CN114988398A - High-heating graphene composite material and preparation method thereof - Google Patents
High-heating graphene composite material and preparation method thereof Download PDFInfo
- Publication number
- CN114988398A CN114988398A CN202210709554.3A CN202210709554A CN114988398A CN 114988398 A CN114988398 A CN 114988398A CN 202210709554 A CN202210709554 A CN 202210709554A CN 114988398 A CN114988398 A CN 114988398A
- Authority
- CN
- China
- Prior art keywords
- graphene
- composite material
- heating
- preparation
- graphene composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/12—Metallic powder containing non-metallic particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- 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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a high-heating graphene composite material and a preparation method thereof, and relates to the technical field of heating composite materials and preparation. The composite material comprises the following raw materials: the preparation method comprises the following steps of: s1: placing the aerosol sheet in a vacuum container, and vacuumizing the vacuum container; s2: simultaneously blowing hydrogen and methane into a vacuum container, and heating at 800-950 ℃ for 1.5-2 h to obtain an aerosol sheet deposited with graphene; s3: immersing the aerosol sheet deposited with the graphene in water, oscillating for 30-45 min by an ultrasonic particle oscillator, washing out the graphene in the aerosol, and taking out the aerosol sheet after cleaning. The composite material prepared by the invention has more sufficient composition of iron and graphene, so that the heating is more uniform, and the overall heating efficiency is high.
Description
Technical Field
The invention belongs to the technical field of heating composite materials and preparation, and particularly relates to a high-heating graphene composite material and a preparation method thereof.
Background
Graphene is a two-dimensional lamellar structure, the thickness of the graphene is only one carbon atom thick, the surface of the graphene is a hexagonal reticular structure consisting of the carbon atoms, the graphene has special physical and chemical properties, the graphene is used as a carbon material and has good heat transfer capacity, the carbon atoms in the graphene generate heat when being mutually rubbed, the heat is also called far infrared radiation, the heat is light rays which can be absorbed by a human body, and people gradually develop a graphene composite material with self-heating aiming at the characteristic;
as disclosed in the prior publication CN 109718003A-a graphene exothermic composite material and a preparation method thereof, the material comprises the following raw materials: 90-95% of iron powder, 0.01-5% of modified graphene oxide material, 0.1-3% of water-absorbent resin and 0.1-5% of mineral salt. The preparation method of the material comprises the following steps: step 1, weighing raw materials in proportion; step 2, preparing modified graphene oxide powder; step 3, carrying out modified grafting on the modified graphene oxide powder and iron powder through ultrasonic stirring; and 4, mixing the modified graphene oxide and iron powder composite material with the water-absorbent resin and the mineral salt according to the proportion, and stirring and mixing the mixture by using a high-speed rotary pot to prepare the graphene heating composite material. According to the invention, the iron powder is modified by the graphene oxide, so that the heating material prepared from the modified graphene oxide and iron powder composite material has excellent uniform heating function and excellent physical therapy performance.
Although the graphene heating composite material in the above publication can improve the heating function, the above composite material only changes the functional group of graphene, and the distribution of the iron powder in the graphene oxide is not adjusted, which results in the uneven distribution of the iron powder in the graphene oxide, and thus the heating uniformity is low;
therefore, there is a need for improvement of the prior art to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a high-heating graphene composite material and a preparation method thereof.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a high-heating graphene composite material which adopts the raw materials of hydrogen, methane, ferrous sulfate, zinc powder, N-dimethylacetamide, 70% sodium chloride solution, deionized water, clean water and inert gas.
Furthermore, the adopted auxiliary materials comprise aerosol thin plates, and the thickness of the aerosol thin plates is 0.3-1 mm.
Furthermore, the adopted raw materials also comprise 98% concentrated sulfuric acid and potassium permanganate.
