CN115466528B - Carbon black aerogel and preparation method thereof - Google Patents
Carbon black aerogel and preparation method thereof Download PDFInfo
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Abstract
The invention discloses carbon black aerogel and a preparation method thereof. The preparation method comprises the following steps: making a carbon felt cylinder by using a carbon felt as a deposition substrate; taking natural gas, propylene or propane as carbon source gas, taking argon or nitrogen as protective gas, and carrying out chemical vapor deposition under the conditions that the temperature is 900-1150 ℃ and the pressure is 20-101 kPa to obtain the carbon black aerogel. The preparation method of the carbon black aerogel provided by the invention is simple, efficient, clean and environment-friendly; the prepared carbon black aerogel is a novel full-carbon aerogel, has the characteristics of low density, strong compression resistance, super-hydrophobicity, low thermal conductivity and the like, has excellent comprehensive performance, and has great application potential in the fields of super capacitors, energy storage materials, wastewater treatment, thermal insulation materials and the like.
Description
Technical Field
The invention belongs to the technical field of carbon aerogel preparation, and particularly relates to carbon black aerogel and a preparation method thereof.
Background
As a novel carbon nano material, the carbon aerogel has the excellent characteristics of low density, high specific surface area, rich pore structure, high conductivity and the like, has wide application potential in the fields of adsorption materials, electrochemistry, hydrogen storage materials and the like, and becomes the front edge and hot spot of carbon material research.
From the current state of research, the development and preparation of new carbon aerogels, raw materials are critical. At present, main raw materials for preparing the carbon aerogel comprise carbon nano tubes, graphene, biomass and phenolic aldehyde, wherein a phenolic aldehyde polymerization process is complex, the cost is high, the environment is polluted, the process for preparing the carbon aerogel is complex, the cost is high, and the price is high, so that the industrial production of the carbon aerogel is limited, and the carbon aerogel has important practical significance and theoretical value if the novel carbon aerogel prepared by adopting renewable, environment-friendly and pollution-free biomass raw materials is realized. Carbon black is a polymeric structure formed by fusing together a plurality of nano-sized particles, particularly carbon black aggregates, which can be entangled together so that the distance distribution between the particles is narrow, thereby forming a network of carbon black clusters. This network structure is consistent with the carbon aerogel microstructure currently being widely studied. From the structural aspect, the carbon black particles can be used as the basic unit of the carbon aerogel. In comparison, the carbon black has low production and preparation cost, simple and reliable process and wide raw material sources, but the carbon black is rarely used independently at present, and basically, carbon black powder is combined with other components to form a composite material. Therefore, if carbon black is used as a raw material to prepare the carbon aerogel, the problems of complex production operation, long period, low yield and the like of the carbon aerogel can be avoided.
Disclosure of Invention
Aiming at the current research situation, the invention aims to provide the carbon black aerogel and the preparation method thereof, wherein the method has the advantages of simple process, low energy consumption, high production efficiency, low density of the prepared carbon black aerogel, good water-repellent capacity, good electric conduction performance and good heat insulation capacity, and can realize continuous industrial production.
The preparation method of the carbon black aerogel provided by the invention comprises the following steps:
1) The carbon felt is manufactured into a cylindrical deposition substrate, one end of the cylindrical deposition substrate is provided with an air inlet hole, and the other end of the cylindrical deposition substrate is sealed by a cover plate or is provided with an opening as an air outlet;
2) And (3) placing the cylindrical deposition substrate prepared in the step (1) into a deposition furnace or a tubular furnace, introducing carbon source gas and protective gas, performing chemical vapor deposition, cooling after the deposition is finished, and cutting and stripping the cylindrical deposition substrate to obtain the carbon black aerogel.
Preferably, in the step 1), the carbon felt is at least one of a short fiber carbon felt, a needled felt and a three-dimensional puncture woven carbon felt; the porosity of the cylindrical deposition substrate is 40% -90%, and the thickness is 1-12 mm; the cylindrical deposition substrate is a rectangular parallelepiped or cylindrical deposition substrate.
