CN111908464B - Method for preparing foam carbon material by using tannic acid - Google Patents
Method for preparing foam carbon material by using tannic acid Download PDFInfo
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- CN111908464B CN111908464B CN202010667316.1A CN202010667316A CN111908464B CN 111908464 B CN111908464 B CN 111908464B CN 202010667316 A CN202010667316 A CN 202010667316A CN 111908464 B CN111908464 B CN 111908464B
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- tannic acid
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- urotropine
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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
- C01B32/318—Preparation characterised by the starting materials
Abstract
The invention provides a method for preparing a carbon foam material by using tannic acid, which relates to the technical field of carbon foam material preparation and obtains the carbon material by directly carbonizing and activating an organic carbon source.
Description
Technical Field
The invention provides a method for preparing a carbon foam material by using tannic acid, and relates to the technical field of carbon foam material preparation.
Background
As a porous carbon, the foam carbon is widely focused due to the advantages of abundant pore structure, huge specific surface, stable physicochemical properties and the like, is widely researched and applied to a plurality of fields such as adsorption, catalysis, energy storage, filtration and the like, and has wide market demands.
At present, a template is mostly used for loading in the process of preparing the carbon material, and the carbon source is loaded on the template after being processed and carbonized through selecting the carbon source and the template. In general, the template method is used for preparing the carbon material, acid liquor or alkali liquor is required to be cleaned, the operation is complex, environmental pollution is easy to cause, and the selected template cannot be recovered, the cost is high, and a large number of production cannot be performed, so that a novel efficient and low-cost preparation method for producing the porous carbon is necessary to be developed.
Disclosure of Invention
The invention provides a method for preparing a foam carbon material by using tannic acid, which solves the technical problems of complex operation and high cost in the prior art of a porous carbon preparation method.
The invention is realized in the following way: the method comprises the following steps:
(1) Mixing tannic acid, urotropine and distilled water according to the mass ratio of 1:0.4-1:4, and magnetically stirring until the tannic acid, urotropine and distilled water are fully dissolved;
(2) Placing the solution obtained in the step (1) into a surface dish for pre-freezing treatment, and freeze-drying after the pre-freezing is carried out until the sample is completely solidified;
(3) Collecting the freeze-dried sample obtained in the step (2), placing the freeze-dried sample into a surface dish, placing the surface dish into a muffle furnace for pretreatment of carbon materials, heating to 200 ℃ at a heating rate of 2 ℃ per minute, preserving heat for 1 hour, continuously heating to 250 ℃ at the heating rate of 2 ℃ per minute, preserving heat for 1 hour, and then cooling;
(4) And (3) placing the pretreated carbon material in the step (3) into a quartz boat, placing the quartz boat into a tube furnace for further carbonization, heating to 900 ℃ at a heating rate of 2 ℃ per minute, keeping the temperature for one hour, cooling, and keeping the nitrogen atmosphere in the carbonization process.
Further preferably, in the step (1), the temperature at which the tannic acid, urotropine and distilled water are mixed and dissolved is 22 ℃.
As a further preferred aspect, in step (1), the mass ratio of tannic acid, urotropine and distilled water is 1:1:4.
As a further preference, the lyophilization time in step (2) is 8 hours.
As a further preferred, the pre-freezing treatment condition in the step (2) is a cold trap temperature of-60 ℃ for 2 hours.
As a further preference, in step (4), the nitrogen flow is 100ml/min.
The invention has the beneficial effects that: the invention obtains the carbon material by directly carbonizing and activating the organic carbon source, reduces the production cost, and has the advantages of short preparation time, easy control of reaction, large specific surface area of the product and the like. Too high room temperature can cause insufficient mixing of tannic acid and urotropine, so that layering phenomenon of the solution can occur, and freeze drying can not be performed, and therefore, the mixing temperature of tannic acid, urotropine and distilled water is limited to be 22 ℃. The surface dish is selected as a pretreatment container, so that the contact between the sample and the air is ensured to the greatest extent during pretreatment.
Drawings
FIG. 1 is a graph showing the desorption of nitrogen from carbon foam prepared in example 1;
FIG. 2 is a graph showing pore size distribution of the carbon foam prepared in example 1;
FIG. 3 is a SEM image of the carbon foam prepared in example 1.
Detailed Description
Embodiments of the present invention will now be described more fully hereinafter with reference to the accompanying drawings, in which it is shown, however, that the embodiments shown are only some, and not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) Weighing 5g of tannic acid and 2g of urotropine, sequentially adding into 20ml of distilled water, and magnetically stirring to fully dissolve the tannic acid and the urotropine.
(2) The obtained solution is introduced into a surface dish, pre-freezing treatment is carried out at the temperature of a cold trap of about-60 ℃, freeze-drying treatment is carried out after the solution is completely solidified for about 2 hours, and a vacuum pump of a vacuum gauge is sequentially started for about 8 hours.
(3) Taking out the freeze-dried sample, weighing 3g, and carrying out carbon material pretreatment. Placing the freeze-dried sample into a surface dish, placing the surface dish into a muffle furnace, heating to 200 ℃ at a heating rate of 2 ℃ per minute, and preserving heat for 2 hours; continuously heating to 250 ℃ at the heating rate of 2 ℃ per minute, preserving heat for 1 hour, completing the reaction, and carrying out cooling treatment.
(4) And (3) placing the obtained pretreatment sample into a quartz boat, and placing the quartz boat into a tube furnace for further carbonization treatment. And heating to 900 ℃ at a heating rate of 2 ℃ per minute by nitrogen with a flow rate of 100ml/min, preserving heat for 1 hour, completing the reaction, and performing cooling treatment to obtain the porous foam carbon material.
