CN111422867A - Aerosol and preparation method thereof - Google Patents
Aerosol and preparation method thereof Download PDFInfo
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- CN111422867A CN111422867A CN201910020599.8A CN201910020599A CN111422867A CN 111422867 A CN111422867 A CN 111422867A CN 201910020599 A CN201910020599 A CN 201910020599A CN 111422867 A CN111422867 A CN 111422867A
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- carbon aerogel
- aerosol
- aerogel
- catalyst
- carbon
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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
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/336—Preparation characterised by gaseous activating agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/20—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with polyhydric phenols
- C08G8/22—Resorcinol
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F42—AMMUNITION; BLASTING
- F42B—EXPLOSIVE CHARGES, e.g. FOR BLASTING, FIREWORKS, AMMUNITION
- F42B12/00—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material
- F42B12/02—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect
- F42B12/36—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect for dispensing materials; for producing chemical or physical reaction; for signalling ; for transmitting information
- F42B12/46—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect for dispensing materials; for producing chemical or physical reaction; for signalling ; for transmitting information for dispensing gases, vapours, powders or chemically-reactive substances
- F42B12/48—Projectiles, missiles or mines characterised by the warhead, the intended effect, or the material characterised by the warhead or the intended effect for dispensing materials; for producing chemical or physical reaction; for signalling ; for transmitting information for dispensing gases, vapours, powders or chemically-reactive substances smoke-producing, e.g. infrared clouds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- General Engineering & Computer Science (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The application discloses an aerosol and a preparation method thereof. The preparation method comprises the following steps: obtaining carbon aerogel; and crushing the carbon aerogel to obtain a granular material of the carbon aerogel, wherein the granular material of the carbon aerogel is used as an aerosol. The carbon aerogel obtained by the preparation method is used as a smoke agent, and the wave-absorbing property of the carbon aerogel is utilized to improve the shielding effect under the electromagnetic detection condition.
Description
Technical Field
The invention belongs to the field of carbon materials, and particularly relates to an aerosol and a preparation method thereof.
Background
The aerosol is a relatively stable aerosol formed by burning or physical dispersion, and contains solid or liquid particles for absorbing and scattering light rays to shield a target.
The existing smoke agent mainly adopts white phosphorus as a smoke agent, and the white phosphorus generates a large amount of smoke in the combustion process so as to achieve the purpose of disturbing the sight. However, this aerosol has the following disadvantages: the smoke outlet has overhigh temperature, is easy to be detected by infrared and laser weapons, and cannot achieve perfect interference effect; the shielding effect is poor, and only the visible light is acted; there is a time delay from emission to formation of the effective smoke.
Therefore, development of a new aerosol is expected to improve the masking effect under electromagnetic detection conditions.
Disclosure of Invention
The invention aims to provide an aerosol and a preparation method thereof, and the aerosol adopts carbon aerogel as a smoke agent to improve the shielding effect under the electromagnetic detection condition.
According to a first aspect of the present invention there is provided a method of preparing an aerosol characterised by the steps of: obtaining carbon aerogel; and crushing the carbon aerogel to obtain a granular material of the carbon aerogel, wherein the granular material of the carbon aerogel is used as an aerosol.
Preferably, the step of obtaining the carbon aerogel comprises: dissolving a phenolic compound, an aldehyde compound and a catalyst in a reaction solvent to form a precursor solution; mixing the precursor solution with a surfactant to form a mixed solution; performing constant-temperature culture, and forming organic aerogel through polymerization reaction of phenolic compounds and aldehyde compounds; carbonizing under the protection of inert gas to form carbon aerogel; and activating the carbon aerogel by using reaction gas.
Preferably, the phenolic compound comprises at least one selected from polyhydroxybenzene, dihydroxybenzene and trihydroxybutane.
Preferably, the aldehyde compound includes at least one selected from the group consisting of formaldehyde, paraformaldehyde, trioxane, methyl formaldehyde, acetaldehyde, propionaldehyde, and butyraldehyde.
Preferably, the catalyst is any one selected from an acidic catalyst and a basic catalyst.
Preferably, the acidic catalyst comprises at least one selected from boric acid, hydrochloric acid, citric acid, ascorbic acid.