Preferably, in the step 1), the cover plate is at least one of a carbon felt plate, a graphite plate and a quartz plate; the total area of the air outlets is not more than 8mm 2 。
Preferably, in the step 2), the carbon source gas is at least one of natural gas, propylene and propane; the shielding gas is at least one of nitrogen and argon.
Preferably, in the step 2), the chemical vapor deposition adopts a fluidized bed chemical vapor deposition method, and the carbon black particles have similar flow performance with fluid under the action of air flow in the deposition process; the volume ratio of the carbon source gas to the shielding gas is 1-3:1-2; the chemical vapor deposition process conditions are as follows: the temperature is 900-1150 ℃, the pressure is 20-101 kPa, and the deposition time is 2-12 hours.
Preferably, in the step 2), the chemical vapor deposition furnace body includes a cooling water inlet 2, a cooling water outlet 6, an air inlet 1 and a tail gas outlet 7 provided on the furnace body, a graphite heating body 3 provided around the base 4, a soft thermocouple 8 for detecting the temperature in the reaction chamber, a support plate 9 provided in the reaction chamber, a heat insulation plate 10 provided opposite to the support plate, and an air inlet pipe 1 penetrating through the bottom wall of the furnace body, the heat insulation plate 10 and the support plate 9 in sequence, a cylindrical base 4 provided on the support plate tooling 9, wherein the upper end of the cylindrical base 4 is sealed with a cover plate 5, and carbon source gas and protective gas enter the area formed by surrounding the cylindrical base 4, the support plate 9 and the cover plate 5 through the air inlet pipe 1, and then flow around the cavity of the cylindrical base, so that the reaction gas and the carbon felt base are fully contacted and deposited to form carbon black aerogel.
The carbon black aerogel is prepared according to the preparation method.
Preferably, the carbon black aerogel is formed by stacking and depositing carbon black particles layer by layer after a branched chain structure is formed; the particle size of the carbon black particles in the carbon black aerogel is 50-500 nm.
Preferably, the density of the carbon black aerogel is 0.1 to 0.2g/cm 3 。
Preferably, the hydrophobic angle of the carbon black aerogel is 130 ° to 160 °.
The invention has the beneficial effects that:
1) The carbon black aerogel disclosed by the invention is a novel full-carbon aerogel, and the carbon black raw material is easy to obtain and wide in source.
2) According to the method, carbon black is deposited by a chemical vapor deposition method, and the carbon black can be directly used for preparing the solid aerogel from a gas-phase carbon source without a catalyst to form the aerogel material with the full carbon component, so that the method is simple in process treatment, high in production efficiency, clean and environment-friendly, reduces the preparation cost of the aerogel, and can realize industrial popularization.
3) According to the invention, the deposition state of the carbon black aerogel is effectively controlled by regulating and controlling the deposition time, temperature, pressure and other parameters, and the obtained carbon black aerogel material has low density and good water-repellent capacity, conductive performance and heat insulation capacity.
4) The invention can obtain the carbon black aerogel material with specific shape and size by cutting.
5) The carbon black aerogel prepared by the method enriches the variety of the aerogel, expands the variety of carbon black materials, and improves the position of carbon black in material design and production.
Drawings
FIG. 1 is a schematic view of a chemical vapor deposition furnace according to the present invention;
1-an air inlet pipe; 2-a cooling water inlet; 3-graphite heating element; 4-a substrate; 5-cover plate; 6-a cooling water outlet; 7-an air outlet; 8-a soft thermocouple; 9-supporting plates; 10-heat insulation board.
FIGS. 2 (a) and (b) are scanning electron microscope images of the carbon black aerogel prepared in example 1 at different magnifications.
Fig. 3 is a diagram of a rectangular parallelepiped and cylindrical carbon felt substrate.
