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Microwave auxiliary preparation method of keto-enamine covalently linked organic framework

A covalent organic framework, microwave-assisted technology, used in chemical instruments and methods, other chemical processes, etc., can solve the problems of high cost, inability to realize industrial production, and the performance of covalent organic frameworks cannot meet the needs, and achieves good crystallinity. , The requirements of the equipment are simple, the effect of high specific surface area

Active Publication Date: 2015-09-23
芩洋科技(上海)有限公司
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Problems solved by technology

At present, in the field of gas adsorption storage and energy transfer materials, the performance of covalent organic frameworks cannot meet the needs, and the production method has high requirements for equipment and high cost, and cannot realize industrial production

Method used

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  • Microwave auxiliary preparation method of keto-enamine covalently linked organic framework
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  • Microwave auxiliary preparation method of keto-enamine covalently linked organic framework

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Embodiment 1

[0026] This example provides a microwave-assisted preparation method for ketoenamines linking covalent organic frameworks, the steps are as follows:

[0027] Step 1, get 63mg of 1,3,5-triformylpyroglucinol (C 9 h 6 o 6 ), 48mg of p-phenylenediamine (C 6 h 8 N 2 ), add 7ml of mesitylene / dioxane / 3mol / L acetic acid (volume ratio: 3:3:1) solvent, put it into a 10ml heat-resistant glass reaction tube, and ultrasonically disperse for 5 minutes to form suspension A;

[0028] Step 2: Suspension A undergoes 3 liquid nitrogen freezing-vacuumizing-degassing steps, seals it and puts it into a microwave reactor, and reacts at 100 degrees for 1 hour to obtain crude product B;

[0029] Step 3: After the crude product B is centrifuged, the insoluble matter is collected, washed twice with 2 ml of mesitylene and 2 ml of acetone solvent, and dried to obtain a covalent organic framework linked by ketoenamine.

[0030] Implementation effect, the electron micrograph of the covalent organic fr...

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Abstract

The invention discloses a microwave auxiliary preparation method of a keto-enamine covalently linked organic framework. The method comprises the following steps: charging 1 , 3 , 5-triformylphloroglucinol and p-phenylenediamine into solvent, and ultrasonically dispersing to form suspension; the solvent is mixed solvent of sym-trimethylbenzene, dioxane and acetum; freezing, by liquid nitrogen, vacuumizing and degassing the suspension for at least three times, then sealing, carrying out the thermal reaction for 1 hour under the assistance of microwaves at the temperature of 100 DEG C, and obtaining a crude product; and centrifuging the crude product, collecting insoluble matters, washing the insoluble matters sequentially by sym-trimethylbenzene and acetone to obtain the keto-enamine covalently linked organic framework, and obtaining the keto-enamine covalently linked organic framework. The method is pollution-free, the reaction condition is moderate and simple, the requirement on equipment is simple, and the method is suitable for the industrialized mass production.

Description

technical field [0001] The invention relates to a preparation method in the technical field of polymer materials, in particular to a microwave-assisted preparation method in which ketoenamine is connected to a covalent organic framework. Background technique [0002] Covalent Organic Frameworks (COFs) are a class of polymer porous materials with regular porous structures, which are formed by connecting organic units through covalent bonds, and have a large specific surface area, diverse structures, and adjustable The physical and chemical properties make it have great application prospects in the fields of energy storage and transfer. After searching the literature of the prior art, it was found that in 2012 Donglin JIANG et al. published Covalent Organic Framework (covalent organic framework) on pages 6010-6022 of Volume 41 of "Chemical Society Reviews". Compared with traditional linear and three-dimensional polymers, covalent organic frameworks have completely different s...

Claims

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Application Information

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IPC IPC(8): C08G73/00B01J20/22
Inventor 魏浩柴双志李明杨志魏良明
Owner 芩洋科技(上海)有限公司
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