CN115160829A - Carbon black aerogel and preparation method thereof - Google Patents
Carbon black aerogel and preparation method thereof Download PDFInfo
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- CN115160829A CN115160829A CN202210928006.XA CN202210928006A CN115160829A CN 115160829 A CN115160829 A CN 115160829A CN 202210928006 A CN202210928006 A CN 202210928006A CN 115160829 A CN115160829 A CN 115160829A
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Abstract
The invention discloses a carbon black aerogel and a preparation method thereof. The preparation method comprises the following steps: manufacturing a carbon felt cylinder by using a carbon felt as a deposition substrate; taking natural gas, propylene or propane as a carbon source gas, argon or nitrogen as a protective gas, and carrying out chemical vapor deposition at the temperature of 900-1150 ℃ and the pressure of 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 all-carbon aerogel, has the characteristics of low density, strong compressive capacity, super hydrophobicity, low thermal conductivity and the like, has excellent comprehensive performance, and has great application potential in the fields of supercapacitors, energy storage materials, wastewater treatment, heat 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 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 leading edge and the hotspot of carbon material research.
In view of the current research situation, the development and preparation of new carbon aerogel are key raw materials. At present, main raw materials for preparing carbon aerogel comprise carbon nano tubes, graphene, biomass and phenolic compounds, wherein a phenolic aldehyde polymerization process is complex, has high cost and pollutes the environment, and a process for preparing carbon aerogel is complex, has high cost and high price, so that the industrial production of the carbon aerogel is limited. Carbon black is a grape-like polymeric structure formed by fusing a plurality of nano-scale particles together, and particularly carbon black aggregates can be entangled, so that the distance distribution among the particles is narrow, and a network consisting of carbon black clusters is formed. This network structure is consistent with the carbon aerogel microstructure that is currently being studied extensively. From a structural standpoint, carbon black particles can serve as the basic unit for the composition of the carbon aerogel. In contrast, carbon black is low in production and preparation cost, simple and reliable in process and wide in raw material source, but at present, carbon black is rarely used alone, and carbon black powder and other components are basically combined to form a composite material. In addition, at present, carbon aerogel is obtained by adopting organogel through a critical drying and carbonization method, and the method has the defects of complex operation, long period, large energy consumption, low yield and the like.
Disclosure of Invention
In view of the current research situation, the invention aims to provide the carbon black aerogel and the preparation method thereof, the method has the advantages of simple process, low energy consumption and high production efficiency, and the prepared carbon black aerogel has low density, good hydrophobic capability, good conductive capability and good heat insulation capability, and can realize continuous industrial production.
The preparation method of the carbon black aerogel provided by the invention comprises the following steps:
1) Manufacturing the carbon felt into a cylindrical deposition substrate, wherein 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 putting 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 deposition is finished, 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 needle 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 cuboid or cylindrical deposition substrate.
Preferably, in the step 1), the cover plate is at least one of a carbon felt, 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 protective 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 exhibit flow performance similar to that of a fluid under the action of a gas flow during the deposition process; the volume ratio of the carbon source gas to the protective gas is 1-3; the process conditions of the chemical vapor deposition are as follows: the temperature is 900-1150 ℃, the pressure is 20-101 kPa, and the deposition time is 2-12 h.
Preferably, in the step 2), the furnace body of the chemical vapor deposition furnace comprises a cooling water inlet 2, a cooling water outlet 5, an air inlet 1 and a tail gas outlet 7 which are arranged in the furnace body, a reaction chamber which is formed by enclosing a heat preservation felt 4 and is arranged in the furnace body, an electrified copper coil 3 which is arranged around the heat preservation felt, a soft thermocouple 12 for detecting the temperature in the reaction chamber, a graphite support frame tool 10 which is arranged in the reaction chamber, a support plate tool 9 which is arranged opposite to the support frame, an air inlet pipe 11 which sequentially penetrates through the bottom wall of the furnace body, the bottom wall of the heat preservation felt, the support frame tool 10 and the support plate tool 9, a cylindrical substrate 8 which is arranged on the support plate tool 9, and the upper end of the cylindrical substrate 8 is sealed by a cover plate 6; carbon source gas and protective gas enter an area formed by the cylindrical substrate 8, the support plate tool 9 and the cover plate 6 through the gas inlet pipe 11, and then flow around in a cavity of the cylindrical substrate, so that reaction gas is in full contact with the carbon felt substrate for deposition.