FIG. 4 is a diagram of a carbon felt substrate embodying a specific shape (disk shape).
FIGS. 5 (a) and (b) are illustrations of thickness measurement and morphology display, respectively, of carbon black aerogel after being cut in example 1.
FIGS. 6 (a) and (b) are, respectively, graphs of the hydrophobic effect and static hydrophobic angle measurements of the carbon black aerogel of example 1.
Detailed Description
The present invention is further described below in connection with specific embodiments in order to better understand the technical solution of the present invention and to make the objects, features and advantages of the present invention more apparent to those skilled in the art.
A schematic structure of a chemical vapor deposition furnace used in an embodiment of the present invention is shown in FIG. 1.
Example 1
Firstly, a carbon felt having dimensions of 955mm×10mm×300mm (density of 0.1 g/cm) 3 ) Sewing carbon felt with carbon fiber to obtainThe cylindrical carbon felt is used as a deposition substrate and is placed in a chemical vapor deposition furnace. The temperature rising rate is controlled to be less than 80 ℃/min, so that the temperature in the furnace is raised to 1030 ℃ and then the heat preservation is carried out. At this time, air is introduced from the lower end of the cylindrical carbon felt base, and the upper end is sealed with a carbon felt cover plate. The chemical vapor deposition process was carried out at 1030℃and 45kPa, with propane (purity 99.6%) as the carbon source gas and argon (purity 99.9%) as the shielding gas. The volume ratio of propane to argon is 3:2, and the total flow of the mixed gas is 3.5L/min. And (5) after the deposition treatment is carried out for 10 hours, cooling to obtain the carbon black aerogel material. The heating and cooling processes in the furnace are carried out under the argon atmosphere, and the propane charging time is the same as the deposition time.
FIGS. 2 (a) and (b) are scanning electron microscope images of the carbon black aerogel prepared in example 1 at different magnifications; FIGS. 5 (a) and (b) are illustrations of thickness measurement and morphology display, respectively, of carbon black aerogel after being cut in example 1; FIGS. 6 (a) and (b) are, respectively, graphs of the hydrophobic effect and static hydrophobic angle measurements of the carbon black aerogel of example 1.
The obtained carbon black aerogel material has a height of 290mm, a cylindrical shape as a whole, an inner diameter of about 240mm and an outer diameter of about 300mmThe thickness of the carbon black aerogel is about 30mm; cutting the carbon felt substrate to obtain carbon black aerogel, wherein the density of the carbon black aerogel is 0.15g/cm 3 The surface is soft and moist, the cross section has a lamellar deposition characteristic band, the hydrophobic angle is 151.2 degrees, the compressive strength is about 0.8MPa, and the thermal conductivity at room temperature is 0.049W (m.k) -1 。
Example 2
Firstly, a carbon felt with dimensions of 880mm by 10mm by 150mm (density of 0.2 g/cm) 3 ) Sewing carbon felt with carbon fiber to obtainThe cylindrical carbon felt is used as a deposition substrate and is placed in a chemical vapor deposition furnace. The temperature rising rate is controlled to be less than 80 ℃/min, so that the temperature in the furnace is raised to 930 ℃ and then the heat preservation is carried out. Air is introduced from the lower end of the cylindrical carbon felt substrate, the upper end is sealed by a carbon felt cover plate, and 6mm of air is reserved in the middle of the cover plate 2 The round hole of the air inlet is used as an air outlet hole. The chemical vapor deposition process was performed at a temperature of 930 ℃ and a pressure of 55kPa, with propylene (purity 99.6%) as a carbon source gas and nitrogen (purity 99.8%) as a shielding gas. The volume ratio of propylene to nitrogen is 1:1, and the total flow of the mixed gas is 3L/min. And (3) after the deposition treatment is carried out for 8 hours, cooling to obtain the carbon black aerogel material. The heating and cooling processes in the furnace are carried out under the nitrogen atmosphere, and the propylene charging time is the same as the deposition time.
