Solvent and method suitable for liquid-phase intercalation stripping of lamellar graphite material

Abstract

The invention relates to a solvent suitable for liquid-phase intercalation stripping of a lamellar graphite material. The solvent is characterized in that the solvent comprises a fluorine-chlorine-carbon compound, and the fluorine-chlorine-carbon compound comprises tetrafluoromonochloroethane and tetrafluoroethane with boiling points both lower than -10 DEG C; the fluorine-chlorine-carbon compoundis colorless gas at atmospheric pressure, and is in a mixed state of saturated liquid and saturated gas in a closed container at a temperature above a boiling point; and under the condition that process temperature ranges from 10 DEG C to 50 DEG C s and corresponding pressure in the closed container ranges from 0.23 MPa to 1.32 MPa, a material state can be converted between a liquid phase and a gas phase along with the changes of the temperature and the pressure and is in a stable state. The fluorine-chlorine-carbon compound comprises a single solvent, and also comprises a solution componentformed by mixing and dissolving substances according to any proportion. The fluorine-chlorine-carbon compound is non-toxic, non-flammable, low in solvent viscosity, good in permeability in a liquid phase state and good in diffusivity in a gas phase state, and especially under the condition that an auxiliary working medium applies high equilibrium pressure, liquid phase solvent molecules can permeate into interlamellar gaps of lamellar graphite.

Description

technical field

[0001] The invention relates to the field of manufacturing nano-powder materials with lamellar structure characteristics, in particular to a solvent and method suitable for liquid-phase intercalation and exfoliation of lamellar graphite materials. Background technique

[0002] Graphene is the thinnest nanomaterial known so far, and it has physical and chemical properties beyond existing materials in many aspects. The single-layer graphene with a two-dimensional crystal structure has a thickness of about 0.34 nanometers and a theoretical specific surface area of ​​2630m 2 / g, meanwhile, has excellent electrical, thermal, force and magnetic properties.

[0003] Powdered graphene is an excellent filler for the preparation of various composite materials, and has a wide range of uses in the fields of microelectronics, new energy, and new materials.

[0004] Lamellar graphite, as a mineral material formed by geological mineralization, is essentially composed of c...

Examples

Embodiment 1

[0045] Raw materials: natural flake graphite with a particle size of 0.1-0.5 mm

[0046] Intercalation solvent Ⅰ: Tetrafluorochloroethane (R-124a), solvent parameters:

[0047]

[0048] Auxiliary working fluid: nitrogen (N 2 )

[0049] as attached figure 2 As shown, put the raw materials into a closed container, vacuumize, the working gauge pressure is -0.06MPa, and remove the non-condensable gas inside the container;

[0050] Add the intercalation solvent I to a closed container at a ratio of 20 times the graphite mass, and mix naturally for 5 minutes at a process temperature of 10°C and a working gauge pressure of 0.23MPa;

[0051] Inject N into the mixture 2 For gas, boost the pressure of the solvent mixture to 5MPa working gauge pressure;

[0052] Driven by the high-pressure pump body, the mixed liquid enters at a high pressure of 12MPa (this pressure is the outlet pressure of the high-pressure pump.) Figure 4 In the four-stage "Rafal nozzle" connected in series...

Embodiment 2

[0059] Raw materials: natural flake graphite with a particle size of 0.1-0.5 mm

[0060] Intercalation solvent Ⅱ: tetrafluoroethane (R134a), solvent parameters:

[0061]

[0062] Auxiliary working fluid: CO 2

[0063] as attached figure 2 As shown, put the raw materials into a closed container, vacuumize, the working gauge pressure is -0.08MPa, and remove the gas inside the container;

[0064] Add the solvent R134a to the airtight container at a ratio of 50 times the mass of graphite, and mix naturally for 20 minutes at a process temperature of 50°C and a working gauge pressure of 1.32MPa (at 50°C, the absolute pressure of R134a gas is 1.32MPa);

[0065] Inject CO into the mixture 2 For gas, boost the pressure of the solvent mixture to the working gauge pressure of 10MPa;

[0066] Driven by the high-pressure pump body, the mixed liquid enters the Figure 4 In the series-connected five-stage "Rafal nozzle" as shown, after the process of "compression-diffusion and inst...