The invention also provides a preparation method of the high-heating graphene composite material, which comprises the following steps:
s1: placing the aerosol sheet in a vacuum container, and vacuumizing the vacuum container;
s2: simultaneously blowing hydrogen and methane into a vacuum container, and heating at 800-950 ℃ for 1.5-2 h to obtain an aerosol sheet deposited with graphene;
s3: immersing the aerosol sheet deposited with the graphene in water, vibrating for 30-45 min by an ultrasonic particle vibrator, washing out the graphene in the aerosol, and taking out the aerosol sheet after cleaning;
s4: preparing water containing graphene into water-soluble graphene oxide by a Hummers method;
s5: adding ferrous sulfate into the aqueous solution containing graphene oxide, uniformly stirring, adding zinc powder, and continuously vibrating for 20-30 min by using an ultrasonic particle shaker;
s6: adding N, N-dimethylacetamide into the solution, and heating for 20-30 min by microwave heater-assisted irradiation;
s7: filtering the solution by a filtering device, collecting solids, adding 70% sodium chloride solution into the solids, immersing the solids in the solution, and extracting suspended matters;
s8: and cleaning the suspended matters sequentially through deionized water and clear water, and drying the suspended matters through a drying device after cleaning, wherein the drying temperature is 120-150 ℃, and the drying time is 35-50 min, so that the high-heating graphene composite material is obtained.
Further, the ratio of the hydrogen to the methane in the step S2 is 12-16: 23-25, and the pressure of the vacuum container after the hydrogen and the methane are blown in is 3-5 atm.
Further, methane may also be replaced by other carbon source gases.
Further, the Hummers method in step S4 may be substituted for the preparation of graphene oxide by the Brodie method and the staudenmaeer method.
Further, the mass ratio of the ferrous sulfate to the zinc powder to the N, N-dimethylacetamide in the steps S5-S6 is 1: 1-1.2: 0.1-0.13, and 30-38 g of ferrous sulfate is added to each 500ml of graphene oxide aqueous solution.
Further, the microwave heating in step S6 is under an inert gas atmosphere.
The invention has the following beneficial effects:
during preparation, iron in ferrous sulfate can be replaced by replacement reaction between ferrous sulfate and zinc powder, and the replacement reaction is matched with vibration, so that iron atoms can be uniformly distributed in grid gaps of graphene oxide, the iron is more uniformly distributed in the graphene, the heating uniformity is improved, and due to the high resistance of the iron atoms, the heat generation can be improved when current passes through, the Brownian motion of carbon atoms is improved, and the composite material has the characteristic of high heating.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below.
The invention relates to a high-heating graphene composite material which comprises the raw materials of hydrogen, methane, ferrous sulfate, zinc powder, N-dimethylacetamide, 70% sodium chloride solution, deionized water, clear water and inert gas, and the auxiliary materials comprise aerosol sheets.
The invention also provides a preparation method of the high-heating graphene composite material, which comprises the following steps:
s1: the aerosol thin plate is placed in a vacuum container, and the vacuum container is vacuumized, so that the firmness of graphene attachment can be improved due to the characteristic of high porosity of the aerosol thin plate;
s2: simultaneously blowing hydrogen and methane into a vacuum container, heating for 1.5-2 hours at 800-950 ℃ to obtain an aerosol sheet deposited with graphene, wherein the ratio of the hydrogen to the methane is 12-16: 23-25, the pressure of the vacuum container after the hydrogen and the methane are blown into the vacuum container is 3-5 atmospheric pressures, and the hydrogen and the methane are heated in a vacuum environment to realize the cracking of the methane and generate carbon atoms;
methane can also be replaced by other carbon source gases, such as ethane and propane;
s3: immersing the aerosol sheet deposited with the graphene in water, and oscillating for 30-45 min by an ultrasonic particle oscillator to wash out the graphene in the aerosol, and taking out the aerosol sheet after cleaning is finished, wherein the ultrasonic particle oscillator can wash out the graphene on the aerosol sheet and is convenient for separation between graphene layers;
s4: preparing water containing graphene into water-soluble graphene oxide by a Hummers method;
the preparation of graphene oxide by the Hummers method can be replaced by a Brodie method and a Staudenmaeer method, and the three methods are conventional methods for preparing graphene oxide by graphene, so that redundant description is not provided herein;