The obtained carbon black aerogel material has the height of 150mm, the whole body is in a base cylinder shape, the inner diameter is about 220mm, the outer diameter is about 270mm, and the thickness of the carbon black aerogel is about 25mm; cutting the carbon felt substrate, taking out the carbon black aerogel, and measuring the density of the carbon black aerogel to be 0.11g/cm 3 The surface is soft and moist, the cross section has a lamellar deposition characteristic band, the hydrophobic angle is 155.6 degrees, the compressive strength is about 1.12MPa, and the thermal conductivity at room temperature is 0.039W (m.k) -1 。
Example 3
Firstly, cutting a carbon felt with the dimensions of 880mm multiplied by 10mm multiplied by 150mm (the density of the carbon felt is 0.2 g/cm) 3 ) Sewing carbon felt with carbon fiber to obtainThe cylindrical carbon felt is used as a deposition substrate and is placed in a chemical vapor deposition furnace. The temperature rising rate is controlled to be less than 80 ℃/min, so that the temperature in the furnace is raised to 1150 ℃ and then the heat preservation is carried out. Air is introduced from the lower end of the cylindrical carbon felt substrate, and the upper end of the cylinder is sealed by a quartz cover plate. The chemical vapor deposition process is carried out at the temperature of 1150 ℃ and the pressure of 65kPa, natural gas is selected as carbon source gas, and nitrogen (the purity is 99.8%) and argon (the purity is 99.9%) are mixed to be used as protective gas. The volume ratio of the natural gas to the argon to the nitrogen is 2:1:1, and the total flow of the mixed gas is 6L/min. And (3) cooling after 8 hours of deposition treatment to obtain the carbon black aerogel material. The heating and cooling processes in the furnace are carried out under the argon atmosphere, and the natural gas charging time is the same as the deposition time.
The obtained carbon black aerogel material has a height of 145mm, a whole substrate cylindrical shape, an inner diameter of about 226mm, an outer diameter of about 270mm and a carbon black aerogel thickness of about 22mm. Cutting the carbon felt substrate, taking out the carbon black aerogel, and measuring the density of the carbon black aerogel to be 0.15g/cm 3 The hydrophobic angle is 153.3 degrees, the compressive strength is about 0.6MPa, and the thermal conductivity at room temperature is 0.043W (m.k) -1 。
Example 4
Firstly, a square carbon felt with the dimensions of 280mm multiplied by 10mm (density of 0.13 g/cm) 3 ) And sewing the carbon felt with carbon fiber to obtain square carbon felt cylinder with thickness of 280mm x 280mm and 10mm as deposition base, and setting in chemical vapor deposition furnace. The temperature rising rate is controlled to be less than 80 ℃/min, so that the temperature in the furnace is raised to 980 ℃ and then the heat preservation is carried out. Air is introduced from the lower end of the square carbon felt cylinder, and the upper end of the cylinder is sealed by a carbon felt cover plate. The chemical vapor deposition process is carried out at the temperature of 980 ℃ and the pressure of 55kPa, and propylene (with the purity of 99.6%) is selected as carbon source gas and argon (with the purity of 99.9%) is selected as protective gas. The volume ratio of propylene to argon is 1:1, and the total flow of the mixed gas is 3L/min. And (3) cooling after the deposition treatment for 10 hours to obtain the carbon black aerogel material. The heating and cooling processes in the furnace are carried out under the argon atmosphere, and the propylene charging time is the same as the deposition time.
