Hydrophobic zirconium-metal organic framework material and preparation method thereof

A metal-organic framework and hydrophobic technology, applied in the field of preparation of zirconium-containing metal-organic framework materials, can solve the problem of poor competitive adsorption of VOC and water, and achieve the effects of good hydrophobicity, shortened reaction time, and improved adsorption capacity

Active Publication Date: 2018-02-23
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a hydrophobic M-UiO-66 (

Method used

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  • Hydrophobic zirconium-metal organic framework material and preparation method thereof
  • Hydrophobic zirconium-metal organic framework material and preparation method thereof
  • Hydrophobic zirconium-metal organic framework material and preparation method thereof

Examples

Experimental program
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Example Embodiment

[0049] Example 1

[0050] Dissolve 4mmol of zirconium chloride and 4mmol (equimolar amount) of terephthalic acid in 1.5mL of methanol, and add 0.3mL of glacial acetic acid to it, then ultrasonically (60KHz frequency) for 10min, then transfer to the set Mill in a ball mill jar (one ball milling bead with a diameter of 10.3 mm, five ball milling beads with a diameter of 5.1 mm) for 30 min. Setting procedure: frequency 50Hz; time 30min, speed 1000r / min. After the reaction, the obtained product was washed successively with methanol and DMF for 3-4 times, centrifuged at 7000r / min for 20min, filtered, and dried at 180°C for 20h to obtain the zirconium without nitrogen source of the present invention. The metal-organic framework material is denoted as M-UiO-66(Zr).

Example Embodiment

[0051] Example 2

[0052] Dissolve 4mmol of zirconium chloride and 0.06mmol of dopamine (molar ratio is 1.5%) in 1.5mL of methanol, and add 0.3mL of glacial acetic acid to it, and then ultrasonically (frequency is 60KHz) for 10min, then transfer to the set Mill in a ball mill jar (one ball milling bead with a diameter of 10.3 mm, five ball milling beads with a diameter of 5.1 mm) for 30 min. Setting procedure: frequency 50Hz; time 30min, speed 1000r / min. Add an equivalent amount of terephthalic acid to it after the reaction is over, and continue ball milling for 30 min under the same conditions. Then the obtained product was washed with methanol and DMF for 3-4 times respectively, centrifuged at 7000r / min for 20min, filtered, and dried at 180°C for 20h to obtain the zirconium metal organic framework doped with nitrogen source of the present invention Material, denoted as M-UiO-66 (Zr-N 1.5 ).

Example Embodiment

[0053] Example 3

[0054] Dissolve 4mmol of zirconium chloride and 0.12mmol of dopamine (molar ratio is 3.0%) in 1.5mL of methanol, and add 0.3mL of glacial acetic acid to it, and then ultrasonically (frequency is 60KHz) for 10min, then transfer to the set Mill in a ball mill jar (one ball milling bead with a diameter of 10.3 mm, five ball milling beads with a diameter of 5.1 mm) for 30 min. Setting procedure: frequency 50Hz; time 30min, speed 1000r / min. Add an equivalent amount of terephthalic acid to it after the reaction is over, and continue ball milling for 30 min under the same conditions. Then the obtained product was washed with methanol and DMF for 3-4 times respectively, centrifuged at 7000r / min for 20min, filtered, and dried at 180°C for 20h to obtain the zirconium metal organic framework doped with nitrogen source of the present invention Material, denoted as M-UiO-66 (Zr-N 3.0 ).

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Abstract

The invention discloses a hydrophobic zirconium-metal organic framework material and a preparation method thereof. The preparation method comprises the following steps: (1) feeding and dissolving zirconium chloride in methanol or DMF (Dimethyl Formamide) according to the molar ratio of 100:1.5-7.0, then adding glacial acetic acid for dissolving to obtain a mixture; (2) feeding the mixture in the step (1) into a ball milling tank to carry out ball milling for 10-30 minutes; (3) after the ball milling in the step (2) is finished, adding terephthalic acid with the amount equal to that of the zirconium chloride, continuing ball milling for 10-30 minutes; and (4) washing a product obtained after the step (3) is finished by using the methanol or the DMF in sequence, centrifuging, filtering, anddrying to prepare the nitrogen-doped zirconium-metal organic framework material. The hydrophobic zirconium-metal organic framework material prepared by adopting chemical and mechanical methods has higher specific surface area and higher hydrophobic property, so that the stronger adsorption force of the hydrophobic zirconium-metal organic framework material for chlorobenzene-aldehyde VOC (VolatileOrganic Compound) organic matters is improved.

Description

technical field [0001] The invention belongs to the technical field of metal organic framework materials, and mainly relates to a preparation method and application of zirconium-containing metal organic framework materials. Background technique [0002] Metal-organic frameworks (referred to as: MOFs) are a new type of multifunctional porous material formed by self-assembly of transition metal ions or metal clusters and organic ligands. It has a large specific surface area and modifiable pore structure. Energy storage, gas adsorption and separation, electrical conductivity, catalysis and other fields have shown promising application prospects, especially the prospect of capturing various gases and organic vapors is even more interesting. The huge specific surface area and porosity of MOFs provide materials with huge surface energy, large adsorption capacity and strong adsorption force, which can form advantageous adsorption for various gases and VOCs, such as the use of MOFs ...

Claims

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Application Information

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IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 赵祯霞胡鹏赵钟兴
Owner GUANGXI UNIV
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