for example, the Hummers method mainly comprises the steps of adding 98% concentrated sulfuric acid and potassium permanganate, and carrying out oxidation reaction on graphene to obtain brown graphene oxide with derived carboxylic acid groups on the edges and mainly phenolic hydroxyl groups and epoxy groups on the plane;
in addition, the graphene oxide dissolved in water means that after the preparation of the graphene oxide is completed, the graphene oxide is diluted by adding clear water after purification, impurity removal (removing redundant potassium permanganate), PH adjustment (adjustment to be neutral) and the like;
s5: adding ferrous sulfate into an aqueous solution containing graphene oxide, uniformly stirring, adding zinc powder, and continuously vibrating for 20-30 min by using an ultrasonic particle oscillator, wherein iron in the ferrous sulfate can be replaced by a replacement reaction due to the fact that the activity of zinc is greater than that of iron and lower than that of potassium, so that the problem of replacing potassium is solved;
the vibration of the ultrasonic particle vibrator can avoid excessive combination of iron atoms in the graphene grid and external iron atoms to cause the adhesion of a large amount of iron on the graphene;
s6: adding N, N-dimethylacetamide into the solution, and heating for 20-30 min by microwave heater assisted irradiation, wherein the graphene oxide can be reduced to graphene by the arrangement under the inert gas environment of microwave heating, and the specific preparation method is the prior art, so that the detailed description is omitted, and the heating in the inert gas is carried out to avoid partial oxidation of the graphene due to heating;
the mass ratio of the ferrous sulfate to the zinc powder to the N, N-dimethylacetamide is 1: 1-1.2: 0.1-0.13, and 30-38 g of ferrous sulfate is added into every 500ml of graphene oxide aqueous solution;
s7: filtering the solution through a filtering device, collecting solids, adding 70% of sodium chloride solution into the solids, immersing the solids in the solution, extracting suspended matters, wherein the density of the 70% of sodium chloride solution is greater than that of water, so that iron-containing graphene can be suspended, and iron particles are precipitated due to high density, so that iron and iron-containing graphene can be separated;
s8: the suspended substance is sequentially washed by deionized water and clear water, the deionized water can remove ions on the suspended substance, and the suspended substance is dried by a drying device after washing, wherein the drying temperature is 120-150 ℃, and the drying time is 35-50 min, so that the high-heating graphene composite material is obtained.
The present invention is not limited to the above embodiments, and any modifications, equivalent substitutions and improvements of some technical features, which are made to the technical solutions described in the above embodiments, are all within the scope of the present invention.
Claims (9)
1. The high-heating graphene composite material is characterized in that the adopted raw materials comprise hydrogen, methane, ferrous sulfate, zinc powder, N-dimethylacetamide, 70% sodium chloride solution, deionized water, clean water and inert gas.
2. The high-emissivity graphene composite material of claim 1, wherein: the auxiliary material used comprises an aerosol sheet.
3. The high-emissivity graphene composite material of claim 2, wherein: the adopted raw materials also comprise 98 percent of concentrated sulfuric acid and potassium permanganate.
4. The preparation method of the high-heating graphene composite material according to claim 3, which is characterized by comprising the following steps:
s1: placing the aerosol sheet in a vacuum container, and vacuumizing the vacuum container;
s2: simultaneously blowing hydrogen and methane into the vacuum container, and heating at 800-950 ℃ for 1.5-2 h to obtain an aerosol sheet deposited with graphene;
s3: immersing the aerosol sheet deposited with the graphene in water, vibrating for 30-45 min by an ultrasonic particle vibrator, washing out the graphene in the aerosol, and taking out the aerosol sheet after cleaning;
s4: preparing water containing graphene into water-soluble graphene oxide by a Hummers method;
s5: adding ferrous sulfate into the aqueous solution containing graphene oxide, uniformly stirring, adding zinc powder, and continuously vibrating for 20-30 min by using an ultrasonic particle shaker;
s6: adding N, N-dimethylacetamide into the solution, and heating for 20-30 min by microwave heater auxiliary irradiation;
s7: filtering the solution by a filtering device, collecting solids, adding 70% sodium chloride solution into the solids, immersing the solids in the solution, and extracting suspended matters;
s8: and cleaning the suspended matters sequentially through deionized water and clear water, and drying the suspended matters through a drying device after cleaning, wherein the drying temperature is 120-150 ℃, and the drying time is 35-50 min, so that the high-heating graphene composite material is obtained.
