CN110790265A - Inlaying method of potassium ion graphene - Google Patents
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- CN110790265A CN110790265A CN201911070708.3A CN201911070708A CN110790265A CN 110790265 A CN110790265 A CN 110790265A CN 201911070708 A CN201911070708 A CN 201911070708A CN 110790265 A CN110790265 A CN 110790265A
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- C01B32/00—Carbon; Compounds thereof
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Abstract
The invention discloses a method for inlaying potassium ion graphene, which comprises the steps of respectively placing natural crystalline flake graphite powder and a potassium material into two different molybdenum boat vessels, and placing the two different molybdenum boat vessels into a vacuum reaction kettle for vacuumizing; heating the temperature in the vacuum reaction kettle by adopting a high-frequency heating method to ensure that potassium ions in the potassium material are sublimated to the natural crystalline flake graphite powder to form potassium ion graphite powder; and after the potassium ion graphite powder is cooled, adding the potassium ion graphite powder into base oil to strip the oil phase graphene, so as to obtain the oil phase graphene embedded with potassium ions. The scheme is that potassium ions are sublimated to natural flake graphite powder, and the natural flake graphite powder is permeated like a coating film. And after the infiltration is finished, the oil phase graphene stripping process is carried out, so that the graphene inlaid with potassium ions is obtained. The potassium ion graphene is added into engine oil, so that a lubricating effect can be achieved, and the effects of cooling an engine and saving oil can be achieved.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a method for inlaying potassium ion graphene.
Background
A potassium ion graphene mosaic method is mainly characterized in that the research and development group members also engage in the research and development of the application of finding more functional characteristics on functional graphene made by ion mosaic to carry out scientific and technological research on the development of the future graphene industry. Such as in a cathode application of a battery, or an anode application, and the like. It is understood that the functional direction … on graphene of different properties may also be for catalytic reactions and the like as a corresponding material purpose. The potassium ion graphene mosaic method is also one of important links in graphene application science and technology in the future, and certainly, the functional application coordination is developed from the perspective of environmental protection and no pollution on the basis of battery application.
Disclosure of Invention
Aiming at the defects in the technology, the invention provides the potassium ion graphene inlaying method which is low in cost and convenient to operate.
In order to achieve the above purpose, the invention provides a method for inlaying potassium ion graphene, comprising the following steps:
respectively putting natural crystalline flake graphite powder and a potassium material into two different molybdenum boat utensils, and putting the boat utensils into a vacuum reaction kettle for vacuumizing;
heating the temperature in the vacuum reaction kettle by adopting a high-frequency heating method to ensure that potassium ions in the potassium material are sublimated to the natural crystalline flake graphite powder to form potassium ion graphite powder;
and after the potassium ion graphite powder is cooled, carrying out water-phase graphene stripping on the potassium ion graphite powder to obtain the potassium ion graphene.
The method for stripping the aqueous graphene from the potassium ion graphite powder comprises the following steps:
mixing the potassium ion graphite powder, the layer removing agent and the sugar;
stirring for 3-5 h to ensure that the delamination agent is fully mixed between the graphite layers of the potassium ion graphite powder to form a water phase mixture;
adding a chelating impacting agent into the water phase mixture, and uniformly stirring to form a water phase reactant;
and standing the water-phase reactant for 1-1.5h to form the potassium ion graphene.
Wherein, the vacuum-pumping of vacuum reaction kettle is two to five negative atmospheric pressures, and the mixed mass ratio of potassium material and crystalline flake graphene is potassium material: crystalline flake graphene is 1:10-3: 10.
The natural crystalline flake graphite powder is 200-3000 meshes in size, and the potassium material is one or more of potassium carbonate and potassium hydroxide.
Wherein the sugar is sucrose, and the addition amount of the sucrose is 0.1-10% of the potassium ion graphite powder by mass fraction.
The delamination agent is one or more of potassium bicarbonate, ammonium bicarbonate, potassium peroxide and ammonium peroxide, and the addition amount of the delamination agent accounts for 10-20% of the potassium ion graphite powder by mass fraction.
The chelating impact agent is one or more of EDTA, PTDA, PDTA and HEDTA, and the addition amount of the chelating impact agent is 10-20% of the potassium ion graphite powder by mass fraction.
The invention relates to the use of the potassium ion graphene intercalation method according to claims 1-7, and the potassium ion graphene produced by the method is used in chemical batteries as anodes of aluminum oxygen batteries.
