CN110980723B - Graphite puffing treatment process - Google Patents
Graphite puffing treatment process Download PDFInfo
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- CN110980723B CN110980723B CN201911376950.3A CN201911376950A CN110980723B CN 110980723 B CN110980723 B CN 110980723B CN 201911376950 A CN201911376950 A CN 201911376950A CN 110980723 B CN110980723 B CN 110980723B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/22—Intercalation
- C01B32/225—Expansion; Exfoliation
Abstract
The invention relates to a graphite swelling treatment process, in particular to a process for dipping graphite in a certain vacuum environment by using alkane organic matters as swelling agents at a certain temperature and under a certain pressure, then contacting water vapor with the graphite dipped with alkane to swell the graphite, and then purging and replacing residual swelling agents by using inert gas to obtain dry graphite. Compared with the prior art, the method has the advantages of low puffing temperature, simple operation, recyclable puffing agent, low production cost and large-scale production.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a graphite puffing treatment process.
Background
The expanded graphite is prepared by oxidizing and intercalating natural crystalline flake graphite, inserting compound between graphite flake layers, heating and vaporizing the compound at high temperature, generating great tension on the graphite flake layers by the generated gas, and expanding the graphite into vermicular expanded graphite.
The expanded graphite has the excellent performances of high electric and heat conductivity, high and low temperature resistance, corrosion resistance and the like of natural graphite, and also has the characteristics of compressibility, resilience, large specific surface area, good adsorbability and the like which are not possessed by the natural graphite, so that the expanded graphite is widely used as a sealing material, an environment-friendly adsorption material, a fireproof flame-retardant material, a biomedical material and the like.
The common processes for graphite expansion include chemical oxidation, electrochemical process, ultrasonic radiation, explosion, gas phase diffusion, etc. The chemical oxidation method is that under a certain temperature, the flake graphite is oxidized by an oxidant, the interlayer structure is destroyed, an intercalator is inserted between the flake graphite layers, and then the expanded graphite is prepared by auxiliary procedures of washing, drying and the like. The method has the advantages of high reaction speed, low equipment cost, good expansion effect of the prepared expanded graphite and wide industrial application. However, a large amount of acid and strong oxidant are used in the reaction, some chemical factors are difficult to control, peroxidation may be caused, the yield is reduced, the reaction speed is not easy to regulate, and the structure and the performance of the expanded graphite product are difficult to accurately control. The electrochemical method is characterized in that direct current or pulse current is utilized, concentrated sulfuric acid is used as electrolyte, the flake graphite is placed in an electrolytic cell to form an anode chamber with an auxiliary anode, and after a period of oxidation reaction, washing and drying are carried out to obtain the expanded graphite, wherein the expansion mode is the same as that of the chemical oxidation method. The electrochemical method has the advantages that electrode parameters and reaction time can be regulated, so that the reaction degree and the performance of the expanded graphite product are controlled, and the automation degree is higher; the electrolyte can be recycled; the dosage of the oxidant is greatly reduced compared with the chemical method. But has the disadvantages of large electricity consumption, easy peroxidation and inferior product stability to the chemical oxidation method. The ultrasonic radiation method is characterized in that in the graphite oxidation process, the reactants are oscillated by utilizing the ultrasonic radiation effect to dissociate graphite sheets, so that the intercalation agent can enter the graphite layers more easily. The expandable graphite prepared by the ultrasonic radiation method has a wide expansion temperature range, can be expanded at a low temperature and has a stable structure. But the process conditions, throughput and scale are limited.
CN201210009109.2 introduces a process method for preparing graphene oxide by microwave puffing, which adopts microwave puffing. CN201420636320.1 also provides a microwave device for preparing graphene material by traveling wave irradiation, and the puffing treatment of graphite is performed in a manner of arranging materials on a microwave transmission path. CN201821624182.X discloses a high-temperature furnace device for expanded graphite, which has the technical scheme that the device comprises a discharge barrel, wherein one end of the discharge barrel is fixedly provided with a feed pipe connected with a discharge port of the high-temperature furnace, the top of the high-temperature furnace is fixedly provided with a material pumping pipe, and the material pumping pipe is provided with a fan; the feed cylinder has set firmly vertical spiral branch flitch in, this utility model provides a graphite directly is taken away after high temperature furnace heating is popped, thoughtlessly has the problem of the graphite of sintering in the graphite after the popped, and discharge gate department through at high temperature furnace is provided with discharging device, reaches the graphite separation's after will popped graphite that thoughtlessly has sintering in the graphite after with the popped effect. CN201621489711.0 describes an electric-steam mixed heating graphite high-temperature expansion furnace.