5. The preparation method of the high-heat-generation graphene composite material according to claim 4, characterized by comprising the following steps: the ratio of the hydrogen to the methane in the step S2 is 12-16: 23-25, and the pressure of the vacuum container after the hydrogen and the methane are blown in is 3-5 atmospheric pressures.
6. The preparation method of the high-heat-generation graphene composite material according to claim 5, characterized by comprising the following steps: the methane may also be replaced by other carbon source gases.
7. The preparation method of the high-emissivity graphene composite material according to any one of claims 4 to 6, wherein the preparation method comprises the following steps: the Hummers method in step S4 may be used instead of the method of preparing graphene oxide by the Brodie method and the Staudenmaier method.
8. The preparation method of the high-heat-generation graphene composite material according to claim 7, characterized by comprising the following steps: the mass ratio of the ferrous sulfate to the zinc powder to the N, N-dimethylacetamide in the steps S5-S6 is 1: 1-1.2: 0.1-0.13, and 30-38 g of ferrous sulfate is added into every 500ml of graphene oxide aqueous solution.
9. The preparation method of the high-heat-generation graphene composite material according to claim 8, characterized by comprising the following steps: the microwave heating in step S6 is under an inert gas atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210709554.3A CN114988398B (en) | 2022-06-21 | 2022-06-21 | High-heating graphene composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210709554.3A CN114988398B (en) | 2022-06-21 | 2022-06-21 | High-heating graphene composite material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114988398A true CN114988398A (en) | 2022-09-02 |
| CN114988398B CN114988398B (en) | 2023-08-04 |
Family
ID=83036590
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210709554.3A Active CN114988398B (en) | 2022-06-21 | 2022-06-21 | High-heating graphene composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114988398B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923686A (en) * | 2011-08-09 | 2013-02-13 | 海洋王照明科技股份有限公司 | Graphene/carbon nanotube composite material preparation method |
| CN105037762A (en) * | 2015-07-17 | 2015-11-11 | 南京邮电大学 | Preparation method of graphene oxide polyetheramine composite film with high mechanical property |
| KR20180128611A (en) * | 2017-05-24 | 2018-12-04 | 대주전자재료 주식회사 | Graphene-Carbon Nanotube Composites and Manufacturing Method Thereof |
| CN109161715A (en) * | 2018-09-03 | 2019-01-08 | 大同新成新材料股份有限公司 | A kind of metallic graphite carbon alkene composite material and preparation method and preparation facilities |
| CN110127678A (en) * | 2019-05-20 | 2019-08-16 | 天津市职业大学 | A kind of preparation method of magnetic graphene |
| CN111996066A (en) * | 2020-07-14 | 2020-11-27 | 南宁职业技术学院 | Preparation method of cutting fluid for metal processing |
| CN113828317A (en) * | 2021-09-26 | 2021-12-24 | 大连大学 | Method for preparing metal monoatomic-graphene composite material |
-
2022
- 2022-06-21 CN CN202210709554.3A patent/CN114988398B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923686A (en) * | 2011-08-09 | 2013-02-13 | 海洋王照明科技股份有限公司 | Graphene/carbon nanotube composite material preparation method |
| CN105037762A (en) * | 2015-07-17 | 2015-11-11 | 南京邮电大学 | Preparation method of graphene oxide polyetheramine composite film with high mechanical property |
| KR20180128611A (en) * | 2017-05-24 | 2018-12-04 | 대주전자재료 주식회사 | Graphene-Carbon Nanotube Composites and Manufacturing Method Thereof |
| CN109161715A (en) * | 2018-09-03 | 2019-01-08 | 大同新成新材料股份有限公司 | A kind of metallic graphite carbon alkene composite material and preparation method and preparation facilities |
| CN110127678A (en) * | 2019-05-20 | 2019-08-16 | 天津市职业大学 | A kind of preparation method of magnetic graphene |