The invention has the beneficial effects that:
compared with the prior art, the scheme is that potassium ions are sublimated to natural flake graphite powder as a coating film to permeate. And after the permeation is finished, the water-phase graphene stripping process is carried out, so that the graphene inlaid with potassium ions is obtained. The potassium ion graphene serving as the functional graphene can serve as an anode sheet of the chemical battery, plays a role in catalyzing the reaction of the anode and the cathode, can reduce the use of solution type conductive liquid, and enhances the safety and the practicability of the chemical battery.
Drawings
Fig. 1 is a schematic flow chart of a method for inlaying potassium ion graphene according to the present invention;
FIG. 2 is a schematic flow chart of a method for water-phase stripping of potassium ion graphite powder.
Detailed Description
In order to more clearly describe the present invention, the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 1, the method for inlaying potassium ion graphene of the present invention includes the following steps:
step S100, raw material preparation:
respectively putting natural crystalline flake graphite powder and a potassium material into two different molybdenum boat utensils, and putting the boat utensils into a vacuum reaction kettle for vacuumizing; the vacuumizing of the vacuum reaction kettle is negative two to negative five atmospheric pressures, and the mixing mass ratio of the potassium material to the crystalline flake graphene is that of the potassium material: flake graphene is 1:10-3: 10; the natural crystalline flake graphite powder is 200-3000 meshes in size, and the potassium material is one or more of potassium carbonate and potassium hydroxide.
Step S200, high-temperature sublimation of potassium ions:
heating the temperature in the vacuum reaction kettle by adopting a high-frequency heating method to ensure that potassium ions in the potassium material are sublimated to the natural crystalline flake graphite powder to form potassium ion graphite powder;
step S300, graphene water phase stripping:
and after the potassium ion graphite powder is cooled, carrying out water-phase graphene stripping on the potassium ion graphite powder to obtain the potassium ion graphene.
The natural crystalline flake graphite powder is processed, potassium ions are sublimated to enter the crystalline flake graphite by vacuum heating. By imitating the vacuum coating principle, potassium ions are plated on the crystalline flake graphite, and functional graphene with potassium ion characteristics is produced by a water graphene slurry production method. Can be conveniently used for exerting effects on battery application in the future, including some catalytic applications.
Referring to fig. 2, the method for peeling off the aqueous graphene from the potassium ion graphite powder includes the following steps:
s310, mixing the potassium ion graphite powder, the layer removing agent and the sugar; the sugar is sucrose, and the addition amount of the sucrose is calculated by mass fraction and accounts for 0.1-10% of the potassium ion graphite powder. The delamination agent is one or more of potassium bicarbonate, ammonium bicarbonate, potassium peroxide and ammonium peroxide, and the addition amount of the delamination agent is 10-20% of the potassium ion graphite powder by mass fraction.
S320, stirring for 3-5 hours to ensure that the delamination agent is fully mixed between graphite layers of the potassium ion graphite powder to form a water phase mixture;
the delaminators are necessary, however, in the present application, the delaminators are of two general types. Namely the acidity and alkalinity, but our development direction is in the graphene development field. The method is developed in an environment-friendly direction to achieve the purpose of zero emission. Therefore, the research and development of the delamination agent are based on food grade and environmental protection, which is a technical position for the industrialization and mass production of graphene.
Firstly, the formula of the layer-splitting agent is applied, and materials in the aspects of strong acid and strong alkali are not used as main materials. In the industry, … is treated with strong acid and strong alkali and needs to be treated in an environment-friendly way, and the sequelae of pollution are most feared. And the prepared graphene is strict in environmental protection and zero emission requirements by developing a delaminating agent applied to flake graphite. For many years we have developed delaminators from food grade materials.
On food grade delaminators we were exempted from the use of sodium ion compound materials. Of course, sodium chloride is a salt, but we do not use compounds with sodium ions. For this reason, during the manufacture of graphene, especially when processed in the aqueous phase. The sodium ions are used, and cannot be discharged, because the compounds with the sodium ions on land and land can not be applied to plant irrigation. Since sodium ions reverse plant growth, even those in many countries indicate that human and animal excreta cannot be used as fertilizer … because of the relationship with sodium ions. So we use a split layer of food grade material based on compounds free of sodium ions, typically based on potassium-based and amine-based compounds.
S330, adding a chelating impacting agent into the water-phase mixture, and uniformly stirring to form a water-phase reactant; the chelating impact agent is one or more of EDTA, PTDA, PDTA and HEDTA, and the addition amount of the chelating impact agent is 10-20% of the potassium ion graphite powder by mass fraction.