The obtained carbon black aerogel material has the size of 280mm multiplied by 23mm; cutting the carbon felt cylinder substrate, taking out the carbon black aerogel, and measuring the carbonThe density of the black aerogel is 0.13g/cm 3 The hydrophobic angle is 148.3 degrees, the hydrophobic material has good hydrophobicity, the compressive strength is about 1.15MPa, and the thermal conductivity at room temperature is 0.045W (m.k) -1 。
Example 5
Firstly, a carbon felt with the size of about 975mm×10mm×300mm (density of 0.1 g/cm) 3 ) Sewing carbon felt with carbon fiber to obtainThe cylindrical carbon felt is used as a deposition substrate and is placed in a chemical vapor deposition furnace. The temperature rising rate is controlled to be less than 80 ℃/min, so that the temperature in the furnace is increased to 900 ℃ and then the heat preservation is carried out. At this time, air is introduced from the lower end of the cylindrical carbon felt base, and the upper end is sealed with a carbon felt cover plate. The chemical vapor deposition treatment process is carried out at the temperature of 900 ℃ and the pressure of 101kPa (normal pressure), propylene (with the purity of 99.6%) is selected as carbon source gas, and argon (with the purity of 99.9%) is selected as protective gas. The volume ratio of propylene to argon is 3:2, and the total flow of the mixed gas is about 8L/min. And (5) stopping the furnace for cooling after 12 hours of deposition treatment to obtain the carbon black aerogel material. The heating and cooling processes in the furnace are carried out under the argon atmosphere, and the propylene charging time is the same as the deposition time.
The obtained carbon black aerogel material had a height of 295mm, an overall cylindrical shape, an inner diameter of about 232mm, an outer diameter of about 300mm, and a carbon black aerogel thickness of about 34mm (overall dimensions of about ) The method comprises the steps of carrying out a first treatment on the surface of the The density of the carbon black aerogel was measured to be 0.18g/cm 3 The cross section of the ceramic material has a layered deposition characteristic band, the hydrophobic angle is 157.3 degrees, the compressive strength is about 1.2MPa, and the thermal conductivity at room temperature is 0.051W (m.k) -1 。
Example 6
Firstly, a carbon felt with dimensions of 975mm×10mm×300mm (density of 0.1 g/cm) 3 ) Sewing carbon felt with carbon fiber to obtainThe cylindrical carbon felt is used as a deposition substrate and is placed in a chemical vapor deposition furnace. The temperature rising rate is controlled to be less than 80 ℃/min, so that the temperature in the furnace is raised to 1050 ℃ and then the heat preservation is carried out. At this time, air is introduced from the lower end of the cylindrical carbon felt base, and the upper end is sealed with a carbon felt cover plate. The chemical vapor deposition treatment process is carried out at 1050 ℃ and 20kPa, and propane (purity of 99.6%) is selected as carbon source gas and nitrogen (purity of 99.9%) is selected as protective gas. The volume ratio of propane to nitrogen is 2:1, and the total flow of the mixed gas is about 6L/min. And (5) after the deposition treatment is carried out for 2 hours, stopping the furnace and cooling to obtain the carbon black aerogel material. The heating and cooling processes in the furnace are carried out under the nitrogen atmosphere, and the propane charging time is the same as the deposition time.
The obtained carbon black aerogel material has soft and moist surface gloss, the height of the carbon black aerogel material is about 293mm, the whole carbon black aerogel material is cylindrical, the inner diameter of the carbon black aerogel material is about 288mm, the outer diameter of the carbon black aerogel material is about 300mm, and the thickness of the carbon black aerogel material is about 6mm; the carbon black aerogel product was removed from the inside wall of the carbon felt cylinder and its density was measured to be about 0.10g/cm 3 The hydrophobic angle was 152.6℃and the compressive strength was about 0.46MPa, and the thermal conductivity at room temperature was 0.036 W.multidot.k -1 。
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention.