Embodiment 3

[0073] Raw materials: natural graphite with a particle size of 0.1 to 0.5 mm

[0074] Intercalation solvent: select the mixture of R124a and R134a, the volume ratio is about 1:1, and prepare it as a liquid phase intercalation solvent Ⅲ, the solvent parameter range:

[0075]

[0076] Auxiliary working fluid: CO 2 gas

[0077] as attached figure 2 As shown, put the raw materials into the airtight container, evacuate, the working gauge pressure is -0.08MPa, and remove the gas inside the container;

[0078]Add the liquid phase intercalation solvent III to the airtight container at a ratio of 40 times the mass of graphite, and mix naturally for 20 minutes under the conditions of process temperature 25°C and working gauge pressure 0.9MPa;

[0079] Inject CO into the mixture 2 For gas, pressurize the solvent mixture to a working gauge pressure of 8MPa;

[0080] Driven by the mechanical pump body, the mixed liquid enters such as Figure 4 In the multi-stage series "Rafal noz...

technical field

[0001] The invention relates to the field of manufacturing nano-powder materials with lamellar structure characteristics, in particular to a solvent and method suitable for liquid-phase intercalation and exfoliation of lamellar graphite materials. Background technique

[0002] Graphene is the thinnest nanomaterial known so far, and it has physical and chemical properties beyond existing materials in many aspects. The single-layer graphene with a two-dimensional crystal structure has a thickness of about 0.34 nanometers and a theoretical specific surface area of ​​2630m 2 / g, meanwhile, has excellent electrical, thermal, force and magnetic properties.

[0003] Powdered graphene is an excellent filler for the preparation of various composite materials, and has a wide range of uses in the fields of microelectronics, new energy, and new materials.

[0004] Lamellar graphite, as a mineral material formed by geological mineralization, is essentially composed of c...

Examples

Embodiment 1

[0045] Raw materials: natural flake graphite with a particle size of 0.1-0.5 mm

[0046] Intercalation solvent Ⅰ: Tetrafluorochloroethane (R-124a), solvent parameters:

[0047]

[0048] Auxiliary working fluid: nitrogen (N 2 )

[0049] as attached figure 2 As shown, put the raw materials into a closed container, vacuumize, the working gauge pressure is -0.06MPa, and remove the non-condensable gas inside the container;

[0050] Add the intercalation solvent I to a closed container at a ratio of 20 times the graphite mass, and mix naturally for 5 minutes at a process temperature of 10°C and a working gauge pressure of 0.23MPa;

[0051] Inject N into the mixture 2 For gas, boost the pressure of the solvent mixture to 5MPa working gauge pressure;

[0052] Driven by the high-pressure pump body, the mixed liquid enters at a high pressure of 12MPa (this pressure is the outlet pressure of the high-pressure pump.) Figure 4 In the four-stage "Rafal nozzle" connected in series...

Embodiment 2

[0059] Raw materials: natural flake graphite with a particle size of 0.1-0.5 mm

[0060] Intercalation solvent Ⅱ: tetrafluoroethane (R134a), solvent parameters:

[0061]

[0062] Auxiliary working fluid: CO 2

[0063] as attached figure 2 As shown, put the raw materials into a closed container, vacuumize, the working gauge pressure is -0.08MPa, and remove the gas inside the container;

[0064] Add the solvent R134a to the airtight container at a ratio of 50 times the mass of graphite, and mix naturally for 20 minutes at a process temperature of 50°C and a working gauge pressure of 1.32MPa (at 50°C, the absolute pressure of R134a gas is 1.32MPa);

[0065] Inject CO into the mixture 2 For gas, boost the pressure of the solvent mixture to the working gauge pressure of 10MPa;

[0066] Driven by the high-pressure pump body, the mixed liquid enters the Figure 4 In the series-connected five-stage "Rafal nozzle" as shown, after the process of "compression-diffusion and inst...

Embodiment 3

[0073] Raw materials: natural graphite with a particle size of 0.1 to 0.5 mm

[0074] Intercalation solvent: select the mixture of R124a and R134a, the volume ratio is about 1:1, and prepare it as a liquid phase intercalation solvent Ⅲ, the solvent parameter range:

[0075]

[0076] Auxiliary working fluid: CO 2 gas

[0077] as attached figure 2 As shown, put the raw materials into the airtight container, evacuate, the working gauge pressure is -0.08MPa, and remove the gas inside the container;

[0078]Add the liquid phase intercalation solvent III to the airtight container at a ratio of 40 times the mass of graphite, and mix naturally for 20 minutes under the conditions of process temperature 25°C and working gauge pressure 0.9MPa;

[0079] Inject CO into the mixture 2 For gas, pressurize the solvent mixture to a working gauge pressure of 8MPa;

[0080] Driven by the mechanical pump body, the mixed liquid enters such as Figure 4 In the multi-stage series "Rafal noz...

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