S340, standing and reacting the water-phase reactant for 1-1.5h to form the potassium ion graphene.
The invention relates to the use of the potassium ion graphene intercalation method according to claims 1-7, and the potassium ion graphene produced by the method is used in chemical batteries as anodes of aluminum oxygen batteries.
After the sugar with the proportion is added, the wetting speed and the penetration are increased by seven to eight times compared with the original speed. The ability to penetrate and wet the delaminator is typically accomplished in three hours, and power and time savings … is an effective method for large volume production applications. The substance of sugar has a molecular structure of poly-poly and polysaccharide chains, is very effective in water-soluble wetting of natural flake graphite powder, is matched with a plurality of complex mode delaminating agents, such as a polycarbonate chelate, a peroxide compound and the like, and can be well wetted and matched even with an embedded ion metal and the like in the delaminating agents. In experiments, we found that natural flake graphite powder is easily combined with a delaminating agent in water. And the graphite powder wetting preparation is carried out without long-time stirring required in the prior treatment wetting. The time required for the preparation of the reagent from the previous reaction is generally at best after 24 hours, depending also on the climate. The reason is that the mixed delamination agent is on the crystalline flake graphite, and because air exists between the crystalline flake graphite, negative pressure is added to pump out air to allow the delamination agent to permeate in the mixture. The combination of a novel delaminating agent formulation and a sugar is applied herein, which allows the production of graphene in a very short time. In the experimental process, the preparation liquid is prepared by adding the delaminating agent and water into the scale graphite powder and mixing the mixture, and finally the impact agent is added, so that the graphene can be produced within five hours on average. According to the graphite lamination needs, can shorten the manufacturing time, added the sugar on tearing the layering agent, can accelerate the osmosis and need not the evacuation and handle, let graphite infiltration tear the layering agent open, do not influenced by the air and carry out the preparation agent and go to strike and produce graphite alkene.
Example one
The invention discloses a method for inlaying potassium ion graphene, which comprises the following steps:
1) respectively putting 100g of natural crystalline flake graphite powder and 10g of potassium material into two different molybdenum boat vessels, putting the two different molybdenum boat vessels into a vacuum reaction kettle, and vacuumizing to reach negative two atmospheric pressures to negative five atmospheric pressures;
2) heating the temperature in the vacuum reaction kettle to 900-1100 ℃ by adopting a high-frequency heating method, so that potassium ions in the potassium material are sublimated to the natural crystalline flake graphite powder to form potassium ion graphite powder;
3) after the potassium ion graphite powder is cooled, mixing the potassium ion graphite powder, 11g of potassium bicarbonate and 0.11g of sugar;
4) stirring for 3-5 h to ensure that the delamination agent is fully mixed between the graphite layers of the potassium ion graphite powder to form a water phase mixture;
5) adding 11g of EDTA and PTDA into the aqueous phase mixture, and uniformly stirring to form an aqueous phase reactant;
6) and standing the water-phase reactant for 1-1.5h to form the potassium ion graphene.
The potassium ion graphene serving as the functional graphene can be used as a positive and negative electrode reaction catalyst of the chemical battery, so that the use of solution type conductive liquid can be reduced, and the safety and the practicability of the chemical battery are enhanced.
Example two
The invention discloses a method for inlaying potassium ion graphene, which comprises the following steps:
1) respectively putting 100g of natural crystalline flake graphite powder and 30g of potassium material into two different molybdenum boat vessels, and putting the two different molybdenum boat vessels into a vacuum reaction kettle for vacuumizing to reach negative two atmospheric pressures to negative five atmospheric pressures;
2) heating the temperature in the vacuum reaction kettle to 900-1100 ℃ by adopting a high-frequency heating method, so that potassium ions in the potassium material are sublimated to the natural crystalline flake graphite powder to form potassium ion graphite powder;
3) after the potassium ion graphite powder is cooled, mixing the potassium ion graphite powder, 26g of potassium bicarbonate and 13g of sugar;
4) stirring for 3-5 h to ensure that the delamination agent is fully mixed between the graphite layers of the potassium ion graphite powder to form a water phase mixture;
5) adding 26g of EDTA and PTDA into the aqueous phase mixture, and uniformly stirring to form an aqueous phase reactant;
6) and standing the water-phase reactant for 1-1.5h to form the potassium ion graphene.
