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Rapid preparation method of environment-friendly metal-organic framework material

A metal-organic framework, environmentally friendly technology, applied in the direction of 1/11 group organic compounds without C-metal bonds, 2/12 groups of organic compounds without C-metal bonds, copper organic compounds, etc., which can solve the complex preparation process. , increase production cost, slow precipitation and other problems, to achieve the effect of fast adsorption rate, low production cost, no secondary pollution

Active Publication Date: 2016-06-22
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the synthesis methods of metal-organic frameworks reported more mainly include solvothermal method and hydrothermal synthesis method. These two methods need to set a certain pressure in a closed reaction system, and the reaction temperature is generally 100-200°C. higher energy consumption
The liquid phase diffusion method is also a commonly used method. This method is to mix, contact, and stand the metal ions and organic ligands in a certain way, and finally slowly precipitate crystals. The serious disadvantage of this method is that it takes too long
In recent years, the ionic liquid method, microwave method, ultrasonic method, etc. have been developed. The increase of auxiliary equipment increases the production cost and complicates the preparation process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 0.5mol of copper sulfate into 1.0L of deionized water and stir to fully dissolve it. Dissolve 1mol NaOH in 0.5L deionized water and add it to a beaker containing a mixture of 0.3mol glutamic acid and 0.4mol glycine. After the amino acid is completely dissolved, add 50mL triethylamine. Slowly add the copper sulfate solution to the glutamic acid solution dropwise under magnetic stirring. After 30 minutes, a solid appears in the solution, and the reaction is continued for 2-3 hours. After the reaction, the resulting mixture is suction filtered, and the solid product is washed with water and alcohol for several times. Afterwards, it was dried at 60° C. for 24 hours to obtain a solid copper-amino acid framework material with a yield of 89.8%.

Embodiment 2

[0017] Add 0.5mol of zinc nitrate into 1.0L of deionized water and stir to fully dissolve it. Dissolve 1 mol of NaOH in 0.5 L of deionized water and add it to a beaker containing 0.3 mol of aspartic acid and 0.2 mol of glutamic acid. After the glutamic acid is completely dissolved, add 35 mL of diethanolamine. The zinc nitrate solution was slowly added dropwise to the amino acid solution under magnetic stirring. After 50 minutes, a solid appeared in the solution, and the reaction was continued for 3 hours. After the reaction was completed, the resulting mixture was subjected to suction filtration. Dry at °C for 24 hours to obtain a solid zinc-amino acid framework material with a yield of 92.6%.

Embodiment 3

[0019] Weigh 0.6 g of the framework material in Example 1 and add it to 0.2 L of acid blue black 1 and reactive red 23 dye solutions with a concentration of 0.1 to 0.5 g / L, stir magnetically for 30 min, and after centrifugation, measure the concentration of the dye solution. Absorbance, dye clearance were 93-95% and 89-93%, respectively.

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PUM

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Abstract

The invention discloses a rapid preparation method of an environment-friendly metal-organic framework material. Amino acid is dissolved in deionized water containing sodium hydroxide, an ethylamine derivative with the volume percentage being 3%-10% is added as a catalyst, a metal salt solution with the concentration being 0.5 mol / L is slowly dropwise added under the action of stirring, and the mixture continues to react for 1-5 h after the solution is dropwise added; the mixture is dried for at least 24 h at the temperature of 80 DEG C after being treated multiple times through filtration, water washing and ethanol washing, and the metal-organic framework material is obtained. The synthesized metal-organic framework material has a large specific surface area and high porosity; the preparation is operated at the room temperature, and energy consumption is reduced; water is taken as a solvent, and the metal-organic framework material is environment-friendly; when the metal-organic framework material is used in dye wastewater, the metal-organic framework material has a high adsorption rate for dye and has high adsorption efficiency; the framework material adsorbing the dye is easily recovered and can be repeatedly used.

Description

Technical field: [0001] The technical field of water treatment of the present invention relates to the rapid preparation and application of an environment-friendly metal-organic framework material used in sewage adsorption technology. Background technique [0002] Metal-organic framework materials are a new type of material developed in recent years. It is a porous material with an infinite network structure formed by self-assembly of inorganic metal ions and organic ligands through coordination, and its metal components are mainly transition metals. Metal ion. There are coordination bond force, hydrogen bond force and other interaction forces in the skeleton material. The metal ions act as nodes in the framework material to connect the ligands, prompting the complexes to form a network structure. Due to the different coordination configurations and particle sizes of different metal ions, the spatial structure and properties of the framework materials obtained by the react...

Claims

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Application Information

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IPC IPC(8): C07F1/08C07F3/06B01J20/22B01J20/30C02F1/28C02F101/34C02F101/38
CPCB01J20/226B01J20/30C02F1/285C02F2101/308C02F2101/34C02F2101/38C07F1/005C07F3/003
Inventor 孙德帅张晓东方龙张中一刘亚丽
Owner QINGDAO UNIV
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