Preparation method and application of metal organic frame material

A metal-organic framework, mass-part technology, applied in the field of inorganic and material chemistry science, can solve problems such as insufficient structural stability, and achieve the effects of low production cost, increased size, and high safety factor

Inactive Publication Date: 2018-04-10
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In general, most metal-organic framework materials with strong adsorption capacity are synthesized by simple carboxylic acid ligands, and the structure is usually not stable enough.

Method used

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  • Preparation method and application of metal organic frame material
  • Preparation method and application of metal organic frame material
  • Preparation method and application of metal organic frame material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1) Add 0.029 parts by mass of nickel nitrate hexahydrate, 0.016 parts by mass of 4,4'-bipyridyl and 0.01 parts by mass of 4-(5-tetrazolyl)-benzoic acid to N,N-dimethylformamide , water, ethanol and hydrofluoric acid in a mixed solvent to obtain a mixed solution, wherein: the mixed solvent includes 0.95 parts by mass of N,N-dimethylformamide, 1.6 parts by mass of ethanol, 4 parts by mass of water And the hydrofluoric acid of 0.5 mass parts;

[0036] 2) Put the mixed liquid obtained in step 1) in a closed high-pressure reactor, heat it to 115°C and keep it warm for 72 hours, and then cool it to room temperature at a rate of 0.15°C per minute to obtain a reaction product;

[0037] 3) Filter the reaction product obtained in step 2) to obtain green blocky crystals (i.e. the initial synthesis sample of the metal-organic framework), the chemical formula of the green blocky crystals is [Ni(tzba) 0.5 (F)(bipy)]·0.5H 2 O DMF, in the formula: tzba is the negative dianion ligand ...

Embodiment 2

[0042] 1) Add 0.025 parts by mass of nickel nitrate hexahydrate, 0.015 parts by mass of 4,4'-bipyridyl and 0.008 parts by mass of 4-(5-tetrazolyl)-benzoic acid to N,N-dimethylformamide , water, ethanol, and hydrofluoric acid to form a mixed solvent to obtain a mixed solution, wherein: the mixed solvent includes 0.8 parts by mass of N,N-dimethylformamide, 1.4 parts by mass of ethanol, and 3 parts by mass of water And the hydrofluoric acid of 0.6 mass parts;

[0043] 2) Put the mixed solution obtained in step 1) in a closed high-pressure reactor, heat it to 110°C and keep it warm for 65 hours, and then cool it down to room temperature at a rate of 0.1°C per minute to obtain a reaction product;

[0044] 3) Filter the reaction product obtained in step 2) to obtain green blocky crystals (i.e. the initial synthesis sample of the metal-organic framework), the chemical formula of the green blocky crystals is [Ni(tzba) 0.5 (F)(bipy)]·0.5H 2 O DMF, in the formula: tzba is the negative...

Embodiment 3

[0047] 1) Add 0.025 parts by mass of nickel nitrate hexahydrate, 0.017 parts by mass of 4,4'-bipyridine and 0.012 parts by mass of 4-(5-tetrazolyl)-benzoic acid to N,N-dimethylformamide , water, ethanol and hydrofluoric acid mixed solvent to obtain a mixed solution after stirring, wherein:

[0048] The mixed solvent includes 1.1 parts by mass of N,N-dimethylformamide, 1.8 parts by mass of ethanol, 5 parts by mass of water and 0.7 parts by mass of hydrofluoric acid;

[0049] 2) Put the mixed solution obtained in step 1) in a closed high-pressure reactor, heat it to 120°C and keep it warm for 85 hours, and then cool it down to room temperature at a rate of 0.2°C per minute to obtain a reaction product;

[0050] 3) Filter the reaction product obtained in step 2) to obtain green blocky crystals (i.e. the initial synthesis sample of the metal-organic framework), the chemical formula of the green blocky crystals is [Ni(tzba) 0.5 (F)(bipy)]·0.5H 2 O DMF, in the formula: tzba is the...

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Abstract

The invention discloses a preparation method and application of a metal organic frame material. The preparation method comprises the steps: adding nickel nitrate hexahydrate, 4,4'-bipyridine and 4-(5-tetrazolyl)-benzoic acid into a mixed solvent composed of N,N-dimethylformamide, ethanol, water and hydrofluoric acid, and then, carrying out uniform stirring to obtain a mixed solution, wherein the mixed solvent comprises water, ethanol, N,N-dimethylformamide and hydrofluoric acid; placing the obtained mixed solution into a sealed high-pressure reactor, heating the mixed solution to 110-120 DEG C, preserving the heat for 65-85h, and then, cooling the mixed solution to the room temperature at the speed of 0.1-0.2 DEG C / min to obtain a reaction product; filtering the obtained reaction product to obtain a green bulk crystal; and exchanging the obtained green bulk crystal with methanol for 48-96h, and then, carrying out vacuum heating at 180 DEG C for 4-8h to obtain the metal organic frame material. The metal organic frame material is used for realizing selective adsorptive separation of C2H4 in the mixed gas of C2H4 and CH4.

Description

technical field [0001] The invention relates to the field of inorganic and material chemistry sciences, in particular to a metal organic framework material and its preparation method and application. Background technique [0002] Low-carbon hydrocarbons are important energy chemicals and play a very important role in the field of petrochemicals. Whether it is in the preparation of chemicals or used as energy, it is very important to obtain high-purity low-carbon hydrocarbons. While realizing ethylene (C 2 h 4 ) and methane (CH 4 ) is a very important industrial process. As the main component of natural gas, methane is an efficient clean energy and one of the most potential energy sources to replace fossil fuels; ethylene is the basic component of synthetic fibers, synthetic rubber, synthetic plastics (polyethylene and polyvinyl chloride), and synthetic ethanol Chemical raw materials are the core of the petrochemical industry. It is of great practical significance to se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01J20/22B01J20/30B01D53/02
CPCB01D53/02B01J20/226C08G83/008
Inventor 侯磊王海华杨红云时文娟马丽娜王尧宇
Owner NORTHWEST UNIV
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