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8-hydroxyquinoline-based organic ligand, organic frameworks and preparation methods of organic frameworks

An organic ligand, hydroxyquinoline technology, applied in the field of inorganic-organic nanomaterial preparation, can solve problems such as limiting the application of organometallic frameworks, and achieve the effects of simple and easy preparation method, good stability, and mild reaction conditions

Inactive Publication Date: 2016-06-22
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the existing organometallic framework materials have a better adsorption effect on gases at low temperature and high pressure, which limits the application of organometallic frameworks in gas adsorption.

Method used

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  • 8-hydroxyquinoline-based organic ligand, organic frameworks and preparation methods of organic frameworks
  • 8-hydroxyquinoline-based organic ligand, organic frameworks and preparation methods of organic frameworks
  • 8-hydroxyquinoline-based organic ligand, organic frameworks and preparation methods of organic frameworks

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Metal-organic framework Zn-MOF based on Zn(II)

[0034] Taking 8-hydroxyquinoline as the preparation method of the organic ligand L of the parent, comprises the steps:

[0035]

[0036] N Under protection, add 5,7-dibromo-8-p-methoxypyridine quinoline 14.0g (10mmol), 4-pyridine boric acid 3.2g (26mmol), anhydrous sodium carbonate 13.6g ( 128mmol), tetrakistriphenylphosphine palladium 0.8g (0.6mmol), benzene, ethanol, water 40ml each mixed solution (ultrasonic deoxygenation 15min), heated to reflux for 30h. After the reaction liquid was cooled, it was poured into water, extracted twice with dichloromethane, and the extract was spin-dried to obtain a crude product, which was obtained by column chromatography as a white solid, 3.4 g, with a yield of 67.20℅.

[0037] The preparation method of the metal organic framework comprises the following steps:

[0038] The organic ligand L (11.7mg0.03mmol) and zinc perchlorate (11.1mg0.03mmol) were placed in N,N-dimet...

Embodiment 2

[0040] Example 2: Co(II)-based metal-organic frameworks

[0041] The preparation method of the metal organic framework comprises the following steps:

[0042] Substituting cobalt nitrate for zinc perchlorate and repeating the synthesis of Zn-MOF, a purple-red bulk single-crystal Co-MOF was obtained, whose structural formula is [ZnC 20 h 12 N 3 o 3 ] n , n is a non-zero natural number; the yield is 21.0 mg, and the yield is 84.0%. The schematic diagram of the single crystal structure of Co-MOF is shown in figure 2 As shown, the X-ray powder diffraction pattern is shown in image 3 As shown, the infrared spectrum is shown as Figure 5 As shown, the TGA spectrum is as Figure 7 shown.

[0043] The newly prepared Co-MOF (80mg) was heated at 200°C for 2 hours under normal pressure to remove all the guest water molecules, and then heated at 70°C for 8 hours in a vacuum state to obtain a sample without the object for gas adsorption performance characterization. CO at room ...

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Abstract

The invention discloses an 8-hydroxyquinoline-based organic ligand, organic frameworks and preparation methods of the organic frameworks. The 8-hydroxyquinoline-based organic ligand L is shown as the chemical structural formula below. Each metal-organic framework is prepared according to the steps of dissolving the organic ligand L and divalent metal salt into an N,N- dimethylformamide aqueous solution, regulating a pH (potential of hydrogen) value to enable the solution to be faintly acid, keeping the solution at 120 DEG C for 72-76 hours and decreasing the temperature of the solution to 20-35 DEG C after 48-50 hours. Taking the 8-hydroxyquinoline-based organic ligand as a substrate, two different metal-organic frameworks are prepared and are large in cavity structure and high in stability, thereby being excellent in gas storage and micromolecule adsorption and capable of adsorbing gas micromolecules such as CO2 and CH4 at the room temperature, wherein at the room temperature, maximum CO2 adsorption quantity and maximum CH4 adsorption quantity of a Zn-MOF (metal-organic framework) reaches 76.1cm<3> / g and 7.1cm<3> / g respectively, and maximum CO2 adsorption quantity and maximum CH4 adsorption quantity of a Co-MOF reaches 64.9cm<3> / g and 13.2cm<3> / g respectively.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic-organic nanometer materials, and specifically relates to an organic ligand based on 8-hydroxyquinoline, an organic framework and a preparation method thereof. Background technique [0002] Metal-organic framework (Metal-organic Framework, MOF) is a research hotspot in recent years. It is assembled to form a porous material through the interaction between metal ions or metal clusters and organic ligands. Compared with traditional porous materials, MOF With porosity, large specific surface area and pore volume in the frame, it has been widely studied and applied in the fields of gas storage, drug loading, chemical sensing, catalysis, and enrichment separation detection. [0003] At present, with the increase of carbon dioxide emissions, the greenhouse effect is becoming more and more serious, how to reduce the CO in the air 2 content has become a worldwide environmental problem. D...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/14C07F3/06C07F15/06C07F1/08B01J20/22B01D53/02
CPCB01D53/02B01D2257/504B01D2257/7025B01J20/223C07D401/14C07F1/08C07F3/06C07F15/065Y02C20/20Y02C20/40Y02P20/151
Inventor 董育斌刘毅尉永良马建平
Owner SHANDONG NORMAL UNIV
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