CN109437147B - Preparation method of multifunctional carbon foam - Google Patents
Preparation method of multifunctional carbon foam Download PDFInfo
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- CN109437147B CN109437147B CN201811288266.5A CN201811288266A CN109437147B CN 109437147 B CN109437147 B CN 109437147B CN 201811288266 A CN201811288266 A CN 201811288266A CN 109437147 B CN109437147 B CN 109437147B
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- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
The invention discloses a preparation method of multifunctional carbon foam, and belongs to the technical field of carbon foam preparation. The preparation method of the multifunctional carbon foam comprises the following steps: soaking the polymer foam material in a cellulose solution, washing, drying and carbonizing to prepare multifunctional carbon foam; or soaking the polymer foam material in the mixed solution of the cellulose solution and the metal salt, soaking in an alkali solution, washing, drying, and carbonizing to obtain the multifunctional carbon foam; wherein the metal salt includes one or more combinations of nickel, iron, aluminum, copper, cobalt, manganese, rubidium, and vanadium salts. The preparation method has the advantages of simple process, wide raw material source and low production cost, can realize the control of the surface wettability of the carbon foam, and meets different requirements.
Description
Technical Field
The invention relates to the technical field of carbon foam preparation, in particular to a preparation method of multifunctional carbon foam.
Background
The carbon material is a material which is quite common in daily production, life and research, and comprises activated carbon, biomass carbon, carbon black, graphene, carbon nano tubes, carbon foam and the like. Among these types of carbon materials, carbon foams have been the focus of scientific research in recent years due to their advantages such as low density, high specific surface area, interconnected pore network structure, and compressibility. Especially, the interconnected pore network layer structure is beneficial to the diffusion and storage of ions and molecules, so that the carbon foam material is widely applied to the fields of adsorption, energy storage, sensors, catalyst carriers and the like.
The preparation method of the carbon foam mainly comprises the following steps: chemical Vapor Deposition (CVD), hydrothermal, drop coating, and carbonized polymer foam processes. Other foams are taken as templates, and carbon nanotubes grow on the surface of the template by a vapor deposition method, so that carbon nanotube foam can be prepared; or reduced graphene oxide foam can be prepared by hydrothermally treating the graphene oxide dispersion. Although the obtained carbon nanotube foam or reduced graphene oxide foam has good performance, the preparation methods have strict process requirements, high production cost and low yield, so that large-scale production and industrial application cannot be realized.
For the application of carbon foam, in addition to the characteristics of interconnected porous structure and high surface area, the hydrophilicity and hydrophobicity of the material surface are important factors. Different application areas have different wettability requirements for the carbon foam surface. Fields such as organic solvent adsorption and oil-water separation often require carbon foams to have hydrophobic surface properties; carbon foams are often required to have hydrophilic surface properties as catalytic supports or as energy storage materials. Because the carbon foam prepared by the previous method has poor surface wettability and cannot be regulated, the carbon foam prepared by the same method cannot meet the application requirements of multiple fields. Meanwhile, the carbon material prepared by carbonization often cannot reach the degree of super-hydrophobicity or super-hydrophilicity, and further modification is needed to improve the performance. Therefore, it is necessary to develop a new simple method for preparing a multifunctional carbon foam material, and the adjustment of the surface wettability of the carbon foam material and even the adjustment between super-hydrophobic/super-hydrophilic properties can be realized through simple experimental condition adjustment. Not only can improve the performance of the carbon foam, but also can meet the surface characteristic requirements of different application fields.
Disclosure of Invention
The invention aims to provide a preparation method of multifunctional carbon foam, and aims to solve the problems that the existing carbon foam preparation process is complex, the production cost is high, the surface wettability of the carbon foam is poor, the carbon foam cannot be regulated and controlled, and the carbon foam is difficult to be simultaneously applied to different fields.
The technical scheme for solving the technical problems is as follows:
a method of preparing a multifunctional carbon foam, comprising:
soaking the polymer foam material in a cellulose solution, washing, drying and carbonizing to prepare multifunctional carbon foam; or
Soaking a polymer foam material in the mixed solution of the cellulose solution and the metal salt, soaking in an alkali solution, washing, drying, and carbonizing to obtain multifunctional carbon foam;
wherein the metal salt includes one or more combinations of nickel, iron, aluminum, copper, cobalt, manganese, rubidium, and vanadium salts.
