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A kind of preparation method of porous metal organic framework material hkust-1

A HKUST-1, metal-organic framework technology, applied in the field of preparation of porous metal-organic framework material HKUST-1, can solve problems such as inability to efficiently remove residues, product quality and stability cannot be guaranteed, and affect product quality. The cost is green and pollution-free, prevents by-products, and is easy to operate

Active Publication Date: 2021-01-15
NINGBO NOTTINGHAM NEW MATERIALS INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the initial HKUST-1 is obtained, it needs to be activated. The existing activation technology is to soak the initial HKUST-1 in ethanol or methanol three to four times, and then add an active agent to activate it by vacuum drying. However, this method cannot efficiently remove the residue , there will be some residual unreacted reactants remaining in the finished product, affecting product quality
The specific surface area of ​​the HKUST-1 material prepared by the existing hydrothermal method is 700-1500m 2 / g, its product quality and stability cannot be guaranteed

Method used

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  • A kind of preparation method of porous metal organic framework material hkust-1
  • A kind of preparation method of porous metal organic framework material hkust-1
  • A kind of preparation method of porous metal organic framework material hkust-1

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Embodiment 1

[0039] Such as figure 1 As shown, a preparation method of porous metal-organic framework material HKUST-1 includes the following steps: S1: Make a mixed solution of copper source and benzenetricarboxylic acid by hydrothermal method, and dry the mixed solution to obtain the initial HKUST-1 solid ; S2: The initial HKUST-1 solid was ground into powder, dissolved in methanol for activation, and the activated precipitate was dried to obtain the HKUST-1 material.

[0040] The step S1 includes the following specific steps:

[0041] S100: Weigh Cu(NO 3 ) 2 ·3H 2 O was dissolved in deionized water to obtain a copper source solution, and trimesic acid was weighed and dissolved in ethanol to obtain a trimesic acid solution.

[0042] S110: heating the copper source solution and the trimesic acid solution to 30-80° C. and mixing, respectively, to obtain a first mixed solution.

[0043] S120: heating the first mixed solution at 30-80° C. for 3-5 hours, and stirring during the heating p...

Embodiment 2

[0054] 6.5g of Cu(NO 3 ) 2 ·3H 2 O was dissolved in 200 mL of deionized water to obtain a copper source solution, and 3.5 g of trimesic acid was dissolved in 200 mL of ethanol to obtain a trimesic acid solution. The copper source solution and the trimesic acid solution were respectively heated to 40° C., and then mixed into a round bottom flask to obtain a first mixed solution. Place the round-bottomed flask in a heating mantle and heat at 40°C for 3h, and stir with a rotor at a rotational speed of 200r / min. Then pour the liquid in the round-bottomed flask into a beaker, and then put it in a drying oven to dry at 80°C for 8 hours to obtain the initial HKUST-1 solid.

[0055]The obtained initial HKUST-1 solid was ground into powder, and immersed in 400 mL of methanol to obtain the second mixed liquid. The second mixed solution was heated to boiling, and heated under reflux for 2 hours. During the reflux heating process, the rotor was used to stir at a rotational speed of 35...

Embodiment 3

[0057] 7.5g of Cu(NO 3 ) 2 ·3H 2 O was dissolved in 300 mL of deionized water to obtain a copper source solution, and 4.5 g of trimesic acid was dissolved in 300 mL of ethanol to obtain a trimesic acid solution. The copper source solution and the trimesic acid solution were heated to 60°C respectively, and then mixed into a round bottom flask to obtain the first mixed solution. Place the round-bottomed flask in a heating mantle and heat at 60°C for 5h, and stir with a rotor at a rotational speed of 260r / min. Then pour the liquid in the round-bottomed flask into a beaker, and then put it in a drying oven at 150°C for 12 hours to obtain the initial HKUST-1 solid.

[0058] The obtained initial HKUST-1 solid was ground into powder, and immersed in 600 mL of methanol to obtain the second mixed liquid. The second mixed solution was heated to boiling, and heated under reflux for 5 hours. During the reflux heating process, the rotor was used to stir at a rotational speed of 500 rp...

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Abstract

The invention discloses a preparation method of a porous-grade MOF (metal-organic framework) material HKUST-1. The preparation method comprises the following steps: S1, preparing a mixed solution froma copper source and benzene tricarbonic acid with a hydrothermal method, and drying the mixed solution to obtain an initial HKUST-1 solid; S2, grinding the initial HKUST-1 solid into powder, dissolving the powder in methanol for activation, and drying activated precipitate to obtain the HKUST-1 material. According to the method, the reaction is performed under normal pressure and lower temperature, byproducts can be prevented from being produced, reaction conditions are safe, and operation is convenient; with the unique activation method, the specific surface area of the prepared HKUST-1 canreach 1600 m<2> / kg, and thermal stability, adsorption capacity and chemical stability of the material are improved.

Description

technical field [0001] The invention relates to the field of preparation of porous metal organic framework materials, in particular to a preparation method of porous metal organic framework material HKUST-1. Background technique [0002] Metal-organic frameworks (MOFs) are crystalline materials with periodic network structures formed by self-assembly of inorganic metal ions and multifunctional organic ligands, which have ultra-high specific surface area, adjustable pore size, and topological diversity. It has great application prospects in gas storage, adsorption separation, catalysis, and molecular sensing. In recent years, the research on the design, synthesis, structure and performance of MOFs materials has attracted extensive attention from researchers from all walks of life. [0003] HKUST-1 is one of the metal-organic framework materials that has been widely studied. At present, the usage and dosage of copper source and benzenetricarboxylic acid in most preparations o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 吴韬陈艺珮穆学良赵海涛
Owner NINGBO NOTTINGHAM NEW MATERIALS INST CO LTD
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