The carbon black aerogel was prepared according to the above preparation method.
Preferably, the carbon black aerogel is formed by stacking and depositing layer by layer after the carbon black particles form a branched chain structure; the particle size of the carbon black particles in the carbon black aerogel is 50-500 nm.
Preferably, the carbon black aerogel has a density of 0.1 to 0.2g/cm 3 。
Preferably, the carbon black aerogel has a hydrophobic angle of 130 ° to 160 °.
The invention has the beneficial effects that:
1) The carbon black aerogel is a novel all-carbon aerogel, and the carbon black raw material is simple to obtain and wide in source.
2) According to the invention, carbon black is deposited by a chemical vapor deposition method, a gas-phase carbon source is directly transferred to solid-phase aerogel, and the aerogel material with all carbon components can be formed by adopting the carbon black without a catalyst, so that the process treatment is simple, the production efficiency is high, the aerogel material is clean and environment-friendly, the preparation cost of the aerogel is reduced, and the industrial popularization can be realized.
3) According to the invention, the deposition state of the carbon black aerogel is effectively controlled by regulating and controlling parameters such as deposition duration, temperature and pressure, and the obtained carbon black aerogel material has low density, and has good hydrophobic capability, conductive performance and heat insulation capability.
4) The carbon black aerogel material with a specific shape and size can be obtained 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 the 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-air inlet, 2-cooling water inlet, 3-copper coil, 4-heat preservation felt, 5-cooling water outlet, 6-cover plate, 7-air outlet, 8-cylindrical base, 9-support plate tool, 10-support frame tool, 11-air inlet pipe and 12-soft thermocouple.
FIGS. 2 (a) and (b) are scanning electron micrographs of the carbon black aerogel prepared in example 1 at different magnifications.
FIG. 3 is a base view of rectangular and cylindrical carbon felt.
FIG. 4 is a diagram of a carbon felt substrate with a specific shape (disk shape).
Fig. 5 (a) and (b) are the thickness measurement and form display diagrams of the carbon black aerogel after being cut in example 1.
FIGS. 6 (a) and (b) are respectively a hydrophobic effect graph and a static hydrophobic angle detection graph of the carbon black aerogel in example 1.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention and will better understand the objects, features and advantages of the present invention, the present invention will be further described with reference to the specific embodiments.
Example 1
Firstly, a carbon felt (density of 0.1 g/cm) with the size of 955mm multiplied by 10mm multiplied by 300mm is cut 3 ) Then sewing carbon felt with carbon fiber to obtain
The cylindrical carbon felt is used as a deposition substrate and is placed in a chemical vapor deposition furnace. Controlling the heating rate to be less than 80 ℃/min to ensure that the temperature in the furnace is raised to 1030 ℃ and then carrying out heat preservation. 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 was carried out at a temperature of 1030 ℃ and a pressure of 45kPa, using propane (purity 99.6%) as a carbon source gas and argon (purity 99.9%) as a shielding gas. The volume ratio of propane to argon is 3. And after deposition treatment for 10 hours, cooling to obtain the carbon black aerogel material. The heating and cooling processes in the furnace are carried out in the argon atmosphereThe propane fill time period is the same as the deposition time period.
FIGS. 2 (a) and (b) are scanning electron micrographs of the carbon black aerogel prepared in example 1 at different magnifications; FIGS. 5 (a) and (b) are the thickness measurement and form display diagrams of the carbon black aerogel after being cut in example 1; FIGS. 6 (a) and (b) are respectively a hydrophobic effect graph and a static hydrophobic angle detection graph of the carbon black aerogel in example 1.
The height of the obtained carbon black aerogel material is 290mm, the whole carbon black aerogel material is cylindrical, the inner diameter is about 240mm, the outer diameter is about 300mm, and the thickness of the carbon black aerogel is about 30mm; 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 surface is soft and moist, the cross section has a characteristic band of layered deposition, 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 (density of 0.2 g/cm) with the size of 880mm multiplied by 10mm multiplied by 150mm is cut 3 ) Then sewing carbon felt with carbon fiber to obtain
The cylindrical carbon felt is used as a deposition substrate and is placed in a chemical vapor deposition furnace. Controlling the heating rate to be less than 80 ℃/min to ensure that the temperature in the furnace is raised to 930 ℃ and then carrying out heat preservation. Air is fed from the lower end of the cylindrical carbon felt substrate, the upper end of the cylindrical carbon felt substrate is sealed by a carbon felt cover plate, and 6mm is reserved in the middle of the cover plate 2 The round hole is used as an air outlet. The chemical vapor deposition process was carried out at a temperature of 930 deg.C and a pressure of 55kPa, using 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 was 1. And after 8h of deposition treatment, cooling to obtain the carbon black aerogel material. The heating and cooling processes in the furnace are carried out in the nitrogen atmosphere, and the filling time of the propylene is the same as the deposition time.