The method comprises the steps of soaking a polymer foam material in a cellulose solution, covering the cellulose solution on a polymer foam framework with a layer of regenerated cellulose film, carbonizing the polymer foam at high temperature to obtain carbon foam, and carbonizing the regenerated cellulose film to obtain a carbon film, wherein the carbon film is composed of nano fibers and is in a porous network structure. The carbon foam material has certain hydrophobicity, and the carbon film with the porous network structure on the surface of the carbon foam material improves the roughness of the surface of the carbon foam, so that the hydrophobicity of the carbon foam is improved.
The invention soaks the polymer foam material in the mixed solution of the cellulose solution and the metal salt, at this time, a layer of regenerated cellulose film containing the metal salt is covered on the polymer foam framework, then soaks into the alkali solution, the metal salt in the mixed solution is converted into corresponding hydroxide, after washing and drying, the high temperature carbonization is carried out, the polymer foam is carbonized to obtain carbon foam, the cellulose film is carbonized to obtain the carbon film, and the hydroxide corresponding to the metal salt is carbonized to form the oxide corresponding to the metal salt. The oxide corresponding to the metal salt has good contact with the carbon skeleton, and the roughness of the surface of the carbon foam is improved due to the hydrophilicity of the oxide, so that the hydrophilicity of the carbon foam is improved.
Further, in a preferred embodiment of the present invention, the metal salt is a nickel salt.
The invention soaks the polymer foam material in the mixed solution of the cellulose solution and nickel salt, at this time, a layer of regenerated cellulose film containing nickel salt is covered on the polymer foam framework, then soaks into the alkali solution, the metal salt in the mixed solution is converted into nickel hydroxide, after washing and drying, high temperature carbonization is carried out, the polymer foam is carbonized to obtain carbon foam, the cellulose film is carbonized to obtain carbon film, and the nickel hydroxide is carbonized to obtain nickel oxide. The electron microscope test shows that the NiO nanorods with the shape of the needle mushroom are uniformly distributed on the skeleton length of the carbon foam and have good contact with the carbon skeleton. Because NiO is hydrophilic, the NiO nanorod improves the roughness of the surface of the carbon foam, and the hydrophilicity of the carbon foam is further improved.
Further, in a preferred embodiment of the present invention, the cellulose solution is prepared by sequentially soaking cellulose in water, methanol and a dimethylacetamide solution, and dissolving the soaked cellulose in a dimethylacetamide/lithium chloride solvent system.
Further, in a preferred embodiment of the present invention, the concentration of the cellulose solution is 0.05-2%, and the amount of the nickel salt added is 0.05-5% of the cellulose solution.
According to the invention, when the polymer foam is soaked in the cellulose solution with the concentration, the water contact angle of the obtained carbon foam can reach 162 degrees through a water contact angle test, and the carbon foam is immersed in water under the action of external force, so that the surface of the carbon foam presents a silver mirror phenomenon, and the carbon foam prepared by the method has the super-hydrophobic surface characteristic under the condition.
When polymer foam is soaked in the mixed solution of the cellulose solution and the nickel salt, the mixed solution is soaked in an alkali solution, and finally the obtained carbon foam is carbonized, in a water contact angle test, the water contact angle of the hybrid carbon foam is 0 degrees, and after a test water drop is contacted with the surface of the foam, the carbon foam can be absorbed by the foam within a very short time (0.087s), and under the condition, the carbon foam prepared by the method has super-hydrophilic surface characteristics.
In the invention, when the concentration of the cellulose solution is higher, the carbon film on the surface of the finally generated carbon foam is thicker, so that the roughness of the surface of the carbon foam is higher, the hydrophobicity of the finally generated carbon foam is increased along with the increase of the concentration of the cellulose solution, and finally the super-hydrophobic carbon foam is obtained. And when the concentration of the added nickel salt is higher, the NiO nanorods with the shape of the needle mushroom in the finally generated carbon foam are more, so that the hydrophilicity of the finally generated carbon foam is increased along with the increase of the concentration of the nickel salt, and finally the super-hydrophilic carbon foam is obtained. By adjusting the addition amount of the cellulose solution and the nickel salt, the surface hydrophilicity and hydrophobicity of the carbon foam obtained by final carbonization can be regulated, and the superhydrophobicity or superhydrophobicity of the carbon foam can also be regulated so as to meet different application fields.
Further, in a preferred embodiment of the present invention, the carbonization conditions are: carbonizing at the temperature of 500-1800 ℃ for 1-3h under the protection of inert gas.
Further, in a preferred embodiment of the present invention, the cellulose source includes cotton, wood, bamboo, paper, hemp, waste cotton fiber, straw, reed rhizome.
Further, in a preferred embodiment of the present invention, the polymer foam is one of melamine foam, polyurethane foam, polystyrene foam, and polyethylene foam.