Claims (8)
1. A preparation method of carbon black aerogel comprises the following steps:
1) The carbon felt is manufactured into a cylindrical deposition substrate, one end of the cylindrical deposition substrate is provided with an air inlet hole, and the other end of the cylindrical deposition substrate is sealed by a cover plate or is provided with an opening as an air outlet;
the porosity of the cylindrical deposition substrate is 40% -90%, and the thickness is 1-12 mm; the total area of the air outlets is not more than 8mm 2 ；
2) Putting the cylindrical deposition substrate prepared in the step 1) into a chemical vapor deposition furnace, introducing carbon source gas and protective gas, performing chemical vapor deposition, cooling after the deposition is finished, and cutting and stripping the cylindrical deposition substrate to obtain carbon black aerogel;
the carbon source gas is at least one of natural gas, propylene and propane; the protective gas is at least one of nitrogen and argon;
the chemical vapor deposition adopts a fluidized bed chemical vapor deposition method, and carbon black particles show similar flow performance with fluid under the action of air flow in the deposition process; the volume ratio of the carbon source gas to the shielding gas is 1-3:1-2; the chemical vapor deposition process conditions are as follows: the temperature is 900-1150 ℃, the pressure is 20-101 kPa, and the deposition time is 2-12 hours.
2. The method of claim 1, wherein in step 1), the carbon felt is at least one of a short fiber carbon felt, a needle punched felt, and a three-dimensional puncture woven carbon felt; the cylindrical deposition substrate is a cuboid or cylindrical deposition substrate.
3. The method for preparing carbon black aerogel according to claim 1, wherein in step 1), the cover plate is at least one of a carbon felt, a graphite plate and a quartz plate.
4. The method for preparing carbon black aerogel according to claim 1, wherein in the step 2), the chemical vapor deposition furnace body comprises a cooling water inlet 2, a cooling water outlet 6, an air inlet 1 and a tail gas outlet 7 which are arranged on the furnace body, a graphite heating body 3 which is arranged around a substrate 4, a soft thermocouple 8 for detecting the temperature in a reaction chamber, a supporting plate 9 which is arranged in the reaction chamber, a heat insulating plate 10 which is arranged opposite to the supporting plate, an air inlet pipe 1 which sequentially penetrates through the bottom wall of the furnace body, the heat insulating plate 10 and the supporting plate 9, a cylindrical substrate 4 which is arranged on a supporting plate tool 9, and the upper end of the cylindrical substrate 4 is sealed by a cover plate 5; the carbon source gas and the shielding gas enter the area formed by the surrounding of the cylindrical substrate 4, the supporting plate 9 and the cover plate 5 through the gas inlet pipe 1, and then flow around the cavity of the cylindrical substrate, so that the reaction gas is fully contacted with the carbon felt substrate to deposit and form the carbon black aerogel.
5. A carbon black aerogel produced according to the production method of any one of claims 1 to 4.
6. The carbon black aerogel of claim 5, wherein the carbon black aerogel is formed by stacking and depositing carbon black particles layer by layer after the carbon black particles form a branched structure; the particle size of the carbon black particles in the carbon black aerogel is 50-500 nm.
7. The carbon black aerogel of claim 5, wherein the carbon black aerogel has a density of 0.1 to 0.2g/cm 3 。
8. The carbon black aerogel of claim 5, wherein the carbon black aerogel has a hydrophobic angle of 130 ° to 160 °.
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| CN112723898A (en) * | 2020-12-30 | 2021-04-30 | 内蒙古栢特新材料科技有限公司 | Preparation method of carbon/carbon liner for natural gas chemical vapor deposition furnace |
| CN114031065A (en) * | 2021-11-18 | 2022-02-11 | 郑州大学 | Silicon carbide fiber/carbon mixed aerogel and preparation method thereof |
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| CN112723898A (en) * | 2020-12-30 | 2021-04-30 | 内蒙古栢特新材料科技有限公司 | Preparation method of carbon/carbon liner for natural gas chemical vapor deposition furnace |
| CN114031065A (en) * | 2021-11-18 | 2022-02-11 | 郑州大学 | Silicon carbide fiber/carbon mixed aerogel and preparation method thereof |
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| Title |
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| 生物质碳气凝胶活化类型及其应用进展;梅意意;江西化工;第38卷(第2期);15-17 * |
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