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

[0063] Example 1 A method for covalent organic frame compounds

[0064] This embodiment includes the following steps in turn:

[0065] S11. It is proposed for 3.09 kg (5 mol) of 1,3,6,8-tetra (4-formaldehyde-based phenyl) pyrene and 1.08 kg (10 mol) of phenylenediamine, which is placed in a container, and adjacent dichlorobenzene Ultrasound 30min, auxiliary dissolution form a uniform solution, add 4.65 kg (77.5 mol) of acetic acid during ultrasound, and the container is frozen under liquid nitrogen conditions, and the container is removed, and then the container is degassed Seal in the state;

[0066] S12. The sealed container is tapered to 250 ° C at 25 ° C, and the reactant A is heated to 250 ° C, reactive 48 h.

[0067] S13. The reactant A was washed with acetone, methanol, and dioxane, and then immersed with acetone for 12 h, and finally under vacuum drying under 80 ° C for 12 h, a covalent organic frame compound X1 was obtained.

[0068] The scanning electron microscope diagram

[0071] Example 2-6 Preparation method of covalent organic frame compound

[0072] Example 2-6 is a method of covalent organic frame compounds, respectively, and their steps are substantially the same as in Example 1, and different are only different from the amount of raw materials and process parameters. See Table 1 for details.

[0073] Table 1 Example 2-6 List of process parameters in various

[0074]

[0075]

[0076] Example 7 Method for preparing cage fullerene

[0077] This embodiment includes the following steps in turn:

[0078] S21. Take 3.1 kg (10 mol) of 3- (2-pyridyl) -5,6-diphenyl-1,2,4-triazine and 3.6 kg (5 mol) C60, dissolved in 9L neovenstlobenzene After heating at 150 ° C for 24 h, after cooling to room temperature, use CS 2 For eluent, the eluent is directly subjected to silica gel column chromatography, followed by unreacted C60, and then use CS 2 EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc EtOAc

[0079] S22. Dissolve 10 g of reactant B in 10L CCL 4 In the medium, the high-pressure mercury lamp was irradiated in the oxygen atmosphere in the oxygen atmosphere of 72 hours, and the solution was turned brown by powder purple; the solution was centered, and the residue was subjected to silica gel column chromatography. 2 The solution mixed with ethyl acetate was evaporated as the eluent at a volume ratio of 80: 1, and the second brown belt was collected, and the fullerene product was e