The height of the obtained carbon black aerogel material is 150mm, the whole carbon black aerogel material is in a base cylindrical 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 be0.11g/cm 3 The surface is soft and moist, the cross section has a characteristic band of layered deposition, 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 size of 880mm multiplied by 10mm multiplied by 150mm (the density of the carbon felt is 0.2 g/cm) 3 ) Then sewing carbon felt with carbon fiber to obtain
The cylindrical carbon felt is used as a deposition substrate and is placed in a chemical vapor deposition furnace. Controlling the heating rate to be less than 80 ℃/min to heat the temperature in the furnace to 1150 ℃ and then carrying out heat preservation. Air is fed 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 was carried out at 1150 ℃ and 65kPa using natural gas as the carbon source gas and a mixture of nitrogen (99.8% purity) and argon (99.9% purity) as the shielding gas. The volume ratio of natural gas, argon gas and nitrogen gas is 2. And after 8h of deposition treatment, cooling to obtain the carbon black aerogel material. The heating and cooling processes in the furnace are carried out in the argon atmosphere, and the natural gas filling time is the same as the deposition time.
The obtained carbon black aerogel material has the height of 145mm, the whole body is in a base cylinder shape, the inner diameter is about 226mm, the outer diameter is about 270mm, and the thickness of the carbon black aerogel is 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 (density of 0.13 g/cm) with the size of 280mm multiplied by 10mm is cut 3 ) Then sewing the carbon felt by using carbon fibers to obtain a square carbon felt cylinder with the thickness of 280mm multiplied by 280mm as a deposition substrate, and placing the square carbon felt cylinder in a chemical vapor deposition furnace. Controlling the heating rate to be less than 80 ℃/min to ensure that the temperature in the furnace is raised to 980 ℃ and then carrying out heat preservation. Air is fed from the lower end of a 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 980 ℃ and 55kPaIn the meantime, propylene (purity: 99.6%) was used as a carbon source gas, and argon (purity: 99.9%) was used as a shielding gas. The volume ratio of propylene to argon is 1. And (5) after deposition treatment for 10 hours, cooling to obtain the carbon black aerogel material. The heating and cooling processes in the furnace are carried out in the argon atmosphere, and the filling time of the propylene 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 density of the carbon black aerogel to be 0.13g/cm 3 The hydrophobic angle is 148.3 degrees, the hydrophobic property is good, the compressive strength is about 1.15MPa, and the thermal conductivity at room temperature is 0.045W (m.k) -1 。
Example 5
Firstly, cut a carbon felt (density of 0.1 g/cm) with the size of about 975mm multiplied by 10mm multiplied by 300mm 3 ) Then sewing carbon felt with carbon fiber
The cylindrical carbon felt is used as a deposition substrate and is placed in a chemical vapor deposition furnace. Controlling the heating rate to be less than 80 ℃/min to ensure that the temperature in the furnace is raised to 900 ℃ and then carrying out heat preservation. 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 a temperature of 900 deg.C and a pressure of 101kPa (atmospheric pressure), using propylene (purity 99.6%) as a carbon source gas and argon (purity 99.9%) as a shielding gas. The volume ratio of propylene to argon was 3. And (4) stopping the furnace and cooling after the deposition treatment is carried out for 12 hours to obtain the carbon black aerogel material. The heating and cooling processes in the furnace are carried out in the argon atmosphere, and the filling time of the propylene is the same as the deposition time.
The obtained carbon black aerogel material has a height of 295mm, a cylindrical shape as a whole, an inner diameter of about 232mm, an outer diameter of about 300mm, and a thickness of about 34mm (overall size of about 34 mm)
) (ii) a The density of the carbon black aerogel was measured to be 0.18g/cm 3 The cross section has a characteristic band of layered deposition, 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 (density of 0.1 g/cm) with the size of 975mm multiplied by 10mm multiplied by 300mm is cut 3 ) Then sewing carbon felt with carbon fiber
The cylindrical carbon felt is used as a deposition substrate and is placed in a chemical vapor deposition furnace. Controlling the heating rate to be less than 80 ℃/min to ensure that the temperature in the furnace is raised to 1050 ℃ and then carrying out heat preservation. 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 1050 deg.c and 20kPa, using propane (99.6% purity) as the carbon source gas and nitrogen (99.9% purity) as the protective gas. The volume ratio of propane to nitrogen was 2. And (5) after deposition treatment is carried out for 2 hours, stopping the furnace and cooling to obtain the carbon black aerogel material. The temperature rise and the cooling process in the furnace are both carried out in the nitrogen atmosphere, and the filling time of the propane is the same as the deposition time.
