Ultra-microporous zirconium-based metal organic framework material as well as preparation method and application thereof

An organic framework and metal-based technology, applied in the field of preparation of ultra-microporous zirconium-based metal-organic framework materials, can solve problems such as poor stability, incompatible selectivity, and high adsorption capacity, and achieve weakened acidity, increased adsorption capacity, and increased selectivity. The effect of specific surface area

Active Publication Date: 2020-05-29
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to develop an ultra-microporous zirconium-based metal-organic framework material and its preparation method in view of the problems of poor stability of existing MOFs materials and high adsorption capacity and incompatible selectivity in the two-component gas coexistence system

Method used

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  • Ultra-microporous zirconium-based metal organic framework material as well as preparation method and application thereof
  • Ultra-microporous zirconium-based metal organic framework material as well as preparation method and application thereof
  • Ultra-microporous zirconium-based metal organic framework material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Preparation of zirconium-based MOFs material

[0030] Add the precursor zirconium chloride to 60mL DMF, 10mL acetic acid and the precursor terephthalic acid in an equimolar amount to the zirconium chloride, continue to stir at room temperature for 30min, then transfer to a 100mL reaction kettle, and place it in a programmed incubator, 120 React at ℃ for 24 hours, then wash with DMF and ethanol for 3-4 times respectively, set the centrifugation speed at 4000-6000r / min, set the centrifugation time at 10-15min, and then dry it.

Embodiment 2

[0031] Embodiment 2: Preparation of zirconium-based MOFs material

[0032] The precursor zirconium chloride and basic N-pyrazine molecules were dissolved in 60mL organic solvent DMF at a mass ratio of 100:3.0, and ultrasonically dissolved for 10 minutes to obtain a mixed solution, which was microwaved at 100°C for 10 minutes. The reaction temperature was 100°C; After the reaction is over, add 60mL DMF, 10mL acetic acid and the precursor terephthalic acid in an equimolar amount to zirconium chloride, continue to stir at room temperature for 30min, then transfer to a 100mL reactor and place it in a temperature-programmed oven , reacted at 120°C for 24 hours, then washed with DMF and ethanol for 3-4 times respectively, the centrifugal speed was set at 4000-6000r / min, the centrifugal time was set at 10-15min, and then dried.

Embodiment 3

[0033] Embodiment 3: Preparation of zirconium-based MOFs material

[0034] The precursor zirconium chloride and basic N-pyrazine molecules were dissolved in 60mL of organic solvent DMF at a mass ratio of 100:5.0, and ultrasonically dissolved for 10 minutes to obtain a mixed solution, which was microwaved at 100°C for 10 minutes. The reaction temperature was 100°C; After the reaction is over, add 60mL DMF, 10mL acetic acid and the precursor terephthalic acid in an equimolar amount to zirconium chloride, continue to stir at room temperature for 30min, then transfer to a 100mL reactor and place it in a temperature-programmed oven , reacted at 120°C for 24 hours, then washed with DMF and ethanol for 3-4 times respectively, the centrifugal speed was set at 4000-6000r / min, the centrifugal time was set at 10-15min, and then dried.

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Abstract

The invention discloses an ultra-microporous zirconium-based metal organic framework material as well as a preparation method and application thereof. The method comprises the following steps: (1) respectively dissolving precursor zirconium chloride and alkaline N-pyrazine molecules in an organic solvent DMF (Dimethyl Formamide) according to a mass ratio of 100: (1.5-7.0), and carrying out ultrasonic dissolution to obtain a mixed solution; (2) transferring the mixed solution into a microwave reaction tank, and carrying out microwave reaction; (3) adding DMF (Dimethyl Formamide), acetic acid and precursor terephthalic acid with the same molar weight as zirconium chloride, and continuing to stir at room temperature to obtain a mixed solution; (4) transferring the mixed solution into a reaction kettle, putting the reaction kettle into a temperature programming box, and reacting at 120 DEG C; and (5) washing a product obtained after the reaction in the step (4) by using DMF and ethanol respectively, and centrifuging and drying the product. The zirconium-based MOFs material constructed by adopting a microwave-assisted strategy has relatively high specific surface area and relatively small pore size distribution, and meanwhile, the acidic sites of MOF metal sites are weakened, so that the CO2 adsorption capacity is remarkably improved due to the synergistic effect.

Description

technical field [0001] The invention belongs to the field of porous nano science and technology, and mainly relates to a preparation method and application of an ultramicroporous zirconium-based metal organic framework material. Background technique [0002] Since the 21st century, due to the increasing consumption of non-renewable energy such as coal, oil and natural gas and other fossil fuels while their storage capacity has been decreasing, people are increasingly aware of the need to find a new type of renewable clean energy to curb the further expansion of the energy crisis. necessity. As a new type of clean energy, methane has the highest hydrogen-to-carbon ratio among all hydrocarbons, and can be used in many aspects such as power generation, cooking, heat source and fuel. Biogas from renewable energies contains a lot of methane, but at the same time also a lot of carbon dioxide. Therefore, how to remove carbon dioxide from biogas to obtain high-purity methane is th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01J20/22B01D53/02B01J20/30
CPCB01D53/02B01D2257/504B01J20/226C08G83/008Y02P20/151Y02C20/40
Inventor 纪红兵胡鹏王永庆王皓江春立许君楚周杰
Owner SUN YAT SEN UNIV
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