Further, in a preferred embodiment of the present invention, the alkali solution includes one or more of a combination of sodium hydroxide solution, potassium hydroxide solution and ammonia water.
Further, in a preferred embodiment of the present invention, the nickel salt includes one or more of nickel chloride, nickel sulfate, nickel nitrate, nickel acetate and nickel carbonate.
The invention has the following beneficial effects:
1. the preparation method has the advantages of simple process, wide raw material source and low production cost, and can realize large-scale production and industrial application.
2. The preparation method can realize the control of the surface wettability of the carbon foam so as to prepare the super-hydrophobic or super-hydrophilic carbon foam and meet different application requirements.
3. The super-hydrophobic carbon foam prepared by the invention has excellent oil absorption performance and excellent reusability, and can be regenerated in various modes such as distillation, extrusion, combustion and the like.
4. The hydrophobic carbon foam prepared by the method has super-hydrophobicity, and can continuously clean and collect oil stains without the assistance of any external equipment.
5. The hydrophilic carbon foam prepared by the invention has higher porosity and specific surface area, which is beneficial to the diffusion and transfer of electrolyte, and meanwhile, the generation of the NiO nano rod with the shape of needle mushroom reduces the charge transfer resistance, so that the hydrophilic carbon foam has excellent mechanical property and conductivity.
6. The hydrophilic carbon foam prepared by the invention has excellent energy storage performance because the metal oxide NiO has pseudo capacitance.
Drawings
FIG. 1 is an electron micrograph and a hydrophobicity test micrograph of a CCF of the present invention;
wherein a is a scanning electron microscope photo of CCF and a water contact angle photo of CCF; b is a photograph of a hydrophobicity test of CCF; CCF is the carbon foam obtained in example 3;
FIG. 2 is a CCF and CF adsorption performance test chart and a CCF continuous oil-water separation experimental chart of the present invention;
wherein, a is a comparison graph of the absorption performance of organic solvents and oil of CCF and CF, and b is a CCF continuous oil-water separation experimental graph; CCF is the carbon foam obtained in example 3, and CF is the carbon foam obtained by carbonizing pure melamine foam;
FIG. 3 is a scanning electron micrograph and water contact angle test of NiO @ CCF of the present invention;
wherein a is a scanning electron microscope image of NiO @ CCF, and b is a water contact angle test image of NiO @ CCF; NiO @ CCF is the hybrid carbon foam obtained in example 5.
Detailed Description
The principles and features of this invention are described below in conjunction with embodiments, which are included to explain the invention and not to limit the scope of the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that:
in the specific embodiment of the invention, the solvent system of dimethylacetamide/lithium chloride is prepared by mixing dimethylacetamide and lithium chloride in a mass ratio of 92: 8; the nickel salt is preferably nickel chloride; the addition amount of the alkali solution is more than 10 times of the addition amount of the cellulose solution.
Example 1:
this example is a hydrophobic carbon foam prepared by soaking a polymer foam in a 0.05% strength cellulose solution.
The method for preparing the multifunctional carbon foam of the embodiment comprises the following steps: sequentially soaking cotton in water, methanol and a dimethylacetamide solution, and dissolving the soaked cellulose in a dimethylacetamide/lithium chloride solvent system to obtain a 0.05% cellulose solution;
soaking polystyrene foam in a cellulose solution, washing, drying, and carbonizing at 500 ℃ for 3h under the protection of inert gas to obtain the polystyrene foam.
The carbon foam obtained was subjected to a water contact angle test, and the water contact angle of the carbon foam was 130 ° by the test, indicating that the carbon foam obtained in this example was hydrophobic.
Example 2:
in this example, a superhydrophobic carbon foam was prepared by soaking a polymer foam into a 1% strength cellulose solution.
The preparation method of the multifunctional carbon foam of the present example comprises: sequentially soaking paper in water, methanol and a dimethylacetamide solution, and dissolving the soaked cellulose in a dimethylacetamide/lithium chloride solvent system to prepare a 1% cellulose solution;
and (2) soaking the polyurethane foam in a cellulose solution, washing and drying, and carbonizing at 800 ℃ for 2 hours under the protection of inert gas to obtain the carbon foam.
The resulting carbon foam was subjected to a water contact angle test, which indicated that the carbon foam produced in this example was superhydrophobic by testing the carbon foam at a water contact angle of 157 °.
Example 3:
this example is a superhydrophobic carbon foam prepared by soaking a polymer foam into a 2% strength cellulose solution.
