Fluorinated fullerene and preparation method and application thereof
A technology for fluorinated fullerenes and fluorinated fullerenes, applied in the field of fluorinated fullerenes and their preparation, can solve the problems of poor dispersibility, easy agglomeration of fullerenes, etc., and achieves difficult agglomeration, simple and controllable methods, and good Effects of Compatibility and Dispersion
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[0022] Fluorine atom is the ninth element in the periodic table and has the strongest electronegativity, so that fluorine-containing organic compounds exhibit a series of unique physical and chemical properties. Modification of fluorine atoms on fullerenes can increase the inertness of fullerene molecules, making it more difficult for fluorides of fullerenes to react with other substances, so that they have better dispersibility and can become good raw materials for preparing lubricants. In view of this, an embodiment of the present invention provides a method for preparing fluorinated fullerenes, comprising the following steps:
[0023] S01. Provide reaction raw material fullerene and fluorine-containing precursor;
[0024] S02. After the fullerene and the fluorine-containing precursor are mixed and processed, a solid-phase heating reaction is carried out in a vacuum or an inert environment; wherein, the solid-phase heating reaction is realized by a gradient heating method, a...
Embodiment 1
[0048] S11. Provide 50mg C 60 with 350mg MnF 3 ;
[0049] S12. Put C 60 with MnF 3 After uniform grinding, put into a quartz tube (length: 30cm, diameter: 1.2cm), vacuumize the quartz tube (about 0.1Pa); put the quartz tube into the tube furnace, place the end of the reactant in the heating zone of the furnace In the center, a part of the quartz tube is outside the heating zone. The furnace temperature is set to: rise to 100°C within 10 minutes and maintain for 30 minutes, and rise to 500°C within 30 minutes and maintain for 2 hours; after cooling, the quartz tube is taken out and the product is collected.
[0050] The mixed product was separated and purified by HPLC to obtain 8 mg of fluorinated fullerene. Among them, MnF 3 The diagram of the fluorination reaction device is shown in figure 1 As shown, the liquid chromatographic analysis diagram of the product obtained by solid phase heating is shown in figure 2 shown.
Embodiment 2
[0052] S21. Provides 30mg C 60 with 300mg CF 3 COOAg;
[0053] S22. Put C 60 with CF 3 After COOAg is evenly ground, put it into a quartz tube (length: 30cm, diameter: 1cm), vacuumize the quartz tube (about 0.1Pa); put the quartz tube into the tube furnace, and place the end of the reactant in the heating zone of the furnace In the center, a part of the quartz tube is outside the heating zone. The furnace temperature is set as follows: gradually heat to 100°C and maintain for 30 minutes; raise the temperature to 300°C and maintain for 2 hours; after cooling, take out the quartz tube and collect the product.
[0054] The mixed product was separated and purified by HPLC to obtain 5 mg of fluorinated fullerene.
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