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Preparation method and application of covalent organic framework compound and open-cage fullerene composite material

A technology of covalent organic framework and composite material, applied in the field of chemical synthesis, can solve problems such as high price, and achieve the effects of simple method, increased conductivity and convenient recycling

Pending Publication Date: 2021-12-10
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the noble metal platinum is the electrochemical hydrogen evolution catalyst with the highest catalytic efficiency and the best effect in the hydrogen production process, but its high price has become the key to limit the platinum catalyst. Electrocatalysts and improving their electrocatalytic performance are urgent tasks for electrocatalytic energy conversion

Method used

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  • Preparation method and application of covalent organic framework compound and open-cage fullerene composite material
  • Preparation method and application of covalent organic framework compound and open-cage fullerene composite material
  • Preparation method and application of covalent organic framework compound and open-cage fullerene composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Embodiment 1 A kind of preparation method of covalent organic framework compound

[0064] This embodiment includes the following steps carried out in sequence:

[0065] S11. Weigh 3.09kg (5mol) of 1,3,6,8-tetrakis(4-formaldehyde phenyl)pyrene and 1.08kg (10mol) of p-phenylenediamine respectively in a container, add o-dichlorobenzene Perform ultrasonication for 30 minutes to assist dissolution to form a homogeneous solution. Add 4.65kg (77.5mol) of acetic acid during the ultrasonication process. After the container is frozen under liquid nitrogen conditions, the container is pumped to remove oxygen, and then the container is degassed. Sealed in the state;

[0066] S12. Heat the sealed container to 250°C at a heating rate of 5°C / h under the condition of 25°C, and react for 48 hours to obtain reactant A;

[0067] S13. The reactant A was washed with acetone, methanol, and dioxane in sequence, then soaked in acetone for 12 hours, and finally vacuum-dried at 80° C. for 12 h...

Embodiment 2-6

[0071] The preparation method of embodiment 2-6 covalent organic framework compound

[0072] Examples 2-6 are respectively a preparation method of a covalent organic framework compound, and their steps are basically the same as in Example 1, the only difference being the amount of raw materials and process parameters, see Table 1 for details:

[0073] List of each technological parameter in the embodiment 2-6 of table 1

[0074]

[0075]

Embodiment 7

[0076] Embodiment 7 A kind of preparation method of open cage fullerene

[0077] This embodiment includes the following steps carried out in sequence:

[0078] S21. Take 3.1kg (10mol) of 3-(2-pyridyl)-5,6-diphenyl-1,2,4-triazine and 3.6kg (5mol) of C60 and dissolve them in 9L of o-dichlorobenzene , heated to reflux at 150°C for 24h, cooled to room temperature, and used CS 2 Carry out silica gel column chromatography directly as the eluent, finally remove unreacted C60, and then use CS 2 Carry out secondary elution with the eluent mixed with ethyl acetate at a volume ratio of 80:1 to obtain reactant B;

[0079] S22. Dissolving 10 g of reactant B in 10 L of CCl 4 In the process, a 150-watt high-pressure mercury lamp was used to irradiate in an oxygen atmosphere for 72 hours, and the solution changed from pink purple to brown; the solution was rotary evaporated, and the residue was subjected to silica gel column chromatography. 2 The solution mixed with ethyl acetate at a vol...

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Abstract

The invention discloses a preparation method of a covalent organic framework compound and open-cage fullerene composite material. The method comprises the following steps of: performing chemical cage opening on fullerene, mixing the fullerene with a covalent organic framework, and performing ultrasonic treatment, stirring, washing, soaking and drying to obtain the covalent organic framework compound and open-cage fullerene composite material. The invention further provides application of the composite material, wherein the composite material can be used as an electrocatalyst for efficient hydrogen evolution, can solve the problem that the cost is too high due to the fact that a traditional electrocatalyst depends on precious metal, improves the catalytic activity of the electrocatalyst, can also be applied to adsorption of carbon dioxide, and has higher nitrogen doping rate and larger specific surface area and pore volume compared with traditional adsorbents, so that the material has better adsorbability, selectivity and repeatability. The method is suitable for preparing the covalent organic framework compound and open-cage fullerene composite material, and the prepared composite material can be further applied to carbon dioxide adsorption and can also be used as an electrocatalyst for efficient hydrogen evolution.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to the preparation of a multifunctional compound, in particular to a preparation method and application of a covalent organic framework compound and open cage fullerene composite material. Background technique [0002] With the rapid development of global industrialization, while fossil resources are developed and consumed in large quantities, serious environmental pollution problems also follow. The scarcity and pollution of global fossil resources have become a topic of urgent concern. Carbon emissions, mitigation of increasingly severe environmental pollution and greenhouse effect, and obtaining high value-added chemicals have become the goals pursued by more and more people. [0003] The covalent organic framework has a stable π-conjugated stable structure and a large specific surface area, and its adsorption capacity can be adjusted by adjusting the pore size, so it ca...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/20B01J20/28B01J20/30B01D53/02C25B1/04C25B11/04C01B32/156
CPCB01J20/226B01J20/20B01J20/28057B01J20/28066B01D53/02C25B1/04C25B11/04C01B32/156B01D2257/504Y02E60/36Y02C20/40Y02P20/151
Inventor 李小云杨静董旭莎乔山林李青苏玉金
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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