In the patent of the graphite expansion processing method, the low-temperature expansion is generally carried out by adopting microwave expansion, the intercalation oxidation expansion method is generally carried out by adopting a high-temperature muffle furnace, the oxidation is carried out at 800-1000 ℃, compounds among graphite layers are rapidly decomposed or vaporized by a surface heat conduction mode at high temperature, a large amount of gas is generated, the graphite is stripped along the C-axis direction to form expanded graphite, the expansion mode is long in time, and the electric energy consumption is large.
Disclosure of Invention
Aiming at the technical problems in the graphite puffing treatment process, the invention introduces a novel graphite puffing method, which comprises the steps of impregnating a micromolecule organic solvent under pressure, allowing the micromolecule organic solvent to enter the graphite, and oxidizing and replacing the micromolecule organic solvent by using hot steam at a certain temperature and under a certain steam pressure to achieve a puffing effect.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme, which comprises the following steps:
(1) Putting graphite into the puffing chamber, and sealing the cover plate;
(2) Pumping out air in the puffing chamber to make the puffing chamber in a vacuum state with the pressure below-0.08 MPa;
(3) Selecting alkane organic matter as a swelling agent, spraying alkane steam into the swelling chamber, controlling the temperature of the alkane steam at 70-120 ℃ and the pressure in the swelling chamber at 0.1-1MPa, and keeping the alkane steam impregnated graphite for more than 30 min;
(4) After the alkane steam is fully impregnated into the graphite, keeping the temperature in the puffing chamber constant, discharging redundant alkane steam, collecting and converting the redundant alkane steam into liquid for storage and standby application, wherein the pressure change is realized under the constant temperature condition;
(5) After alkane steam is discharged, spraying water steam into the puffing chamber to expand the graphite impregnated with the alkane, controlling the water steam pressure in the puffing chamber to be 0.1-0.6MPa, and stopping water steam feeding when the temperature of the puffing chamber rises to 120 ℃ after the expansion stage is considered to be completed;
(6) Discharging condensate and swelling agent in the swelling chamber, and separating and recovering;
(7) Vacuumizing the puffing chamber to the pressure below-0.08 MPa, purging and replacing residual puffing agent and water vapor in the puffing chamber by using inert gas, and drying the puffed graphite;
(8) And opening the puffing chamber after the puffing chamber is naturally cooled to normal temperature (25 ℃), releasing the pressure to normal pressure (0 MPa), and taking out the graphite to detect the puffing effect.
The graphite variety in the invention is preferably crystalline flake graphite, and can also be natural graphite, asphalt, microcrystalline graphite and the like.
The object of the invention is further achieved by the following technical measures.
In the graphite puffing treatment process, before the graphite is puffed, the particles can be milled, the particle size of the graphite is required to be 30-1500 meshes, and is preferably 500-800 meshes, and then the puffing treatment is carried out.
In the graphite puffing treatment process, the pressure in the puffing chamber is reduced to be lower than-0.08 MPa, and the air in the puffing chamber is pumped out so as to prevent the air from influencing the impregnation of the graphite by alkane steam when the air exists. It is preferable to depressurize to full vacuum if possible.
In the graphite puffing treatment process, the alkane used in the graphite puffing treatment process is n-pentane, isopentane and the like.
In the graphite puffing treatment process, alkane steam must be completely gasified when being introduced into the puffing chamber, and attention is paid to avoid liquid alkane entering. Since alkane is a highly volatile and flammable solvent, the process design for disposal and recovery must be rigorous. The temperature of the alkane steam entering the puffing chamber is controlled within the range of 70-120 ℃. Alkane vapors above 120 c can impair the subsequent steam expansion treatment. Conversely, if the temperature is below 70 ℃, liquid alkane enters the expansion chamber. The alkane steam entering the puffing chamber at low temperature can be liquefied by cooling the container, the energy of the system can be taken away during evaporation in the presence of liquid alkane, and the liquid alkane is required in an increased amount, so that the recovery process is increased.
