Preparation method of oxidized graphite fluoride

A technology of fluorinated graphite and fluorine oxide, applied in the direction of graphite, etc., can solve the problems of fluorinated graphite, such as large size, complicated process, poor thermal stability, etc., and achieve the effect of improved stability, simple process and easy realization

Active Publication Date: 2014-10-01
SHENZHEN NANKE NEW MATERIALS TECH CO LTD
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Problems solved by technology

The graphene oxide and N 2 and F 2 Under the conditions of the reaction temperature of 20-200°C and the reaction time of 0.5-24h, the mixed gas composed of the composition can obtain graphite containing partial oxidized groups and fluorine atoms similar to oxidized functionalized fluorinated graphite, which does not have fluorinated graphite. The basic structural characteristics and related properties of graphite, and due to the large energy between fluorine-carbon bonds and high stability, lead to the following shortcomings: 1) When the degree of fluorine substitution for oxygen is low, the fluorine content is small, and the material properties are closer to graphite oxide, and Poor thermal stability; 2) When the degree of fluorine substitution is high, the electronegativity of fluorine is extremely high, and the high content of fluorine makes it impossible to ensure the existence of remaining oxidized groups, and the fluorination reaction is violent, the reaction environment is dangerous and the process is complicated
[0008] So far, the existing technology has been unable to solve the problem of fluorinated graphite being dispersed in oily and aqueous media due to its large size and hydrophobic and oleophobic surface.

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  • Preparation method of oxidized graphite fluoride
  • Preparation method of oxidized graphite fluoride
  • Preparation method of oxidized graphite fluoride

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[0053] The invention provides a method for preparing surface functionalized oxidized graphite fluoride, the main steps of which are as follows:

[0054] 1) reflux pretreatment of fluorinated graphite raw materials;

[0055] 2) ultrasonic treatment is carried out to described graphite fluoride solution;

[0056] 3) suction filtration and drying of the graphite fluoride solution to obtain graphite fluoride with exposed carbon atoms on the edge of the preliminary intermediate;

[0057] 4) Oxidative modification of graphite fluoride with exposed carbon atoms at the edge;

[0058] 5) Suction filtration and drying to obtain the final product graphite fluoride oxide.

[0059] In step 1), the commercial fluorinated graphite is placed in a specific reagent to reflux, and the specific reagent is isopropanol (IPA) or tetrahydrofuran (THF); reflux process parameters: temperature 90°C, time 1-10h.

[0060] In step 2), the fluorinated graphite solution in step 1) is irradiated with power...

Embodiment 1

[0066] 10g graphite fluoride [ Picture 1-1 , Figure 1-2 , Figure 5-1 】Reflux in 300ml isopropanol at 90°C for 1 hour; irradiate with ultrasound at a frequency of 40kHz, output power 1.5KW, duty ratio 1:0.5, and power for 8 hours to obtain a fluorinated graphite solution with reduced size and exposed carbon atoms at the edge; Suction filtration and drying to obtain fluorinated graphite with exposed carbon atoms on the edge; oxidation by the improved Hummers method, adding 5g of sodium nitrate and 230g of concentrated sulfuric acid and mixing evenly, stirring slowly and adding 45g of KMnO 4 , kept at 0°C for 4h, moved to a water bath at 35°C for 30 minutes, gradually added 460ml of deionized water, and continued to react for 3h after the temperature rose to 98°C, diluted with water, and diluted with 30wt% H 2 o 2 Solution neutralization treatment (unreacted KMnO 4 ), fully washed with deionized water at 40°C, and dried in vacuum at 60°C for 48 hours to obtain "graphite flu...

Embodiment 2

[0071] 1g graphite fluoride 【 Picture 1-1 , Figure 1-2 , Figure 5-1 】Put in 100ml tetrahydrofuran and reflux at 90°C for 2h; irradiate ultrasonically at a frequency of 20kHz, output power 1KW, duty ratio 1:2, and power for 6h to obtain a fluorinated graphite solution with reduced size and exposed carbon atoms at the edge; suction filtration, Dry to obtain fluorinated graphite with exposed carbon atoms on the edge; oxidize using the improved Hummers method, add 0.5g sodium nitrate, 23g concentrated sulfuric acid and mix well, stir and slowly add 9g KMnO 4 , kept at 0°C for 2h, moved to a 35°C water bath for 30 minutes, gradually added 46ml of deionized water, and continued to react for 2h after the temperature rose to 98°C, diluted with water, and used 30wt% H 2 o 2 Solution neutralization treatment (unreacted KMnO 4 ), fully washed with deionized water at 40°C, and dried in vacuum at 50°C for 48 hours to obtain "graphite fluoride oxide [ Figure 2-2 , Figure 3-3 , F...

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Abstract

The invention relates to a preparation method of oxidized graphite fluoride and belongs to the technical field of functionalization of materials. The preparation method comprises the following steps: 1) carrying out backflow pre-treatment on a graphite fluoride raw material; 2) carrying out ultrasonic treatment on a graphite fluoride solution; 3) carrying out suction filtering and drying on the graphite fluoride solution to obtain an initial intermedium graphite fluoride with carbon atoms naked at the edge; 4) carrying out oxidization modification on the graphite fluoride with carbon atoms naked at the edge; 5) carrying out suction filtering and drying to obtain the final product oxidized graphite fluoride. The oxidized graphite fluoride with surface functionalization provided by the invention has a grain size smaller than that of the raw material and fewer layers, and has few stably existing oxidizing groups (-COOH, -OH and -O-) on the surface and at the edge, so that oleophylic, hydrophilic and amphiphilic functionalized oxidized graphite fluoride modified in different manners is obtained so as to adapt to different dispersing systems.

Description

technical field [0001] The invention relates to a preparation method of oxidized fluorinated graphite, which belongs to the technical field of material functionalization. Background technique [0002] Graphite fluoride (graphite fluoride) is a newly emerging carbon material. Its quality is unique and it is a wonderful flower in the family of functional materials. Graphite fluoride has excellent lubricity, and its lubricity is better than that of graphite and molybdenum disulfide. When the temperature is 400-500 degrees Celsius in a dry or humid environment, the friction coefficient is smaller and the service life is longer. Graphite fluoride has excellent lubricating properties, adding it to lubricating oil can significantly improve the lubricating effect. Fluorinated graphite has low surface energy (about one-third of polytetrafluoroethylene), and because fluorine atoms enter the graphite layer and form a covalent bond with the large π bond of the graphite layer, resultin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/00C01B32/20
Inventor 张至张柏华张大伏张小伏
Owner SHENZHEN NANKE NEW MATERIALS TECH CO LTD
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