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Synthesis method for increasing Pd content of metal organic framework based on Zr(IV) ions

A metal-organic framework and synthesis method technology, applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve the problems of high temperature, low metal-organic framework Pd content, catalytic efficiency and Low yield and other problems, to achieve the effect of stable Pd content, good reproducibility, and low cost

Inactive Publication Date: 2016-06-15
SHANDONG NORMAL UNIV
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The metal-organic framework prepared by the existing method has low Pd content, and when catalyzing the oxidation of benzyl alcohol to benzaldehyde, the catalytic efficiency and yield are low, and the temperature required in the catalytic process is relatively high, and it needs to be produced under an atmospheric pressure of oxygen. can be carried out and other disadvantages

Method used

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  • Synthesis method for increasing Pd content of metal organic framework based on Zr(IV) ions
  • Synthesis method for increasing Pd content of metal organic framework based on Zr(IV) ions
  • Synthesis method for increasing Pd content of metal organic framework based on Zr(IV) ions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1: Preparation of metal-organic framework (PdUiO-68-IP) of Zr(IV) ions

[0038] Under nitrogen protection, 2,5-dibromoaniline (10nmol, 2.51g), 4-methoxycarbonylphenylboronic acid (30nmol, 5.4g), cesium fluoride (47.5nmol, 7.22g), (PPh 3 ) 4 Pd (3.3mmol, 3.8g) was added to a 250mL three-necked flask, 150mL of anhydrous tetrahydrofuran was added, stirred at a constant temperature of 80°C for 48h, cooled to room temperature, the solvent was removed under reduced pressure, and column chromatography (silicagel, CH 2 Cl 2 ) to obtain 2.3 grams of yellow-green solid powder of intermediate A, yield: 64%.

[0039]Put intermediate A (1.66mmol, 0.60g), THF (20mL) and MeOH (20mL) into a 100mL single-necked bottle, and after the solid was completely dissolved, add 10mL of KOH (3.0g, 53.6mmol) in water, at 40°C Stir at constant temperature for 12 h, cool to room temperature, remove THF and MeOH under reduced pressure, add 100 mL of distilled water, and adjust to pH<2 with ...

Embodiment 2

[0045] Example 2: Application of metal-organic framework (PdUiO-68-IP) of Zr(IV) ions as a catalytic material for oxidation of benzyl alcohol

[0046] PdUiO-68-IP (10mg, 1mol%), benzyl alcohol (1.0mmol) was added to 2mL toluene solution according to the feed ratio (molar ratio) 1:100, stirred at 80°C for 30h, and the reaction was tracked by gas chromatography process, the catalytic oxidation yield can reach more than 99% within 20 hours.

[0047] The metal-organic framework (PdUiO-68-IP) of Zr(IV) ions catalyzes the oxidation of benzyl alcohol, and the reaction results are tracked by gas chromatography. The detection results are as follows Image 6 shown.

Embodiment 3

[0048] Example 3: Application of metal-organic framework (PdUiO-68-IP) of Zr(IV) ions as a catalytic material for benzaldehyde condensation

[0049] PdUiO-68-IP (10mg, 1mol%), benzaldehyde (1.0mmol), malononitrile (1.0mmol) were added to the methanol solution according to the feed ratio (molar ratio) 1:100:120, and stirred at room temperature, The reaction process is tracked by a gas chromatograph, and the catalytic oxidation yield can reach more than 99% within 7 hours.

[0050] The metal-organic framework (PdUiO-68-IP) of Zr(IV) ions catalyzes the benzaldehyde condensation reaction, and the reaction results are tracked by gas chromatography. The detection results are as follows Figure 8 shown.

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Abstract

The invention discloses a synthesis method for increasing the Pd content of a metal organic framework based on Zr(IV) ions. The method comprises the following steps: performing a coordination polymerization reaction between an organic ligand (I) and ZrCl4, and performing post-synthesis modification of the product, wherein the post-synthesis modification comprises the following specific steps: enabling a coordination polymerization reaction product, 2-pyridylaldehyde or salicylaldehyde and a catalyst formic acid in a molar ratio of 1:(1-4):(0.1-0.3) to react in an organic solvent; performing centrifugal washing of the product and dispersing in an organic solvent; adding palladium nitrate in a molar ratio of 1:(0.8-1.2); after the reactions, centrifuging and drying to obtain powder; dispersing the obtained powder into water; adding sodium borohydride in a molar ratio of 1:(0.5-1.5); and after the reactions, centrifuging, washing and drying to obtain the product. In the invention, the synthesized compound is an organic-inorganic composite supermolecular material and has a metal organic framework which is easy to operate and low in cost and has nanoscale particle size; and the compound has very high efficiency when being used as a catalytic material for benzyl alcohol oxidation and benzaldehyde condensation.

Description

technical field [0001] The present invention relates to a synthesis method of a Zr(IV) ion-based metal organic framework (marked as: PdUiO-68-IP), in particular to a synthesis method for increasing the Pd content of a Zr(IV) ion-based metal organic framework. Background technique [0002] Benzaldehyde is one of the simplest aromatic aldehydes, which widely exists in plants, especially Rosaceae plants, mainly in the form of glycosides in the bark, leaves or seeds of plants. Benzaldehyde is a synthetic flavor for food that is allowed to be used in the national standard GB2076-2011, and can be used to prepare cherry, cocoa, vanilla, and almond flavors. It is also widely used in industry. As an important chemical raw material, it is used for the preparation of lauric aldehyde, lauric acid, phenylacetaldehyde and benzyl benzoate, etc.; it is used for the determination of ozone, phenol, alkaloids and methylene next to the carboxyl group Base reagent; it can be used as a special t...

Claims

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Application Information

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IPC IPC(8): C07F19/00B01J31/22C07C45/29C07C47/54C07C253/30C07C255/34
CPCB01J31/1691B01J31/2243B01J2231/342B01J2231/70B01J2531/0213B01J2531/48B01J2531/824C07C45/29C07C253/30C07F15/00C07C47/54C07C255/34
Inventor 董育斌李延安杨松刘启奎
Owner SHANDONG NORMAL UNIV
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