CN114988398B - High-heating graphene composite material and preparation method thereof - Google Patents
High-heating graphene composite material and preparation method thereof Download PDFInfo
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- CN114988398B CN114988398B CN202210709554.3A CN202210709554A CN114988398B CN 114988398 B CN114988398 B CN 114988398B CN 202210709554 A CN202210709554 A CN 202210709554A CN 114988398 B CN114988398 B CN 114988398B
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- C01B32/00—Carbon; Compounds thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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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: hydrogen, methane, ferrous sulfate, zinc powder, N-dimethylacetamide, 70% sodium chloride solution, deionized water, clean water and inert gas, wherein the preparation method specifically comprises the following steps: s1: placing the aerosol thin plate 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 iron prepared by the method is more fully compounded with graphene, so that 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
The graphene is a two-dimensional lamellar structure, the thickness of the graphene is only one carbon atom, the surface of the graphene is a hexagonal net structure composed of carbon atoms, the graphene has special physical and chemical properties, the graphene is used as a carbon material, the graphene has good heat transfer capability, heat is generated by mutual friction of carbon atoms in the graphene, the far infrared radiation is also called, the heat is light which can be absorbed by a human body, and aiming at the characteristic, people develop a graphene composite material with self-heating gradually;
as in the prior publication CN109718003 a-a graphene heating composite material and a preparation method thereof, the raw materials of the material are disclosed to comprise: 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 the 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, water-absorbent resin and mineral salt according to a proportion, and stirring and mixing 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 an excellent uniform heating function and excellent physiotherapy performance.
Although the graphene heating composite material in the above publication can improve the heating function, the composite material only changes the functional groups of graphene, and the distribution of iron powder in graphene oxide is not adjusted, so that the iron powder is unevenly distributed in the graphene oxide, and the heating uniformity is low;
accordingly, there is a need for improvements in the art to address the above-described problems.
Disclosure of Invention
The invention aims to provide a high-heating graphene composite material and a preparation method thereof, wherein the high-heating graphene composite material prepared by the preparation method has uniform heating distribution and good heating effect, and solves the problems of uneven heating distribution and poor heating effect of the existing graphene composite material in actual use.
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 is prepared from raw materials including hydrogen, methane, ferrous sulfate, zinc powder, N-dimethylacetamide, 70% sodium chloride solution, deionized water, clear water and inert gas.
Further, the auxiliary material comprises an aerosol thin plate with the thickness of 0.3-1 mm.
Further, 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 thin plate 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 is completed;
s4: preparing graphene-containing water into graphene oxide dissolved in water 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 through an ultrasonic particle vibrator;
s6: adding N, N-dimethylacetamide into the solution, and heating for 20-30 min by auxiliary irradiation of a microwave heater;
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 by deionized water and clear water, and drying by a drying device after cleaning, wherein the drying temperature is 120-150 ℃ and the drying time is 35-50 min, so as to obtain the high-heating graphene composite material.
Further, the ratio of hydrogen to methane in the step S2 is 12-16:23-25, and the pressure of the vacuum container after the hydrogen and methane are blown in is 3-5 atmospheres.
Further, methane may be replaced by other carbon source gases.
Further, the Hummers method of preparing graphene oxide in step S4 may be replaced by a Brodie method and a staudenmailer method.
Further, the mass ratio of the ferrous sulfate, the zinc powder and 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.
Further, the microwave heating in step S6 is under an inert gas atmosphere.
The invention has the following beneficial effects:
when the preparation method is used, the replacement reaction between ferrous sulfate and zinc powder can be used for replacing iron in the ferrous sulfate, and the iron atoms can be uniformly distributed in grid gaps of the graphene oxide by matching with vibration, so that the iron is more uniformly distributed in the graphene, the heating uniformity is improved, and the heat generation can be improved due to the high resistance of the iron atoms, so that the Brownian motion of carbon atoms is improved when current passes, 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 is prepared from raw materials including hydrogen, methane, ferrous sulfate, zinc powder, N-dimethylacetamide, 70% sodium chloride solution, deionized water, clear water and inert gas, and auxiliary materials including an aerosol sheet.