In the graphite puffing treatment process, the pressure range of the puffing chamber after the alkane steam is introduced is 0.1-1MPa, and preferably 0.4-0.6MPa. When the pressure value of the alkane steam in the puffing chamber reaches 0.4MPa, the temperature of the alkane steam can be continuously increased, and the pressure in the puffing chamber can be continuously increased to about 0.5MPa. At a pressure of at least 0.4MPa, the graphite is always kept in contact with alkane steam for at least 30min, the graphite is impregnated by the alkane, and the alkane in the graphite is extruded into a liquid phase under pressure.
In the graphite puffing treatment process, after the soaking is finished, the pressure in the puffing chamber is released to the normal pressure (0 MPa) as soon as possible, and the redundant alkane steam escapes from the puffing chamber and enters a recovery container for storage and standby. The temperature of the puffing chamber is kept constant in the pressure relief process, so that the phenomenon of alkane temperature reduction and liquefaction is avoided, and the pressure relief is completed within 15-20 min.
In the graphite puffing treatment process, after pressure is released, water vapor is introduced into the puffing chamber immediately, so that the temperature of the puffing chamber is quickly raised to be higher than 100 ℃, liquid alkane immersed in graphite is gasified, the volume is quickly increased and escaped, and the graphite is promoted to expand. Electron microscopy revealed that the treatment resulted in an increase in graphite interlayer spacing and an increase in graphite volume. The pressure of the puffing chamber is controlled at 0.1-0.6MPa, preferably 0.2-0.3MPa after water vapor is introduced into the puffing chamber. The operation must be carefully carried out when the water vapor is introduced for pressurization, so that the graphite turbulence in the expansion chamber is avoided, and the expansion of the graphite is not favorable. When the puffing chamber temperature rises to 120 ℃, the puffing stage is considered to be completed, and the steam supply is stopped. The time from the introduction of the water vapor until the temperature of 120 ℃ is reached is preferably not more than 2min, at most not more than 4min. In the graphite puffing treatment process, after the steam puffing stage is finished, the puffing chamber is vacuumized, purged with inert gas for replacement drying, and pumped out for drying for about 0.5h. And opening the puffing chamber after the puffing chamber is naturally cooled to normal temperature, relieving pressure to normal pressure, and taking out the expanded graphite to detect the effect.
By means of the technical scheme, the invention provides a brand-new graphite expansion treatment process, which comprises the steps of impregnating graphite with alkane in a certain vacuum environment, and then contacting water vapor with the graphite impregnated with alkane to expand the graphite. Compared with the prior art, the method has the advantages of low puffing temperature, simple operation, recyclable puffing agent, low production cost and large-scale production.
The above description is only an overview of the technical solutions of the present invention, and in order to make the purpose and technical solutions of the present invention more clear, the following embodiments will further describe the present invention in detail with reference to the accompanying drawings.
Drawings
FIG. 1 is a schematic view of the experimental apparatus for expanding graphite according to the present invention.
[ reference numerals ]
1-steam generator 2-swelling agent evaporator 3-swelling chamber
4-swelling agent recovery tank 5-condenser 6-cooling water pump
7 cooling water tank 8-mixed liquid recovery tank 9-vacuum pump
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments.
Referring to fig. 1, the present invention provides a graphite swelling treatment process, including impregnating graphite with alkane in a certain vacuum environment, and swelling the graphite by contacting water vapor with the graphite impregnated with alkane, and the specific operation steps are as follows:
(1) The test apparatus was installed, debugged with reference to fig. 1;
(2) Selecting crystalline flake graphite with the particle size of 600 meshes, weighing, putting the crystalline flake graphite into a puffing chamber, sealing a cover plate, and connecting a pipeline;
(3) Pumping out air in the puffing chamber by using a vacuum pump to ensure that the puffing chamber is vacuum and the pressure is below-0.08 MPa;
(4) Selecting isopentane as a swelling agent, spraying isopentane steam at 90 ℃ into the swelling chamber through a swelling agent evaporator, and keeping the pressure in the swelling chamber to be not lower than 0.4MPa for more than 30 min;
(5) After the isopentane steam is fully impregnated with graphite, keeping the temperature in the puffing chamber constant, discharging redundant isopentane steam from the puffing chamber, and converting the residual isopentane steam into liquid isopentane through a condenser for storage and standby;
(6) After all the free isopentane steam is discharged, spraying water vapor into the puffing chamber to increase the pressure of the puffing chamber to 0.14MPa, and stopping spraying the water vapor when the temperature of the puffing chamber reaches 120 ℃;
(7) Discharging condensate and swelling agent in the swelling chamber, and separating and recovering;
(8) Finally, vacuumizing the expansion chamber to the pressure below-0.08 MPa, purging and replacing residual expanding agent and water vapor in the expansion chamber by using inert gas, and drying the expanded graphite;
(9) And taking out the expanded graphite, and detecting the volume change. And (4) opening the puffing chamber after the puffing chamber is naturally cooled to normal temperature, relieving pressure to normal pressure, taking out the puffed graphite, and detecting the volume change.
