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Preparation method and application of porous nano metal organic framework material

A nano metal and organic framework technology is applied to the preparation of porous nano metal organic framework materials and the application field of adsorption and separation, which can solve the problems of cumbersome production steps, high economic cost and low yield, and achieves improved uniformity and synthesis. Efficiency, high surface area, large pore volume effect

Active Publication Date: 2015-09-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these schemes are time-consuming for large-scale production purposes, and the production steps are cumbersome, the yield is low, and the economic cost is relatively high

Method used

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  • Preparation method and application of porous nano metal organic framework material
  • Preparation method and application of porous nano metal organic framework material
  • Preparation method and application of porous nano metal organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1: Synthesis of nanometer Zn-dimethylimidazole framework

[0034] Dissolve 6g of polyvinylpyrrolidone (PVP) in 450g of water, then add 26g of ZnSO 4 .7H 2 O forms a zinc sulfate solution; dissolve 15g of 2-methylimidazole in 300g of methanol; add the 2-methylimidazole methanol solution dropwise into the zinc sulfate solution within 30 minutes under stirring conditions, mix well, and react at 60°C 5 hours. Cool down naturally, filter the white precipitate, and wash twice with 150ml of water. The filter cake was dried at 100°C for 6 hours and then at 130°C for 8 hours under vacuum (0.2 bar) to obtain 21 g of product;

[0035] The product after washing with water is dispersed in ethanol, and its particle size distribution measured in a Malvern ZS90 particle size analyzer is 120-260nm.

[0036] Product N after drying 2 The specific surface area is 1476m 2 / g (as determined by the Langmuir method).

Embodiment 2

[0037] Embodiment 2: Synthetic nanometer Zn-dimethylimidazole frame

[0038] Dissolve 1g of zinc acetate in 150g of methanol, stir, and reflux at 60°C until the solution becomes turbid to form a mixed solution A; dissolve 4g of PVP in 450g of water, and then add 26g of ZnSO 4 .7H 2 O forms a solution, and then is added dropwise to the A mixture to form a suspension B; dissolve 15g of 2-methylimidazole in 150g of methanol, and then dropwise add it to the B suspension and stir for 30min, after mixing evenly, at 60°C React for 5 hours. Cool down naturally, filter the white precipitate, and then wash twice with 150ml of water. The filter cake was dried at 100°C for 6 hours and then at 130°C for 8 hours under vacuum (0.2 bar) to obtain 20 g of product;

[0039] The product after washing with water is dispersed in ethanol, and its particle size distribution measured in a Malvern ZS90 particle size analyzer is 100-510 nm.

[0040] Product N after drying 2 The specific surface ar...

Embodiment 3

[0041] Embodiment 3: Synthetic nano Zn-dimethylimidazole frame

[0042] Dissolve 8g of polyvinyl alcohol in 300g of methanol, stir, add 20g of zinc acetate dihydrate, and reflux at 60°C until the solution is milky white mixed solution A; dissolve 15g of 2-methylimidazole in 300g of methanol to form solution B, and stir 2-Methylimidazole methanol solution B was added dropwise to the mixture A within 50 min under the condition, and the reaction was continued for 5 hours under the condition of 60°C. Cool down naturally, filter the white precipitate, and then wash twice with 150ml of water. The filter cake was dried at 100°C for 6 hours and then at 110°C for 12 hours under vacuum (0.2 bar) to obtain 20 g of product;

[0043] The product washed with water was dispersed in ethanol, and its particle size distribution was measured in a Malvern ZS90 particle size analyzer to be 50-250nm.

[0044] Product N after drying 2 The specific surface area is 1303m 2 / g (as determined by the...

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Abstract

The invention aims to provide a preparation method and application of a porous nano metal organic framework material, and is characterized in that the preparation method comprises the steps: adding a metal ion, an organic ligand, a surfactant and a nanocrystalline guide agent or a reagent forming the nanocrystalline guide agent into a growth medium, forming a framework structure through chemical complexation, crystallizing, filtering, washing, drying, and finally obtaining the porous nano metal organic framework material. The addition amount of the surfactant is 0-30% of the molar concentration of the metal ion; the metal ion is one or more of Cu<II>, Al<III>, Mg<II>, Fe<III>, Ni<II>, Co<II> and Zn<II>; the organic ligand has at least one atom independently selected from oxygen, sulfur and nitrogen and can be subjected to coordinated complexation to the metal ion through the atom. The method not only can effectively suppress the size of MOFs materials, but also easily improves size homogeneity and synthetic efficiency of the product.

Description

technical field [0001] The invention belongs to the field of new materials and synthetic chemistry, and in particular relates to the preparation of a porous nano metal organic framework material and its application in the adsorption and separation of low-quality methane gas. Background technique [0002] Metal Organic Frameworks (MOFs) materials are one-dimensional, two-dimensional or three-dimensional network materials formed by the coordination complexation of metal ions or their nanoclusters and organic linkers. Metal-organic frameworks have high specific surface areas, extremely low densities, and specific pore distributions. In addition, the cavity structure and surface chemical structure of metal organic framework materials can be effectively designed and manufactured by physical and chemical means. Therefore, the applications of MOFs in gas storage / separation, catalytic processes, drug delivery, and optoelectronics have received extensive attention. [0003] Usually...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/58C07C51/41C07C63/307C07C57/15B82Y30/00B01J20/22B01J20/28B01J20/30B01D53/02
CPCB01D53/02B01J20/226B01J20/28064B01J20/28066B01J20/30B82Y30/00C07C51/418C07C57/15C07C63/307C07D233/58
Inventor 王树东孙天军任新宇胡江亮
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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