Preferably, the basic catalyst comprises at least one selected from the group consisting of sodium carbonate, sodium hydroxide, potassium carbonate, and ammonia.
Preferably, the surfactant comprises at least one selected from the group consisting of fluorocarbon, polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, polyether polyol.
Preferably, the carbon aerogel is subjected to jet milling, wherein the feeding pressure adopted in the jet milling is 0.4MPa, the jet pressure of the jet milling is 0.8MPa, and the milling time is 1-2 hours.
According to a second aspect of the present invention there is provided an aerosol prepared by the above method, wherein the particulate material of the carbon aerogel has an average particle size of no more than 2.5 μm.
According to the preparation method provided by the embodiment of the invention, the granular material of the carbon aerogel is used as the smoke agent, and the smoke can be generated by adopting a physical dispersion method during use, so that the problem that infrared detection is visible due to the combustion temperature during the combustion of white phosphorus can be avoided.
In a preferred embodiment, the carbon aerogel material obtained by adding the surfactant is fluffy and has the density as low as 0.1-0.3 g/cm3, and the loss rate of the material in the carbon activation process is effectively reduced.
The particle material of the carbon aerogel in the aerosol is rich in a large number of hydrophilic functional groups, has strong hygroscopicity, namely is easy to nucleate or attach with water drops in the air, and is easy to form fog. The formed smoke-making has strong shielding effect on visible and infrared signals and strong attenuation characteristic on terahertz waves (30 mu m-3 mm).
Drawings
Figure 1 shows a flow diagram of an aerosol preparation method according to the present invention.
FIG. 2 shows a flow diagram of a method of making the carbon aerogel of FIG. 1.
Fig. 3 shows an SEM photograph of an aerosol prepared according to an embodiment of the present invention.
Figure 4 shows a transmission time plot for infrared detection of an aerosol prepared according to an embodiment of the present invention.
Detailed Description
Various embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. Like elements in the various figures are denoted by the same or similar reference numerals. For purposes of clarity, the various features in the drawings are not necessarily drawn to scale.
The inventors have noted that it is suitable to use a carbon aerogel as the aerosol. For example, physical dispersion methods may be used to distribute particulate materials of carbon aerogels in the air to form an aerosol.
The carbon aerogel is a light nano porous material, has the characteristics of high specific surface area, high porosity, high conductivity, controllable nano structure and the like, and is widely applied. The structure of the carbon aerogel has strong absorption characteristics in a wider electromagnetic spectrum and has strong absorption effects on visible light, near infrared, middle and far infrared, terahertz wave and the like.
In addition, the carbon aerogel not only can form large-area smoke in a short time as a single smoke material due to the characteristics of light weight, small density and the like, but also can be more easily nucleated or attached with water drops in the air under the condition of using the carbon aerogel for fogging due to strong hygroscopicity, so that the carbon aerogel can be quickly fogged. Therefore, carbon aerogels have excellent application conditions as aerosols.
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples.
Figure 1 shows a flow diagram of an aerosol preparation method according to the present invention.
In step S01, a carbon aerogel is obtained.
The carbon aerogel obtained in the step S01 is rich in oxygen-containing functional groups and has a density of 0.1-0.3 g/cm3。
In step S02, the carbon aerogel is pulverized to obtain a particulate material of the carbon aerogel. The particulate material of the carbon aerogel is used as an aerosol.
For example, the carbon aerogel is subjected to jet milling, wherein the feeding pressure adopted in the jet milling is 0.4MPa, the jet milling nozzle pressure is 0.8MPa, and the milling time is 1-2 hours. In the jet milling process, the particle size of the material is controlled below 2.5 μm.
FIG. 2 shows a flow diagram of a method of making the carbon aerogel of FIG. 1. Step S01 shown in fig. 1 includes a plurality of sub-steps S11 to S15.
In step S11, the phenolic compound, the aldehyde compound, and the catalyst are dissolved in the reaction solvent to form a precursor solution.
The phenolic compound comprises at least one selected from polyhydroxy benzene, dihydroxy benzene and trihydroxy butane. The aldehyde compound includes at least one selected from the group consisting of formaldehyde, paraformaldehyde, trioxane, methyl formaldehyde, acetaldehyde, propionaldehyde, and butyraldehyde. The catalyst is any one selected from an acidic catalyst and a basic catalyst. The acidic catalyst comprises at least one selected from boric acid, hydrochloric acid, citric acid and ascorbic acid. The alkaline catalyst comprises at least one selected from sodium carbonate, sodium hydroxide, potassium carbonate and ammonia water.
