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Three-dimensional covalent organic framework compound, its preparation method, and its application
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A technology of covalent organic frameworks and compounds, which is applied in the field of three-dimensional covalent organic framework compounds and their preparation, and can solve problems such as limitations in synthesis and preparation
Active Publication Date: 2021-04-13
TSINGHUA UNIV
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[0004] There are many reports on the existing two-dimensional COF, but the three-dimensional COF is subject to more restrictions in terms of design strategy, topology type, synthesis and preparation, etc.
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[0060] The embodiment of the present invention also provides a preparation method of a three-dimensional covalent organic framework compound, comprising the following steps:
[0061] S1, put the triptycene compound shown in formula (5), the pyrene compound shown in formula (6) and the organic solvent together into a container, vacuumize and seal the container;
[0062] S2, heating the sealed container at 50°C to 200°C to make the triptycene compound react with the pyrene compound to form a solid precipitate;
[0063] S3, the precipitate is filtered out, soaked in an organic solvent, washed and dried, and the obtained solid product is the three-dimensional covalent organic framework compound.
[0064]
[0065] R in formula (5) 1 and R in formula (6) 2 The reaction generates the linking group. For example, when the linking group is -C=N-, R 1 and R 2 One of them is an aldehyde group (-CHO), and the other is an amino group (-NH 2 ). When the linking group is -C=N-NH-, R...
[0080] According to the above formula, iron powder (0.22g, 3.94mmol) was added into a solution of triptycene (10.00g, 39.32mmol) in chloroform (150ml). Bromine (12 mL, 234.20 mmol) was added to the mixture at 0° C., and the mixture was stirred for 30 minutes, then heated to room temperature, and heated to reflux for 8 hours after a period of mild reaction. After the reaction, the mixture was cooled to room temperature, the solidiron powder catalyst was removed by filtration, and washed 3 times with water and saturated brine, the organic phase was evaporated, and the crude product was purified by silica gelcolumn chromatography, and the eluent was dichloromethane to obtain 28 g of 2 ,3,6,7,14,15-hexabromotriptycene, yield 97.9%.
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Abstract
The present invention provides a three-dimensional covalent organic framework compound, which is formed by linking a hexavalent group of triptycene and a tetravalent group of pyrene through a linking group. In at least a part of the three-dimensional covalent organic framework compound, each Each triptycene-type hexavalent group is respectively connected with six adjacent pyrene-type tetravalent groups, and each pyrene-type tetravalent group is respectively connected with adjacent four triptycene-type hexavalent groups, thereby A regular hexagonal prism-like three-dimensional topological network structure is formed, and the linking group contains dynamic covalent bonds. The invention provides a preparation method and application of a three-dimensional covalent organic framework compound.
Description
technical field [0001] The invention belongs to the field of covalent organic framework compounds, and in particular relates to a novel three-dimensional covalent organic framework compound, a preparation method thereof, and an application thereof. Background technique [0002] Covalent Organic Frameworks (COF) is a porous framework structure with a very regular periodic order formed by linking organic structural units with dynamic covalent bonds. As an emerging crystalline porous polymer, COFs have shown great application potential in various fields due to their light weight, low density, permanent high porosity, high specific surface area, and relatively high thermal stability. . [0003] COF can be divided into two-dimensional (2D) COF and three-dimensional (3D) COF according to the structure. In 2D COFs, the basic building blocks are covalently bonded to form 2D frameworks, and these 2D frameworks are further stacked to form a periodically aligned stack structure. In ...
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