The preparation method of the multifunctional carbon foam of the present example comprises: sequentially soaking bagasse in water, methanol and a dimethyl acetamide solution, and dissolving the soaked cellulose in a dimethyl acetamide/lithium chloride solvent system to prepare a 2% cellulose solution;
and (2) soaking the melamine foam in a cellulose solution, washing and drying, and then carbonizing at 1800 ℃ for 1h under the protection of inert gas to obtain the carbon foam.
Specifically, the carbon foam obtained by carbonizing a pure melamine foam is labeled CF, and the carbon foam obtained in example 3 is labeled CCF.
And performing electron microscope scanning and hydrophobicity test on the CCF to obtain a scanning electron microscope photo and a hydrophobicity test photo of the CCF, which are shown in figure 1. Wherein in FIG. 1, a is a scanning electron micrograph of CCF, and a water contact angle micrograph of CCF; b is a photograph of a hydrophobicity test of CCF.
It can be seen from fig. 1a that a small portion of the carbon foam pores in the CCF are plugged, but a large portion of the pores remain. After amplification, the foam skeleton was found to be covered with a layer of porous material, which is a carbon layer converted from the regenerated cellulose film covered by the foam skeleton under high temperature conditions. The water contact angle test finds that the obtained carbon foam has a water contact angle of 162 degrees and shows super-hydrophobic property. As can be seen in fig. 1b, the carbon foam can float completely on the water surface, indicating that the carbon foam is not only hydrophobic, but also has a very low density. The carbon foam is immersed in water under the action of external force, and the silver mirror phenomenon is found on the surface of the carbon foam, so that the super-hydrophobic characteristic of the carbon foam is further proved.
The CCF and CF were tested for their adsorption properties with respect to different organic solvents and oils and the CCF was subjected to a continuous oil-water separation experiment to obtain the experimental results of fig. 2. In FIG. 2, a is a comparison graph of absorption performance of CCF and CF on different organic solvents and oils, and b is a CCF continuous oil-water separation experimental graph.
As shown in fig. 2a, after soaking in the cellulose solution, the adsorption performance of CCF to various organic solvents and oils is greatly improved. Wherein, the absorption performance of CCF to organic solvents such as n-hexane, paraffin oil and the like reaches 80 to 170 times of the self weight. After the organic solvent is adsorbed, the carbon foam can be desorbed by various methods such as combustion, extrusion, distillation and the like, and has excellent repeated use performance. Figure 2b shows a plastic hose cut and inserted with one end into the CCF, which is automatically absorbed when it comes into contact with the oil layer and is continuously transferred to another clean container until the oil layer is cleaned. It should be noted here that the continuous oil-water separation experiment is driven by surface tension and gravity, and has no external force or external equipment.
Example 4:
in the mixed solution of the cellulose solution and the nickel salt in this example, the concentration of the cellulose solution was 1%, and the amount of the nickel salt added was 0.05% of the cellulose solution, and the carbon foam was changed in hydrophobicity by adding nickel chloride to the cellulose solution to prepare a hybrid carbon foam.
The preparation method of the multifunctional carbon foam of the present example comprises: sequentially soaking cotton in water, methanol and a dimethylacetamide solution, dissolving the soaked cellulose in a dimethylacetamide/lithium chloride solvent system to obtain a 1% cellulose solution, adding nickel chloride into the cellulose solution, wherein the addition amount of the nickel chloride is 0.05% of the cellulose solution, and stirring until the nickel chloride and the cellulose solution are uniformly mixed to obtain a mixed solution;
and (2) soaking the melamine foam in the mixed solution, taking out the melamine foam, immediately soaking the melamine foam in an alkaline solution of sodium hydroxide, washing and drying the melamine foam, and carbonizing the melamine foam for 3 hours at the temperature of 500 ℃ under the protection of inert gas to obtain the carbon foam.
The resulting hybrid carbon foam was subjected to a water contact angle test, which indicated that the carbon foam had a water contact angle of 50 °, indicating that the carbon foam prepared in this example was hydrophilic.
Example 5:
in the mixed solution of cellulose and nickel chloride in the embodiment, the concentration of the cellulose solution is 1%, and the addition amount of the nickel chloride is 1% of the cellulose solution, and the super-hydrophilic hybrid carbon foam is prepared by adding the nickel chloride into the cellulose solution to change the hydrophobicity of the carbon foam.
The preparation method of the multifunctional carbon foam of the present example comprises: sequentially soaking cotton in water, methanol and a dimethylacetamide solution, putting the soaked cellulose into a dimethylacetamide/lithium chloride solvent system for dissolving to obtain a 1% cellulose solution, adding nickel chloride into the cellulose solution, wherein the addition amount of the nickel chloride is 1% of the cellulose solution, and stirring until the nickel chloride and the cellulose solution are uniformly mixed to obtain a mixed solution;
and (2) soaking the melamine foam in the mixed solution for 60min, taking out the melamine foam, immediately soaking the melamine foam in an alkaline solution of potassium hydroxide, washing and drying the melamine foam, and carbonizing the melamine foam at 800 ℃ for 2h under the protection of inert gas to obtain the multifunctional carbon foam.