Preferably, resorcinol, formaldehyde and sodium carbonate are used as the phenolic compound, the aldehyde compound and the catalyst respectively to prepare the precursor solution. For example, resorcinol and formaldehyde are in a mass ratio of resorcinol: 10-100 parts of formaldehyde, wherein the resorcinol and the sodium carbonate are mixed according to the mass ratio of resorcinol: 50-500 parts of sodium carbonate. However, the present invention is not limited thereto.
In step S12, the precursor solution is mixed with a surfactant to form a mixed solution.
The surfactant comprises at least one selected from fluorocarbon, polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, and polyether polyol
Preferably, the mass ratio of the added amount of the surfactant to the resorcinol is 0.001-0.05. However, the present invention is not limited thereto.
In step S13, isothermal incubation is performed, and an organic aerogel is formed by polymerization of a phenolic compound and an aldehyde compound. For example, the culture temperature is 25-90 deg.C, and the culture time is 2-6 days
In step S14, a carbonization process is performed under an inert gas blanket to form a carbon aerogel.
The inert gas includes at least one selected from nitrogen, argon and helium. For example, the temperature of nitrogen carbonization is 900 to 1100 ℃, and the carbonization time is 2 to 6 hours.
In step S15, the carbon aerogel is subjected to an activation treatment using a reaction gas. For example, the temperature for activating carbon dioxide is 800-1000 ℃, and the activation time is 2-6 hours.
Examples of aerosol preparation methods according to the present invention will be further detailed below.
First embodiment
The resorcinol and the formaldehyde are mixed by mass ratio as resorcinol: mixing and stirring formaldehyde which is 10 percent, and after the foam completely disappears, mixing the mixture by mass ratio of resorcinol: sodium carbonate was added to 50 parts of sodium carbonate, and the mixture was stirred at room temperature for 45min to obtain a precursor solution.
Adding P123 into the precursor solution according to the mass ratio of 0.002, mixing, ultrasonically stirring for 30min to form a uniform mixed solution, and culturing the mixed solution in a thermostat at 50 ℃ for 3 d; and obtaining the organic aerogel after the culture is finished.
Carbonizing the product obtained in the step for 6 hours at 900 ℃ in a nitrogen atmosphere with the flow rate of 100ml/min after replacement; then activated for 6 hours at 800 ℃ in the atmosphere of carbon dioxide to obtain the carbon aerogel material.
And (3) carrying out jet milling on the carbon aerogel material obtained in the step, controlling the feeding pressure to be 0.4MPa, controlling the pressure of a jet milling nozzle to be 0.8MPa, and carrying out milling for 2 hours to obtain the light carbon aerogel material with the particle size of below 2.5 microns, wherein the light carbon aerogel material is used as an aerosol.
Second embodiment
The resorcinol and the formaldehyde are mixed by mass ratio as resorcinol: mixing and stirring formaldehyde 20, and after the foam completely disappears, mixing the mixture by mass ratio of resorcinol: sodium carbonate was added to 80 parts of sodium carbonate, and the mixture was stirred at room temperature for 60min to obtain a precursor solution.
Adding Cetyl Trimethyl Ammonium Bromide (CTAB) and resorcinol into a precursor solution according to the mass ratio of 0.005, mixing, ultrasonically stirring for 30min to form a uniform mixed solution, and culturing the mixed solution in a thermostat at 90 ℃ for 2 d; and obtaining the organic aerogel after the culture is finished.
Replacing the product obtained in the step, and carbonizing the product at 1050 ℃ for 4 hours in a nitrogen atmosphere with the flow rate of 100 ml/min; then activating for 4 hours at 900 ℃ in the atmosphere of carbon dioxide to obtain the carbon aerogel material.
And (3) carrying out jet milling on the carbon aerogel material obtained in the step, controlling the feeding pressure to be 0.4MPa, controlling the pressure of a jet milling nozzle to be 0.8MPa, and carrying out milling for 2 hours to obtain the light carbon aerogel material with the particle size of below 2.5 microns, wherein the light carbon aerogel material is used as an aerosol.
