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Preparation method of multifunctional integrated porous solid material for catalytic oxidation

A technology of catalytic oxidation and solid materials, applied in the field of composite materials, can solve problems such as waste and pollution, and achieve the effect of avoiding difficult recycling

Active Publication Date: 2015-09-16
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention proposes a new method for effectively integrating catalytic functions such as catalytic active centers and organic base functions to prepare novel functionalized green catalytic oxidation materials, effectively solving the need for additional addition of homogeneous organic bases in the oxidation system, resulting in waste and pollution to meet the urgent needs of my country for green and low-carbon production methods

Method used

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  • Preparation method of multifunctional integrated porous solid material for catalytic oxidation
  • Preparation method of multifunctional integrated porous solid material for catalytic oxidation
  • Preparation method of multifunctional integrated porous solid material for catalytic oxidation

Examples

Experimental program
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Effect test

Embodiment example 1

[0023] 1) Add 8mmol of chromium nitrate nonahydrate, 8mmol of 2-aminoterephthalic acid, and 20mmol of NaOH into 60mL of water, stir for 5 minutes until completely dispersed, then transfer the above mixed solution to a 100mL reaction kettle, place In an oven at 150°C, keep warm for 12 hours, wash twice with deionized water, soak in 10 mL of N,N-dimethylformamide for half a day, centrifuge, and wash with methanol three times to obtain Cr-MIL-101 ( NH 2 ).

[0024] 2) At room temperature, 0.6 mmol of Cr-MIL-101 (NH 2 ) with 6mL of CHCl 3 The solvent was added to a 25mL round-bottomed flask, stirred until it was completely dispersed, and then 0.9mmol of aziridine was added to it, and the round-bottomed flask was placed in an oil bath at 45°C. After continuous heating for 6 hours, centrifuged, 10mL of CHCl 3 Add it to the obtained solid, soak for two days, centrifuge, and place the obtained solid in a vacuum oven at 80° C. for 12 hours to dry.

[0025] 3) Weigh 0.5mol% of the ...

Embodiment example 2

[0028] 1) Add 27mmol of 5,5'-dimethyl-2,2'-bipyridine to 125mL of 95% concentrated sulfuric acid and keep stirring, slowly add 82mmol of potassium dichromate, control the adding speed in 20 minutes Complete, stir until the temperature drops to 35°C, pour the above solution into 800mL of ice water to cool, filter, wash with deionized water 5 times, then wash with acetone 3 times, and vacuum dry at 60°C for 12h to obtain 2,2'- Bipyridine-5,5'-dicarboxylic acid ligand. Mix and stir 2,2'-bipyridine-5,5'-dicarboxylic acid ligand with hydrochloric acid aqueous solution to obtain 2,2'-bipyridine-5,5'-dicarboxylic acid hydrochloride.

[0029]2) At room temperature, dissolve 0.2 mmol of ferric nitrate nonahydrate in 20 mL of N,N-dimethylformamide, stir until completely dissolved, and then add 0.2 mmol of 2,2'-bipyridine-5, 5'-dicarboxylic acid hydrochloride until completely dissolved, then add 6mmol of benzoic acid, ultrasonic the above mixed solution for 10 minutes, transfer it to a ...

Embodiment example 3

[0033] 1) Dilute 58g of 65% concentrated nitric acid in 131mL of water, add 35g of 2,4,6-tri(4-methylphenyl)-4,4',4"-triazine to it, dissolve and mix The solution was transferred to a polytetrafluoro reactor, heated to 220°C, kept for 5 hours, and washed 5 times with ether to obtain 2,4,6-tris(4-carboxyphenyl)-1,3,5-triazine ligand stand-by.

[0034] 2) At room temperature, dissolve 0.2 mmol of ferric nitrate nonahydrate in 20 mL of N,N-dimethylformamide, stir until completely dissolved, and then add 0.2 mmol of 2,4,6-tris(4- Carboxyphenyl)-1,3,5-triazine ligand until it is completely dissolved, then add 6 mmol of acetic acid, transfer the above mixed solution to a 100 mL polytetrafluoro reactor after ultrasonication for 10 minutes, and then place it in a 120°C Keep warm in the oven for 3 days. After filtering and washing with DMF for 3 times, the precipitate was soaked in ethanol for half a day, filtered and then soaked in ethanol, repeated 3 times, and dried at 40°C for 12...

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Abstract

The invention relates to a preparation method of a multifunctional integrated porous solid material for catalytic oxidation, and belongs to the field of composite materials. The method comprises the following steps: preparing an organic ligand having a Bronsted alkaline function or capable of modifying Bronsted alkalinity, and carrying out a hydrothermal / co-precipitating reaction on the organic ligand and a transition metal source with catalytic activity to obtain the metal organic skeleton catalysis material integrating multiple catalysis functions. The material is applied in benzyl oxidation and alcohol oxidation systems with molecular oxygen as an oxygen source for the first time. The catalysis material prepared through the preparation method of the multifunctional integrated catalysis material effectively integrates a catalytic activity site with the Bronsted alkaline function, solves the problem of difficult activation of the green molecular oxygen source, and avoids the problems of difficult recovery and severe pollution of a homogeneous organic alkali needed by a catalysis system for realizing H removal of C-H bonds; and the multifunctional integrated catalysis material is used in the catalytic oxidation systems with the molecular oxygen as an oxygen source for the first time to realize establishment of high efficiency catalytic oxidation systems under alkali-free conditions.

Description

technical field [0001] The invention belongs to the field of composite materials, and in particular relates to a preparation method of a multifunctional integrated metal-organic framework material for green catalytic oxidation. Background technique [0002] Catalytic oxidation reaction is the core technology for converting chemical raw materials into industrial products. Compared with traditional organic oxidation process, catalytic oxidation process has many advantages such as short reaction time, high selectivity and less by-products, so it is widely used in fine chemical industry , organic synthesis and many other fields. Catalytic oxidation can increase the added value of chemical products, and plays a very important role in green chemical research and industrial applications. For example, converting n-hexanol into n-hexanal through catalytic oxidation can increase the added value of the product many times, which is of great economic significance in chemical production....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J35/10C07C45/36C07C45/39C07C49/675C07C49/78
Inventor 栾奕齐悦彭雄侯俊英范爽杨明
Owner UNIV OF SCI & TECH BEIJING
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