mixed at a ratio of 1:2 and then reacted. After a brick-red precipitate was formed in the solution, 0.05mol / L vitamin C solution was added dropwise, and the mixture was transferred to a p-polyphenylene (PPL) reactor after stirring for 10 minutes. Place in a drying oven at 5°C min -1 Heating to 180°C at a rate of 12h, followed by 4°C·min -1 rate down to room temperature. Wash with ethanol and ultrapure water for 3 times and then vacuum dry for later use. The obtained product is marked as Fe 3 o 4 nanoparticles.

[0063] (2) Take 230mg Fe 3 o 4The nanoparticles were ultrasonically dispersed in 100 mL of a mixed solution of ethanol and water (ethanol: water = 1:4) for 30 min, then transferred to a three-necked round-bottomed flask and added with 1.5 mL of concentrated ammonia water. ...

Embodiment 2

[0071] 1. Amino-modified magnetic Zr-based MOFs composite Fe 3 o 4 @SiO 2 @UiO-66-NH 2 The synthesis steps are as follows:

[0072] (1) 0.3mol / L of Fe 2 (SO 4 ) 3 solution with 0.45mol / L NaHCO 3 The solution was mixed at a ratio of 1:2 and then reacted. After a brick-red precipitate was formed in the solution, 0.05mol / L uric acid solution was added dropwise. After stirring for 10 minutes, the mixture was transferred to a PPL reactor, and placed in a drying oven for 5 ℃·min -1 Heating to 180°C at a rate of 12h, followed by 4°C·min -1 The rate will come to room temperature. Wash with ethanol and ultrapure water for 3 times and then vacuum dry for later use. The obtained product is marked as Fe 3 o 4 nanoparticles.

[0073] (2) Take 230mg Fe 3 o 4 The nanoparticles were ultrasonically dispersed in 100 mL of a mixed solution of ethanol and water (ethanol: water = 1:4) for 30 min, then transferred to a three-necked round-bottomed flask and added with 1.5 mL of concent...

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Abstract

The invention provides a preciousmetal ion adsorption material based on a magnetic metal organic framework and a preparation method, and belongs to the technical field of adsorption materials, wherein the central metal of the adsorption material MOFs is Zr, the organic ligand is terephthalic acid or a derivative thereof, and the expression is Fe3O4@SiO2@UiO-66-functional group. The preparation method comprises the following steps: mixing a NaHCO3 solution with a ferric iron salt solution, reacting, and adding a reducing agent solution to obtain Fe3O4 nanoparticles; adding the Fe3O4 nanoparticles into a mixed solution of water and ethanol, uniformly dispersing, adjusting the solution to alkalescence, stirring, and adding tetraethyl orthosilicate to obtain magnetic nanoparticles Fe3O4@SiO2; and adding the magnetic nanoparticles Fe3O4@SiO2 into N, N-dimethylformamide (DMF), and adding ZrCl4 and BDC or a BDC derivative to obtain a Fe3O4@SiO2@UiO-66-functional group. According to the invention, the adsorption material is high in precious metal ion adsorption efficiency, easy to regenerate and capable of being recycled, can achieve solid-liquid separation and material recycling through an external magnetic field, reduces the precious metal recovery cost, and has huge commercial application value in the field of precious metal enrichment and recovery.

Description

technical field [0001] The invention relates to the technical field of adsorption materials, in particular to a noble metal ion adsorption material based on a magnetic metal organic framework and a preparation method thereof. Background technique [0002] Noble metals usually refer to gold, silver and platinum group metals (such as platinum, palladium, rhodium, etc.), which have good physical and chemical properties, such as good thermal and electrical conductivity, high temperature resistance, chemical corrosion resistance, strong coordination ability and high catalytic activity etc. It has been widely used in the fields of jewelry, aerospace, electronics, information communication, automation technology and life sciences. With the advancement of science and technology and the popularization of modern lifestyles, the consumption of precious metals is increasing day by day, but the existing production of precious metals is completely unable to meet the growing needs. At the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C22B11/00C22B3/24C22B7/00
CPCB01J20/06B01J20/103B01J20/226B01J20/28009B01J20/28064C22B11/046C22B3/24C22B7/006Y02P10/20
Inventor 常自勇曾亮祁晓月宫晓莎王化军付广钦
Owner UNIV OF SCI & TECH BEIJING
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