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Preparation method for cage type covalent organic framework material

A covalent organic framework and cage technology, applied in the field of preparation of covalent organic framework materials, can solve the problems of restricting the development of new structures and new materials, limited reaction types, few three-dimensional covalent organic framework materials, etc., and achieve easy industrialization The effect of mass production, high chemical and thermal stability, and small density

Active Publication Date: 2018-12-11
江苏宏光布业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far, the preparation of covalent organic framework materials is limited to easy chemical reactions involving a very limited variety of reactions, which limits the development of new structures and materials.
Moreover, more studies focus on 2D covalent organic frameworks, and there are few reports on 3D covalent organic frameworks

Method used

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  • Preparation method for cage type covalent organic framework material
  • Preparation method for cage type covalent organic framework material
  • Preparation method for cage type covalent organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Weigh 0.8524g of copper chloride dihydrate, place it in a 50mL polytetrafluoroethylene-lined autoclave, add 25mL of ethanol, mix well, and cover the kettle tightly.

[0026] (2) Put the autoclave in a muffle furnace and react at 160°C for 24h. Cool to room temperature, filter under reduced pressure, and dry the product in vacuum at 50°C for 12 hours. Store in a dark place under a nitrogen protection atmosphere to obtain cuprous chloride nanocrystals with a diameter of 2-10 nm.

[0027] (3) 10 mg of cuprous chloride crystal powder, 10 mg of p-phenylenediamine and 38 mg of tetrakis(4-anilino)methane were dissolved in 5.0 mL of acetonitrile, and stirred at room temperature for 24 h.

[0028] (4) The reaction mixture was taken out, washed with 25% ammonia water, water and acetone respectively, and dried and stored.

[0029] figure 2 Contains the reaction process and structural schematic diagram of this embodiment.

[0030] image 3 Transmission electron micrograph...

Embodiment 2

[0033] (1) Weigh 0.8524g of copper chloride dihydrate, place it in a 50mL polytetrafluoroethylene-lined autoclave, add 25mL of ethanol, mix well, and cover the kettle tightly.

[0034] (2) Put the autoclave in a muffle furnace and react at 160°C for 24h. Cool to room temperature, filter under reduced pressure, and dry the product in vacuum at 50°C for 12 hours. Store in a dark place under a nitrogen protection atmosphere to obtain cuprous chloride nanocrystals with a diameter of 2-10 nm.

[0035] (3) 10 mg of cuprous chloride crystal powder, 23 mg of p-dibromobenzene and 38 mg of tetrakis(4-anilino)methane were dissolved in 5.0 mL of acetonitrile, and the temperature was maintained at 120° C. under the protection of nitrogen, and stirred for 24 h.

[0036] (4) The reaction mixture was taken out, washed with 25% ammonia water, water and acetone respectively, and dried and stored.

[0037] figure 1 Contains the reaction process and structural schematic diagram of this embodim...

Embodiment 3

[0039] (1) Weigh 0.8524g of copper chloride dihydrate, place it in a 50mL polytetrafluoroethylene-lined autoclave, add 25mL of ethanol, mix well, and cover the kettle tightly.

[0040] (2) Put the autoclave into a muffle furnace and react at 160°C for 24h. Cool to room temperature, filter under reduced pressure, and dry the product in vacuum at 50°C for 12 hours. Store in a dark place under a nitrogen protection atmosphere to obtain cuprous chloride nanocrystals with a diameter of 2-10 nm.

[0041] (3) 20 mg of cuprous chloride crystal powder, 10 mg of p-phenylenediamine and 38 mg of tetrakis(4-anilino)methane were dissolved in 5.0 mL of acetonitrile, and stirred at room temperature for 12 h.

[0042] (4) The reaction mixture was taken out, washed with 25% ammonia water, water and acetone respectively, and dried and stored.

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Abstract

The invention provides a preparation method for a cage type covalent organic framework material. According to the method, a cuprous chloride catalyst with the nanoscale is prepared by adopting a solvothermal method, and the cage type three-dimensional covalent organic framework material is prepared by utilizing tetra(4-anilino)methane and a monomer such as p-phenylenediamine or p-dibromobenzene. The cage type covalent organic framework material prepared through the method has the advantages of being large in conjugated system, relatively high in chemical stability and thermal stability, largein specific surface area, small in density and larger in number of open loci and also has the advantages that the operation process is simple and feasible, the requirement for equipment in the preparation process is low, the industrial batch production is easy, and the like.

Description

technical field [0001] The invention belongs to the field of preparation of covalent organic framework materials, in particular to a cage-type covalent organic framework prepared by utilizing monomers such as tetrakis(4-anilino)methane with a three-dimensional structure and p-phenylenediamine or p-dibromobenzene material method. Background technique [0002] Compared with traditional inorganic porous materials, covalent organic framework materials are connected by light elements through covalent bonds, and have significant advantages such as high thermal stability, extremely low density, large specific surface area, and good structural tailoring. It has important application value and broad market prospects in the research fields of gas adsorption, photoelectricity, catalysis, sensing, heterogeneous catalysis, energy storage, etc., and has aroused strong research interest in the scientific community. Covalent organic framework materials are classified into two-dimensional c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/00
CPCC08G73/00
Inventor 苗中正
Owner 江苏宏光布业有限公司
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