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Hydrophobic palladium/metal organic framework material, preparation method thereof and application of hydrophobic palladium/metal organic framework material to synthesis of 2,5-dimethylfuran

A metal-organic framework and dimethylfuran technology, which is applied in the application field of catalyzing hexose to prepare 2,5-dimethylfuran, can solve the problems of long reaction time, low substrate conversion rate and the like, and achieves a simple preparation method, The effect of high activity and mild reaction conditions

Active Publication Date: 2018-10-16
NANJING AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, metal ions or simple substances act on polymethylhydrogensiloxane to show high selectivity to the target product, but there are disadvantages such as low substrate conversion rate and long reaction time.

Method used

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  • Hydrophobic palladium/metal organic framework material, preparation method thereof and application of hydrophobic palladium/metal organic framework material to synthesis of 2,5-dimethylfuran
  • Hydrophobic palladium/metal organic framework material, preparation method thereof and application of hydrophobic palladium/metal organic framework material to synthesis of 2,5-dimethylfuran
  • Hydrophobic palladium/metal organic framework material, preparation method thereof and application of hydrophobic palladium/metal organic framework material to synthesis of 2,5-dimethylfuran

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Preparation of ordinary Pd / MIL-53(Al) catalytic material

[0043] Press Al(NO 3 ) 3 9H 2 O: terephthalic acid: water molar ratio is 1:1:100, mix and add to 25mL hydrothermal reaction kettle, put it in an oven at 220°C for hydrothermal treatment for 72h, then wash with deionized water and vacuum dry at 100°C A MIL-53(Al) carrier was obtained.

[0044] The prepared 0.25g MIL-53(Al) carrier was added to the solution containing 13mg PdCl 2 In methanol (1.2mL) solution, sonicate for 30min and stir at room temperature for 24h, then centrifuge at 8000r / min, wash with N,N-dimethylformamide 3 times, 10mL each time, vacuum dry at 90°C for 6h, and grind. Finally, it was reduced at 250°C for 3h in a hydrogen atmosphere (20%H 2 / Ar flow rate is 30cm 3 / min, the heating rate is 10℃ / min), and the ordinary Pd / MIL-53(Al) catalytic material is prepared.

[0045] pass figure 1 High Angle Annular Dark Field-Scanning Transmission Electron Microscopy (HAADF-STEM) and figure 2 w...

Embodiment 2

[0061] (1) Preparation of hydrophobic Pd / MIL-101(Cr) catalytic material

[0062] Press Cr(NO 3 ) 3 9H 2 O: terephthalic acid: water molar ratio is 1:1:200, mix and add to 25mL hydrothermal reaction kettle, put hydrothermal treatment in 220°C oven for 12h, then wash with ethanol and vacuum dry at 90°C to obtain MIL -101(Cr) carrier.

[0063] The prepared 0.25g MIL-101 (Cr) carrier was added to the solution containing 21mg PdCl 2 In methanol (1.2mL) solution, sonicate for 30min and stir at room temperature for 24h, then centrifuge at 8000r / min, wash with N,N-dimethylformamide 3 times, 10mL each time, vacuum dry at 90°C for 6h, and grind. Finally, it was reduced at 250°C for 3h in a hydrogen atmosphere (20%H 2 / Ar flow rate is 30cm 3 / min, and the heating rate is 10°C / min), the common Pd / MIL-101(Cr) catalytic material is prepared.

[0064] Weigh 20 mg of ordinary Pd / MIL-101 (Cr) solid powder, evenly spread it into a micro watch glass, and put it into the lining of a hydrothe...

Embodiment 3

[0068] (1) Preparation of hydrophobic Pd / UiO-66(Zr) catalytic materials

[0069] Press ZrCl 4 : Terephthalic acid: N,N-dimethylformamide molar ratio is 1:1:300, mix and add to 25mL hydrothermal reaction kettle, put hydrothermal treatment in 130℃ oven for 24h, then wash with ethanol, The UiO-66(Zr) carrier was obtained after vacuum drying at 90°C.

[0070] The prepared 0.25g UiO-66(Zr) support was added to the solution containing 6mg PdCl 2 In methanol (1.2mL) solution, sonicate for 30min and stir at room temperature for 24h, then centrifuge at 8000r / min, wash with N,N-dimethylformamide 3 times, 10mL each time, vacuum dry at 90°C for 6h, and grind. Reduction at 250°C for 3h in a hydrogen atmosphere (20%H 2 / Ar flow rate is 30cm 3 / min, and the heating rate is 10℃ / min), the ordinary Pd / UiO-66(Zr) catalytic material is prepared.

[0071] Weigh 20mg of ordinary Pd / UiO-66(Zr) solid powder, evenly spread it into a micro watch glass, and put it into the lining of a hydrothermal ...

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Abstract

The invention discloses a hydrophobic palladium / metal organic framework material which is a solid catalytic material prepared by taking a porous metal organic framework as a carrier, introducing elemental palladium by using an impregnation-reduction method, and then, carrying out polydimethylsiloxane coating treatment. The invention further discloses a method for preparing 2,5-dimethylfuran by selectively catalyzing hexose by using the hydrophobic palladium / metal organic framework material. The method comprises the steps: dissolving hexose into alcohol, and carrying out a reaction at 70-130 DEG C for 0.25-12 h under the action of an acidic additive by taking the hydrophobic palladium / metal organic framework material as a catalyst and polymethylhydrosiloxane as a hydrogen donor, wherein theconcentration of hexose in alcohol is 0.2-10wt%, and the total quantity of Pd contained in the used hydrophobic palladium / metal organic framework material is 0.1-5mol% relative to hexose. The hydrophobic palladium / metal organic framework material disclosed by the invention is stable in structure, and the catalytic efficiency is obviously higher than that of a commercially available palladium carbon and common palladium / metal organic framework material under the same condition.

Description

technical field [0001] The invention relates to a hydrophobic palladium / metal organic framework material and its preparation method and application, in particular to a palladium / metal organic framework material with uniform active site distribution, stable structure and strong hydrophobicity and a preparation method thereof, and the catalytic performance of the material Application of hexose sugars to prepare 2,5-dimethylfuran. Background technique [0002] In recent years, 2,5-dimethylfuran has been reported as a liquid biofuel with great application prospects. Its energy density (31.5MJ / L), octane number (119) and boiling point (92-94°C ) are equivalent to or even better than gasoline (energy density 35MJ / L, octane number 95.8, boiling point 96.3°C) [1] . Usually, under the action of metal catalysts (such as Pd, Pt, Ru, Ni, Cu, etc.), 5-hydroxymethylfurfural can be converted into 2,5-dimethylfuran through hydrogenation and dehydration reaction [2] . However, conditions...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/16B01J23/44C07D307/36
CPCC07D307/36B01J23/44B01J31/1691B01J20/22B01J20/30B01J31/16B01J31/28B01J20/3212Y02E50/10Y02P20/584B01J2/30
Inventor 方真李虎
Owner NANJING AGRICULTURAL UNIVERSITY
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