| CN111996066A (en) * | 2020-07-14 | 2020-11-27 | 南宁职业技术学院 | Preparation method of cutting fluid for metal processing |
| CN113828317A (en) * | 2021-09-26 | 2021-12-24 | 大连大学 | Method for preparing metal monoatomic-graphene composite material |
Non-Patent Citations (5)
| Title |
|---|
| LI YOUJIANG;ET AL.: "Enhanced Microwave Absorption Property of Fe Nanoparticles Encapsulated within Reduced Graphene Oxide with Different Thicknesses", vol. 56, no. 31, pages 8872 - 8879 * |
| ZHAN YANHU;ET AL.: "Fabrication of a flexible electromagnetic interference shielding Fe3O4@ reduced graphene oxide/natural rubber composite with segregated network", vol. 344, pages 184 - 193, XP085384310, DOI: 10.1016/j.cej.2018.03.085 * |
| 张海军: "铁基纳米氧化物及复合材料制备与气敏性能研究", pages 020 - 102 * |
| 段沙沙: "金属/金属氧化物-还原氧化石墨烯复合材料的制备、表征及性能研究", pages 020 - 169 * |
| 王剑: "粉体石墨烯对金属基复合材料微观结构和性能的影响", pages 020 - 11 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114988398B (en) | 2023-08-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105088749B (en) | A kind of graphene/cotton compliant conductive fabric and preparation method thereof | |
| CN106881466B (en) | The preparation method of rare earth modified grapheme enhancing metal-based compound bar | |
| CN107628628B (en) | Graphene modified inorganic material, preparation method and application | |
| CN108899521A (en) | Utilize waste silicon powder and the compound method for preparing ion cathode material lithium of carbon | |
| CN105336912A (en) | Method for enhancing lithium ion battery current collector and active material adhesion | |
| CN110433849B (en) | Graphene oxide quantum dot/oxygen-doped porous carbon nitride/graphene oxide ternary aerogel photocatalyst | |
| CN114988398B (en) | High-heating graphene composite material and preparation method thereof | |
| CN104377037B (en) | A kind of preparation method of the graphene thick-film electrode with high adhesion force | |
| CN109763321A (en) | A kind of conductive graphene/silver Composite aramid fiber tow and preparation method thereof | |
| CN111392712B (en) | Nitrogen modified mesoporous carbon material, preparation method thereof and application of nitrogen modified mesoporous carbon material as electro-adsorption desalination electrode material | |
| CN113402725A (en) | Preparation method and application of heteropoly acid modified metal organic framework compound | |
| CN110270312B (en) | Metal organic framework material-activated carbon composite fiber membrane and preparation method thereof | |
| CN109926024B (en) | Preparation method and application of magnetic organic modified nano adsorption material | |
| CN106268719A (en) | A kind of modified activated carbon preparation method loading ferroferric oxide particle | |
| CN105032352B (en) | A kind of method of one pot process magnetic 3D graphene composite adsorbing materials | |
| Guo et al. | Graphene/carbon composite nanofibers for NO oxidation at room temperature | |
| CN109231186B (en) | Preparation method for inducing graphene three-dimensional network by using metal ions | |
| CN109264785A (en) | A kind of Lacking oxygen WO3-XThe fast preparation method of powder body material | |
| CN115050586A (en) | MXene nanosheet-aspergillus niger carbonized carbon composite material and preparation method and application thereof | |
| CN112366316B (en) | Preparation method and application of nitrogen and phosphorus co-doped graphene | |
| CN107244877A (en) | A kind of bimetallic oxide silicon carbide fibre multi-scale reinforcing body enhancing aluminum phosphate ceramic base structural wave-absorbing material and preparation method thereof | |
| CN107325648A (en) | A kind of preparation method of graphene heat conducting film | |
| CN113903859A (en) | Method for preparing perovskite layer by dry method and perovskite type solar device | |
| CN106006628B (en) | A kind of method that high-current pulsed electron beam prepares Nano diamond | |
| CN111705357A (en) | ABS plastic surface coating deplating process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |