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Method for preparing metal organic framework material from dielectric barrier discharge plasma

A technology of dielectric barrier discharge and metal-organic framework, which is applied in the field of plasma preparation, can solve the problems of difficult control of product morphology and stability, difficulty of plasma establishment, and complicated process flow, so as to achieve easy control of product morphology and stability , control the effect of perfect crystal growth and good application prospects

Active Publication Date: 2018-04-13
QINGDAO UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Microwave and ultrasonic methods react quickly and are convenient for rapid crystallization and nucleation, but the reaction is not easy to control, and the shape and stability of the product are difficult to control
Electrochemical method is a very unique method for preparing metal-organic framework materials, but the process is relatively complicated and the production intensity is not high
[0004] In view of the above problems, Chinese patent CN 105037404A discloses a method for preparing metal-organic framework materials based on discharge plasma in the liquid phase. However, due to the conductivity of the liquid, the ions in the liquid will participate in the conduction to form an ion flow, so that the It is difficult to establish a plasma, and this method is limited in the sufficient mixing of the reaction solution and the regulation of metal-organic framework materials with different topological structures.
[0005] At present, there is no research or report on the preparation of metal-organic framework materials by using dielectric barrier discharge plasma at home and abroad.

Method used

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  • Method for preparing metal organic framework material from dielectric barrier discharge plasma
  • Method for preparing metal organic framework material from dielectric barrier discharge plasma
  • Method for preparing metal organic framework material from dielectric barrier discharge plasma

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Embodiment 1: Preparation of iron metal organic framework material

[0043] Weigh 0.8gFeCl 3 ·6H 2 O and 1.6g terephthalic acid, dissolved in 150mL DMF, stirred for 10min until uniformly dissolved, added 150mL absolute ethanol and mixed, then poured into a beaker, pumped into the plasma reactor with a peristaltic pump, at a discharge voltage of 60V, a current of 1.5A Under the condition of reaction 19min. Let it stand still and centrifuge the reaction solution containing the precipitate. After cleaning, put it in a drying oven and dry it at 160°C for 4 hours. The precipitate is tested by X-ray diffraction (XRD). For details, see the attached figure 2 ,exist figure 2 Among them, the main diffraction peaks are at 2θ=9.7, 12.6, 19 and 22, and the relative diffraction intensity of the crystal is the same as that of the MOF-235 standard, which proves that the crystal material is MOF-235.

Embodiment 2

[0044] Example 2: Preparation of iron metal organic framework materials by argon discharge

[0045] Weigh 0.8gFeCl 3 ·6H 2 O and 1.6g terephthalic acid were dissolved in 150mL DMF, stirred for 10min until uniformly dissolved, then poured into a beaker after adding 150mL absolute ethanol to mix, and pumped into the plasma reactor with a peristaltic pump. The reaction was carried out for 19 minutes under the condition of blowing argon gas. Let it stand still and centrifuge the reaction solution containing the precipitate. After cleaning, put it into a drying oven and dry it at 160° C. for 4 hours.

Embodiment 3

[0046] Example 3: Preparation of iron metal organic framework materials by nitrogen discharge

[0047] Weigh 0.8gFeCl 3 ·6H 2 O and 1.6g terephthalic acid were dissolved in 150mL DMF, stirred for 10min until uniformly dissolved, then poured into a beaker after adding 150mL absolute ethanol to mix, and pumped into the plasma reactor with a peristaltic pump. The reaction was carried out for 19 minutes under the condition of blowing nitrogen gas. Let it stand still and centrifuge the reaction solution containing the precipitate. After cleaning, put it into a drying oven and dry it at 160° C. for 4 hours.

[0048] The iron metal organic framework material in 10mg embodiment 1-3 is used to adsorb the methyl orange solution of 100mL100mg / L, and the change curve of methyl orange concentration with time is as follows image 3 shown.

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Abstract

The invention discloses a method for preparing a metal organic framework material from a dielectric barrier discharge plasma. A metal salt and an organic ligand are added into a solvent, the metal salt, the organic ligand and the solvent are mixed and stirred evenly, and dissolved to obtain a reaction solution, the reaction solution is pumped into an inner tube of a dielectric barrier discharge plasma reactor, overflows from the edge of the inner tube lower than an outer tube, forms an even wall-hanging liquid film between the inner tube and the outer tube, and flows downwards slowly; and meanwhile, a working gas is introduced into the inner tube. Driven by a high-frequency high-voltage power supply, the plasma produced because of the discharge between a liquid electrode and a high-voltageelectrode of the outer tube acts on the liquid film flowing between the inner tube and the outer tube, so that the reaction solution reacts for a certain period of time under the action of the plasma, and the metal organic framework material is prepared. The method has the advantages of high synthesis speed, stable and efficient performance, strong adjustability, strong practicality, no secondarypollution and the like, and has a better application prospect.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional materials, and mainly relates to a method for preparing metal-organic framework materials by dielectric barrier discharge plasma. Background technique [0002] Metal-organic framework materials are a new type of porous coordination functional nanomaterials formed by metals and organic ligands, which is a hot research topic in the fields of coordination chemistry, materials science and crystal engineering. Metal-organic framework materials have the characteristics of ultra-high specific surface area, unique pore structure, pore shape and size, and adjustable chemical environment. They have high adsorption capacity and photocatalytic performance for pollutants in wastewater. [0003] Metal-organic framework materials are synthesized by metal salts and organic ligands in a solvent at medium and low temperatures. The main methods include solvothermal synthesis, stirring synthesis, di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 陶旭梅黄亮
Owner QINGDAO UNIV OF SCI & TECH
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