Specifically, the hybrid carbon foam obtained in example 5 was labeled as NiO @ CCF.
And performing electron microscope scanning and water contact angle testing on the NiO @ CCF to obtain a scanning electron microscope image and a water contact angle test image of the NiO @ CCF, which are shown in figure 3. In FIG. 3, a is a scanning electron micrograph of NiO @ CCF, and b is a water contact angle test chart of NiO @ CCF.
As can be seen from the electron microscope scan of fig. 3a, the framework length of the hybrid carbon foam has uniformly distributed nanorods, which is NiO generated in situ by nickel hydroxide during carbonization. After further amplification, the nanorods are found to have the appearance similar to that of flammulina velutipes. In the water contact angle test, the water contact angle of the hybrid carbon foam was 0 °. And when the test water drop contacts the foam surface, the test water drop is absorbed by the foam in a very short time (0.087s), which shows that the hybrid carbon foam has super-hydrophilic surface characteristics.
The hybrid carbon foam has excellent electrochemical performance, the specific capacitance reaches 400F/g, and the carbon foam has excellent mechanical properties, so that the stored energy of the carbon foam is hardly influenced under the conditions of compression and bending, and the hybrid carbon foam has wide application prospects in the fields of flexible electronic devices and wearable equipment.
Example 6:
in the mixed solution of cellulose and nickel chloride in the embodiment, the concentration of the cellulose solution is 1%, and the addition amount of the nickel chloride is 5% of the cellulose solution, and the super-hydrophilic hybrid carbon foam is prepared by adding the nickel chloride into the cellulose solution to change the hydrophobicity of the carbon foam.
The preparation method of the multifunctional carbon foam of the present example comprises: sequentially soaking cotton in water, methanol and a dimethylacetamide solution, putting the soaked cellulose into a dimethylacetamide/lithium chloride solvent system for dissolving to obtain a 1% cellulose solution, adding nickel chloride into the cellulose solution, wherein the addition amount of the nickel chloride is 5% of that of the cellulose solution, and stirring until the nickel chloride and the cellulose solution are uniformly mixed to obtain a mixed solution;
and (3) placing the polyethylene foam into the mixed solution, soaking for 120min, taking out, immediately soaking into an aqueous alkali of ammonia, washing, drying, and carbonizing at 1800 ℃ for 1h under the protection of inert gas to obtain the multifunctional carbon foam.
The resulting carbon foam was subjected to a water contact angle test by which the carbon foam water contact angle was 0 °. The specific capacitance of the hybrid carbon foam reached 372.75F/g.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A method of making a multifunctional carbon foam, comprising:
soaking a polymer foam material in a mixed solution of a cellulose solution and a nickel salt, soaking in an alkali solution, washing and drying, and carbonizing at the temperature of 500-1800 ℃ for 1-3h under the protection of inert gas to prepare multifunctional carbon foam; wherein the concentration of the cellulose solution is 0.05-2%, and the addition amount of the nickel salt is 0.05-5% of the cellulose solution.
2. The method of claim 1, wherein the cellulose solution is prepared by sequentially soaking cellulose in water, methanol and a dimethylacetamide solution, and dissolving the soaked cellulose in a dimethylacetamide/lithium chloride solvent system.
3. The method of claim 1, wherein the polymer foam is one of melamine foam, polyurethane foam, polystyrene foam, and polyethylene foam.
4. The method of claim 1, wherein the alkali solution comprises one or more of a combination of sodium hydroxide solution, potassium hydroxide solution and ammonia water.
5. The method of claim 1, wherein the nickel salt comprises one or more of nickel chloride, nickel sulfate, nickel nitrate, nickel acetate, and nickel carbonate.
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| CN110467228A (en) * | 2019-09-16 | 2019-11-19 | 西北师范大学 | A kind of preparation method of doughnut structure C-Ni/NiO nanocomposite |
| CN111261431B (en) * | 2020-02-28 | 2022-07-19 | 上海应用技术大学 | Preparation method of nano cobaltosic oxide/nitrogen-doped three-dimensional porous carbon skeleton composite material for super capacitor |
| CN111799099A (en) * | 2020-07-21 | 2020-10-20 | 厦门理工学院 | Composite electrode material taking needle mushroom as carbon-based load and preparation method and application thereof |
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