Preparation method and application of macroporous covalent organic framework
A covalent organic framework, toluene technology, applied in the direction of electrical components, circuits, battery electrodes, etc., can solve the problems of long reaction time, reaction temperature, high cost, high equipment requirements, etc., achieve high specific surface area, high stability, and equipment The simple effect of the requirement
Inactive Publication Date: 2016-02-03
SHANGHAI JIAO TONG UNIV +1
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Problems solved by technology
[0003] At present, covalent organic frameworks are generally synthesized by solvothermal method, which requires a long reaction time (3-7 days) and high reaction temperature (greater than 120°C), and the production method requires high equipment and high cost, making it impossible to achieve Industrial production
In addition, in the current field of lithium batteries / supercapacitors, the pore size of covalent organic frameworks cannot meet the needs, and it is necessary to explore the synthesis method of covalent organic framework materials with larger pore diameters, and study the adsorption characteristics of specific macroporous materials Applications in the field of energy conversion and storage such as lithium batteries / supercapacitors
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Embodiment 1
[0028] This example provides a microwave-assisted preparation method for macroporous covalent organic frameworks for lithium batteries / supercapacitors, the steps are as follows:
[0029] Step 1, get 28.3mg of pyromellitic dianhydride (C 10 h 2 o 6 ,Such as figure 1 shown), 35.1mg of s-tris(4-(p-aminophenyl)-phenyl)benzene (C 42 h 33 N 3 ,Such as figure 2 shown), add 2.2ml of toluene / dioxane / isoquinoline (volume ratio of toluene, dioxane and isoquinoline: 5:5:1) solvent, put into 10ml heat-resistant glass reaction tube , dispersed for 10 minutes to form suspension A;
[0030] Step 2: Suspension A undergoes 3 liquid nitrogen freezing-vacuumizing-degassing steps, seals it and puts it into a microwave reactor, and reacts at 120 degrees for 2 hours to obtain crude product B;
[0031] Step 3: After the crude product B is centrifuged, the insoluble matter is collected, washed three times with 10 ml of tetrahydrofuran and 10 ml of toluene solvent, and dried to obtain a macrop...
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The invention provides a preparation method and application of a macroporous covalent organic framework. The structure of the macroporous covalent organic framework is as shown in a formula I; the preparation method of the macroporous covalent organic framework comprises the following steps of adding pyromellitic dianhydride and tris(4-(p-hydroxyphenyl)-phenyl)benzene into solvent, and dispersing to form a suspension, wherein the solvent is a mixed solvent of methylbenzene, dioxane and isoquinoline; performing liquid nitrogen freezing-vacuumizing-degassing treatment on the suspension for at least three times, sealing and carrying out microwave-assisted thermal reaction on the solvent at the temperature of 120DEG C to obtain a crude product; centrifuging the crude product, then collecting insoluble matters, and sequentially washing and drying with tetrahydrofuran and methylbenzene to obtain the macroporous covalent organic framework. The preparation method and the application provided by the invention have the beneficial effects that the method is pollution-free, mild and simple in reaction conditions and simple in requirement on the equipment, and is suitable for industrial large-scale production.
Description
technical field [0001] The invention relates to a preparation method and application of a macroporous covalent organic framework, belonging to the technical field of polymer materials. Background technique [0002] Covalent organic frameworks (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. periodicity, large specific surface area, diverse structures, and tunable physicochemical properties. 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 framework materials have a stable skeleton structure and permanent nanochannels, and have great potential and broad application prospects as electrode materia...
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Login to View More IPC IPC(8): C08G73/10H01M4/60H01G11/30
CPCC08G73/1003C08G73/1067H01G11/30H01M4/60Y02E60/10
Inventor 魏浩柴双志张雪韩洋顾军辉
Owner SHANGHAI JIAO TONG UNIV