Fig. 3 shows an SEM photograph of an aerosol prepared according to an embodiment of the present invention. As can be seen from the photographs, the aerosol prepared according to the method of the first embodiment of the present invention is excellent in morphology in which the average particle size of the particulate material of the carbon aerogel is not more than 2.5 μm.
Figure 4 shows a transmission time plot for infrared detection of an aerosol prepared according to an embodiment of the present invention. The aerosol is distributed by a physical dispersion method, and then the infrared transmittance is changed along with the time by a thermal infrared imager. As can be seen from the measurement graph, the aerosol started to function at 8 seconds, and the infrared transmittance was maintained less than 10% during the measured period of 37 seconds, thereby exhibiting a good infrared shielding effect.
Although the preferred embodiments of the present invention have been disclosed in the foregoing description, it should be understood that they are not intended to limit the scope of the claims appended hereto, and that various changes and modifications may be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of an aerosol is characterized by comprising the following steps:
obtaining carbon aerogel; and
pulverizing the carbon aerogel to obtain a particulate material of the carbon aerogel,
wherein the particulate material of the carbon aerogel is used as an aerosol.
2. The method of claim 1, wherein the step of obtaining a carbon aerogel comprises:
dissolving a phenolic compound, an aldehyde compound and a catalyst in a reaction solvent to form a precursor solution;
mixing the precursor solution with a surfactant to form a mixed solution;
performing constant-temperature culture, and forming organic aerogel through polymerization reaction of phenolic compounds and aldehyde compounds;
carbonizing under the protection of inert gas to form carbon aerogel; and
and activating the carbon aerogel by using reaction gas.
3. The method according to claim 2, wherein the phenolic compound comprises at least one selected from the group consisting of polyhydroxybenzenes, dihydroxybenzenes, and trihydroxybutanes.
4. The method according to claim 2, wherein the aldehyde compound comprises at least one selected from the group consisting of formaldehyde, paraformaldehyde, trioxane, methyl formaldehyde, acetaldehyde, propionaldehyde and butyraldehyde.
5. The production method according to claim 2, wherein the catalyst is any one selected from an acidic catalyst and a basic catalyst.
6. The method according to claim 5, wherein the acidic catalyst comprises at least one selected from boric acid, hydrochloric acid, citric acid, and ascorbic acid.
7. The method according to claim 5, wherein the basic catalyst comprises at least one selected from the group consisting of sodium carbonate, sodium hydroxide, potassium carbonate, and ammonia water.
8. The method according to claim 2, wherein the surfactant comprises at least one selected from the group consisting of fluorocarbons, polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymers, cetyltrimethylammonium bromide, sodium dodecylbenzenesulfonate, and polyether polyols.
9. The method according to claim 2, wherein the carbon aerogel is subjected to jet milling, wherein the feeding pressure used in the jet milling is 0.4MPa, the jet milling nozzle pressure is 0.8MPa, and the milling time is 1 to 2 hours.
10. An aerosol obtained by the method of any one of claims 1 to 9, wherein the particulate material of the carbon aerogel has an average particle size of not more than 2.5 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910020599.8A CN111422867A (en) | 2019-01-09 | 2019-01-09 | Aerosol and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910020599.8A CN111422867A (en) | 2019-01-09 | 2019-01-09 | Aerosol and preparation method thereof |
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| CN111422867A true CN111422867A (en) | 2020-07-17 |
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| CN201910020599.8A Pending CN111422867A (en) | 2019-01-09 | 2019-01-09 | Aerosol and preparation method thereof |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108601316A (en) * | 2018-01-18 | 2018-09-28 | 航天特种材料及工艺技术研究所 | A kind of preparation method and application of electromagnetic shielding material |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108601316A (en) * | 2018-01-18 | 2018-09-28 | 航天特种材料及工艺技术研究所 | A kind of preparation method and application of electromagnetic shielding material |
Non-Patent Citations (1)
| Title |
|---|
| A. ABOLGHASEMI MAHANI等: "Synthesis, characterization and dielectric properties of one-step pyrolyzed / activated resorcinol-formaldehyde based carbon aerogels for electromagnetic interference shielding applications", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
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Application publication date: 20200717 |