The normal temperature in this experiment was 25 ℃ and the normal pressure was 0MPa.
The experimental data of 3 examples carried out according to the above procedure are shown in the following table:
table 1: examples of graphite expansion
| Graphite | Example 1 | Example 2 | Example 3 |
| Volume before treatment (ml) | 50.4 | 47.4 | 46.7 |
| Volume after treatment (ml) | 332.3 | 323.5 | 317.3 |
| Pressure of treatment chamber after completion of impregnation (MPa) | 0.49 | 0.48 | 0.49 |
| Temperature (. Degree.C.) of steam discharged from the puffing completion treatment chamber | 105 | 104 | 104 |
The experimental data of the three examples show that the graphite swelling treatment process can expand the volume of graphite to 6-7 times of the original volume, the graphite swelling effect is obvious, and the swelling agent can be recycled, so that the production cost is reduced.
The above description is only a preferred embodiment of the present invention, and any person skilled in the art can make any simple modification, equivalent change and modification to the above embodiments according to the technical essence of the present invention without departing from the scope of the present invention, and still fall within the scope of the present invention.
Claims (7)
1. A graphite bulking treatment process is characterized in that the process comprises the following steps of impregnating graphite with a small molecular organic solvent under pressure, allowing the impregnated graphite to enter the graphite, and oxidizing and replacing the impregnated graphite with hot steam at a certain temperature and under steam pressure to achieve a bulking effect:
(1) Putting graphite into a puffing chamber, and sealing a cover plate;
(2) Pumping out air in the puffing chamber to make the puffing chamber in a vacuum state with the pressure below-0.08 MPa;
(3) Selecting isopentane organic matter as a swelling agent, spraying alkane steam into a swelling chamber, controlling the temperature of the alkane steam to be 70-120 ℃ and the pressure in the swelling chamber to be 0.1-1MPa, and keeping the alkane steam impregnated graphite for more than 30 min;
(4) After the isopentane steam is fully impregnated with graphite, keeping the temperature in the puffing chamber constant, discharging redundant alkane steam, collecting and converting the alkane steam into liquid for storage and standby application, wherein the pressure change is realized under the constant temperature condition;
(5) After the isopentane steam is discharged, spraying steam into the puffing chamber to expand the graphite impregnated with isopentane, controlling the pressure of the steam in the puffing chamber to be 0.1-0.6MPa, when the temperature of the puffing chamber rises to 120 ℃, namely the puffing stage is finished, stopping feeding the steam, and controlling the time for the temperature of the puffing chamber to reach 120 ℃ to be within 4 min;
(6) Discharging condensate and swelling agent in the swelling chamber, and separating and recovering;
(7) Vacuumizing the puffing chamber to the pressure below-0.08 MPa, purging and replacing residual puffing agent and water vapor in the puffing chamber by using inert gas, and drying the puffed graphite;
(8) And opening the puffing chamber after the puffing chamber is naturally cooled to normal temperature, relieving pressure to normal pressure, and taking out the graphite to detect the expansion effect.
2. The process of claim 1, wherein the graphite is flake graphite or microcrystalline graphite.
3. The process of claim 1, wherein the graphite has a particle size of 30-1500 mesh.
4. The process of claim 1, wherein the pressure of the puffing chamber is maintained at 0.4-0.6MPa after the alkane stream is introduced into the puffing chamber.
5. The graphite puffing treatment process of claim 1, wherein the pressure in the puffing chamber is controlled to be 0.2-0.3MPa after the water vapor is introduced.
6. The graphite puffing treatment process of claim 1, wherein the time for the puffing chamber to reach 120 ℃ after water vapor is introduced cannot exceed 2min.
7. The process of claim 1, wherein the inert gas used for the displacement drying of the expansion chamber is nitrogen or helium.
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