The above disclosure is only for a few specific embodiments of the present invention, but the present invention is not limited thereto, and any variations that can be made by those skilled in the art are intended to fall within the scope of the present invention.
Claims (8)
1. A potassium ion graphene inlaying method is characterized by comprising the following steps:
respectively putting natural crystalline flake graphite powder and a potassium material into two different molybdenum boat utensils, and putting the boat utensils into a vacuum reaction kettle for vacuumizing;
heating the temperature in the vacuum reaction kettle by adopting a high-frequency heating method to ensure that potassium ions in the potassium material are sublimated to the natural crystalline flake graphite powder to form potassium ion graphite powder;
and after the potassium ion graphite powder is cooled, carrying out water-phase graphene stripping on the potassium ion graphite powder to obtain the potassium ion graphene.
2. The method for inlaying potassium ion graphene according to claim 1, wherein the method for performing aqueous phase graphene exfoliation on the potassium ion graphite powder comprises the following steps:
mixing the potassium ion graphite powder, the layer removing agent and the sugar;
stirring for 3-5 h to ensure that the delamination agent is fully mixed between the graphite layers of the potassium ion graphite powder to form a water phase mixture;
adding a chelating impacting agent into the water phase mixture, and uniformly stirring to form a water phase reactant;
and standing the water-phase reactant for 1-1.5h to form the potassium ion graphene.
3. The method for inlaying potassium ion graphene according to claim 1, wherein the vacuum pumping of the vacuum reaction kettle is negative two to negative five atmospheric pressures, and the mixing mass ratio of the potassium material to the crystalline flake graphene is that of the potassium material: crystalline flake graphene is 1:10-3: 10.
4. The method for inlaying potassium ion graphene according to claim 1, wherein the natural crystalline flake graphite powder has a size of 200-3000 mesh, and the potassium material is one or more of potassium carbonate and potassium hydroxide.
5. The method for inlaying potassium ion graphene according to claim 2, wherein the sugar is sucrose, and the addition amount of the sucrose is 0.1-10% of the potassium ion graphite powder by mass fraction.
6. The method for inlaying potassium ion graphene according to claim 2, wherein the delaminating agent is one or more of potassium bicarbonate, ammonium bicarbonate, potassium peroxide and ammonium peroxide, and the delaminating agent is added in an amount of 10-20% of the potassium ion graphite powder by mass fraction.
7. The method for inlaying potassium ion graphene according to claim 2, wherein the chelating impacting agent is one or more of EDTA, PTDA, PDTA and HEDTA, and the addition amount of the chelating impacting agent is 10-20% of the potassium ion graphite powder by mass fraction.
8. Use of the potassium ion graphene mosaic method according to claims 1-7, wherein the potassium ion graphene produced by the method is used in an electrochemical cell as an anode for an aluminum oxygen cell.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815694A (en) * | 2012-03-13 | 2012-12-12 | 华东理工大学 | Graphene preparation method, and graphene prepared through using method |
| US20150353361A1 (en) * | 2013-03-06 | 2015-12-10 | Sekisui Chemical Co., Ltd. | Method for producing random-structure gic, method for producing exfoliated graphite dispersion liquid, exfoliated graphite dispersion liquid, and exfoliated graphite |
| CN106044763A (en) * | 2016-08-08 | 2016-10-26 | 华侨大学 | Method for preparing graphene powder at room temperature |
| CN110127677A (en) * | 2019-05-05 | 2019-08-16 | 陈让珠 | Water body graphene slurry production method |
-
2019
- 2019-11-05 CN CN201911070708.3A patent/CN110790265A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815694A (en) * | 2012-03-13 | 2012-12-12 | 华东理工大学 | Graphene preparation method, and graphene prepared through using method |
| US20150353361A1 (en) * | 2013-03-06 | 2015-12-10 | Sekisui Chemical Co., Ltd. | Method for producing random-structure gic, method for producing exfoliated graphite dispersion liquid, exfoliated graphite dispersion liquid, and exfoliated graphite |
| CN106044763A (en) * | 2016-08-08 | 2016-10-26 | 华侨大学 | Method for preparing graphene powder at room temperature |
| CN110127677A (en) * | 2019-05-05 | 2019-08-16 | 陈让珠 | Water body graphene slurry production method |
Non-Patent Citations (1)
| Title |
|---|
| WEI WEI ET AL.: "Applications of 3D Potassium-Ion Pre-Intercalated Graphene for Perovskite and Dye-Sensitized Solar Cells", 《IND. ENG. CHEM. RES.》 * |
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