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, wherein the firmness of graphene attachment can be improved due to the characteristic of high pores on the aerosol sheet;
s2: simultaneously blowing hydrogen and methane into a vacuum container, heating for 1.5-2 h 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 in is 3-5 atmospheres, and the hydrogen and the methane are heated in a vacuum environment, so that the methane can be cracked to generate carbon atoms, and the specific preparation method is the prior art, so that redundant description is omitted;
methane may also be replaced by other carbon source gases such as ethane and propane;
s3: immersing the aerosol sheet deposited with 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, wherein the ultrasonic particle oscillator can wash out the graphene on the aerosol sheet on one hand, and is also convenient for separation between graphene layers;
s4: preparing graphene-containing water into graphene oxide dissolved in water by a Hummers method;
the Hummers method for preparing graphene oxide can also be replaced by a Brodie method and a Staudenmailer method, and the three methods are conventional methods for preparing graphene oxide from graphene, so that redundant description is omitted here;
for example, the Hummers method is mainly to add 98% concentrated sulfuric acid and potassium permanganate, and obtain brown oxidized graphene with derivative carboxylic acid groups at the edge and phenolic hydroxyl groups and epoxy groups on the plane after the graphene is subjected to oxidation reaction;
in addition, the graphene oxide dissolved in water means that after the preparation of graphene oxide is completed, the graphene oxide is diluted by adding clean water after purification, impurity removal (removing excessive potassium permanganate), PH adjustment (neutral adjustment) and the like;
s5: adding ferrous sulfate into the aqueous solution containing graphene oxide, stirring uniformly, adding zinc powder, and continuously vibrating for 20-30 min through an ultrasonic particle vibration machine, wherein iron in the ferrous sulfate can be replaced through a replacement reaction, and the problem of replacing potassium is avoided because the activity of zinc is greater than that of iron and lower than that of potassium;
the vibration of the ultrasonic particle vibration machine can avoid the excessive combination of iron atoms in the graphene grid and external iron atoms, so that a large amount of iron is attached to the graphene;
s6: adding N, N-dimethylacetamide into the solution, and heating for 20-30 min by auxiliary irradiation of a microwave heater, wherein the microwave heating is in an inert gas environment, and the arrangement can reduce graphene oxide into graphene;
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 by a filtering device, collecting solids, adding 70% sodium chloride solution into the solids, immersing the solids in the solution, extracting suspended matters, wherein the density of the 70% sodium chloride solution is higher than that of water, so that the iron-containing graphene can be suspended, and iron particles are precipitated due to the high density, so that the separation of iron and the iron-containing graphene is realized;
s8: and cleaning the suspended matters sequentially through deionized water and clear water, wherein the deionized water can remove ions on the suspended matters, 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.
The foregoing is only a preferred embodiment of the present invention, and the present invention is not limited thereto, and any modification, equivalent replacement, and improvement of some of the technical features described in the foregoing embodiments are all within the scope of the present invention.
Claims (4)
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, clear water and inert gas;
the adopted raw materials also comprise 98% concentrated sulfuric acid and potassium permanganate;
the auxiliary materials adopted comprise aerosol thin plates;
the raw materials are used for preparing the high-heating graphene composite material according to the following method, and specifically comprise the following steps:
s1: placing the aerosol thin plate 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 is completed;
s4: preparing graphene-containing water into graphene oxide dissolved in water 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 through an ultrasonic particle vibrator;
s6: adding N, N-dimethylacetamide into the solution, and heating for 20-30 min by auxiliary irradiation of a microwave heater;
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 by deionized water and clear water, and drying by a drying device after cleaning, wherein the drying temperature is 120-150 ℃ and the drying time is 35-50 min, so as to obtain the high-heating graphene composite material.
2. The high heat generating graphene composite material according to claim 1, wherein: 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 atmospheres.
3. The high heat generating graphene composite material according to claim 2, wherein: 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.
4. A high heat generating graphene composite material according to claim 3, wherein: the microwave heating in step S6 is under an inert gas atmosphere.
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