The obtained carbon black aerogel material has soft and smooth surface gloss, the height of the material is about 293mm, the whole material is cylindrical, the inner diameter of the material is about 288mm, the outer diameter of the material is about 300mm, and the thickness of the carbon black aerogel is about 6mm; the carbon black aerogel product was removed from the inner wall of the carbon felt cylinder and measured to have a density of about 0.10g/cm 3 The hydrophobic angle is 152.6 degrees, the compressive strength is about 0.46MPa, and the thermal conductivity at room temperature is 0.036W (m.k) -1 。
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. Various changes, modifications, substitutions and alterations to these embodiments will occur to those skilled in the art without departing from the spirit and scope of the present invention.
Claims (10)
1. A preparation method of carbon black aerogel comprises the following steps:
1) Manufacturing the carbon felt into a cylindrical deposition substrate, wherein 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 putting 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 deposition is finished, cutting and stripping the cylindrical deposition substrate to obtain the carbon black aerogel.
2. The method for preparing carbon black aerogel according to claim 1, wherein in the step 1), the carbon felt is at least one of short fiber carbon felt, needle felt and three-dimensional piercing 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 cuboid or cylindrical deposition substrate.
3. The method for preparing carbon black aerogel according to claim 1, wherein in the step 1), the cover plate is at least one of carbon felt, graphite plate and quartz plate; the total area of the air outlet is not more than 8mm 2 。
4. The method for preparing carbon black aerogel according to claim 1, wherein in the step 2), 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.
5. The method for preparing carbon black aerogel according to claim 1, wherein in the step 2), the chemical vapor deposition adopts a fluidized bed chemical vapor deposition method, and the carbon black particles exhibit flow properties similar to those of a fluid under the action of a gas flow during the deposition process; the volume ratio of the carbon source gas to the protective gas is 1-3; the process conditions of the chemical vapor deposition are as follows: the temperature is 900-1150 ℃, the pressure is 20-101 kPa, and the deposition time is 2-12 h.
6. The preparation method of the carbon black aerogel according to claim 1, wherein in the step 2), the furnace body of the chemical vapor deposition furnace comprises a cooling water inlet 2, a cooling water outlet 5, an air inlet 1 and a tail gas outlet 7 which are arranged in the furnace body, a reaction chamber which is arranged in the furnace body and is formed by enclosing a heat-insulating felt 4, an electrified copper coil 3 which is arranged around the heat-insulating felt, a soft thermocouple 12 for detecting the temperature in the reaction chamber, a graphite support frame tool 10 which is arranged in the reaction chamber, a support plate tool 9 which is arranged opposite to the support frame, an air inlet pipe 11 which sequentially penetrates through the bottom wall of the furnace body, the bottom wall of the heat-insulating felt, the support frame tool 10 and the support plate tool 9, a cylindrical substrate 8 which is arranged on the support plate tool 9, and the upper end of the cylindrical substrate 8 is sealed by a cover plate 6; carbon source gas and protective gas enter an area formed by surrounding the cylindrical substrate 8, the support plate tool 9 and the cover plate 6 through the gas inlet pipe 11, and then flow around in a cavity of the cylindrical substrate, so that reaction gas is in full contact with the carbon felt substrate for deposition.
7. A carbon black aerogel produced by the production method according to any one of claims 1 to 6.
8. The carbon black aerogel according to claim 7, wherein the carbon black aerogel is formed by stacking and depositing the carbon black particles layer by layer after forming a branched chain structure; the particle size of the carbon black particles in the carbon black aerogel is 50-500 nm.
9. The carbon black aerogel according to claim 7, wherein the density of the carbon black aerogel is 0.1 to 0.2g/cm 3 。
10. The carbon black aerogel according to claim 7, wherein the hydrophobic angle of the carbon black aerogel is 130 ° to 160 °.
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Application publication date: 20221011 |