The obtained porous foam carbon material is subjected to a nitrogen desorption experiment, and the graph is shown in fig. 1. The pore size distribution of the carbon material is shown in figure 2, and the electron microscope is shown in figure 3.
Example 2
(1) Weighing 5g of tannic acid and 3g of urotropine, sequentially adding into 20ml of distilled water, and magnetically stirring to fully dissolve the tannic acid and the urotropine.
(2) The obtained solution is introduced into a surface dish, pre-freezing treatment is carried out at the temperature of a cold trap of about-60 ℃, freeze-drying treatment is carried out after the solution is completely solidified for about 2 hours, and a vacuum pump of a vacuum gauge is sequentially started for about 8 hours.
(3) Taking out the freeze-dried sample, weighing 3g, and carrying out carbon material pretreatment. Placing the freeze-dried sample into a surface dish, placing the surface dish into a muffle furnace, heating to 200 ℃ at a heating rate of 2 ℃ per minute, and preserving heat for 2 hours; continuously heating to 250 ℃ at the heating rate of 2 ℃ per minute, preserving heat for 1 hour, completing the reaction, and carrying out cooling treatment.
(4) And (3) placing the obtained pretreatment sample into a quartz boat, and placing the quartz boat into a tube furnace for further carbonization treatment. And heating to 900 ℃ at a heating rate of 2 ℃ per minute by nitrogen with a flow rate of 100ml/min, preserving heat for 1 hour, completing the reaction, and performing cooling treatment to obtain the porous foam carbon material.
Example 3
(1) Weighing 5g of tannic acid and 4g of urotropine, sequentially adding into 20ml of distilled water, and magnetically stirring to fully dissolve the tannic acid and the urotropine.
(2) The obtained solution is introduced into a surface dish, pre-freezing treatment is carried out at the temperature of a cold trap of about-60 ℃, freeze-drying treatment is carried out after the solution is completely solidified for about 2 hours, and a vacuum pump of a vacuum gauge is sequentially started for about 8 hours.
(3) Taking out the freeze-dried sample, weighing 3g, and carrying out carbon material pretreatment. Placing the freeze-dried sample into a surface dish, placing the surface dish into a muffle furnace, heating to 200 ℃ at a heating rate of 2 ℃ per minute, and preserving heat for 2 hours; continuously heating to 250 ℃ at the heating rate of 2 ℃ per minute, preserving heat for 1 hour, completing the reaction, and carrying out cooling treatment.
(4) And (3) placing the obtained pretreatment sample into a quartz boat, and placing the quartz boat into a tube furnace for further carbonization treatment. And heating to 900 ℃ at a heating rate of 2 ℃ per minute by nitrogen with a flow rate of 100ml/min, preserving heat for 1 hour, completing the reaction, and performing cooling treatment to obtain the porous foam carbon material.
Example 4
(1) Weighing 5g of tannic acid and 5g of urotropine, sequentially adding into 20ml of distilled water, and magnetically stirring to fully dissolve the tannic acid and urotropine.
(2) The obtained solution is introduced into a surface dish, pre-freezing treatment is carried out at the temperature of a cold trap of about-60 ℃, freeze-drying treatment is carried out after the solution is completely solidified for about 2 hours, and a vacuum pump of a vacuum gauge is sequentially started for about 8 hours.
(3) Taking out the freeze-dried sample, weighing 3g, and carrying out carbon material pretreatment. Placing the freeze-dried sample into a surface dish, placing the surface dish into a muffle furnace, heating to 200 ℃ at a heating rate of 2 ℃ per minute, and preserving heat for 2 hours; continuously heating to 250 ℃ at the heating rate of 2 ℃ per minute, preserving heat for 1 hour, completing the reaction, and carrying out cooling treatment.
(4) And (3) placing the obtained pretreatment sample into a quartz boat, and placing the quartz boat into a tube furnace for further carbonization treatment. And heating to 900 ℃ at a heating rate of 2 ℃ per minute by nitrogen with a flow rate of 100ml/min, preserving heat for 1 hour, completing the reaction, and performing cooling treatment to obtain the porous foam carbon material.
The specific surface area and pore size distribution of the sample were measured by a BET specific surface area analyzer, and the pore volume, specific surface area and average pore diameter of the porous carbon materials prepared in examples 1 to 4 are shown in table 1.
TABLE 1 specific surface area and pore size distribution of porous carbon materials prepared in examples 1 to 4
The invention has the beneficial effects that: the invention obtains the carbon material by directly carbonizing and activating the organic carbon source, reduces the production cost, and has the advantages of short preparation time, easy control of reaction, large specific surface area of the product and the like. Too high room temperature can cause insufficient mixing of tannic acid and urotropine, so that layering phenomenon of the solution can occur, and freeze drying can not be performed, and therefore, the mixing temperature of tannic acid, urotropine and distilled water is limited to be 22 ℃. The surface dish is selected as a pretreatment container, so that the contact between the sample and the air is ensured to the greatest extent during pretreatment.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (4)
1. A method for preparing a carbon foam material by using tannic acid, which is characterized by comprising the following steps:
(1) Mixing tannic acid, urotropine and distilled water according to the mass ratio of 1:0.4-1:4, and magnetically stirring until the tannic acid, urotropine and distilled water are fully dissolved;
(2) Placing the solution obtained in the step (1) into a surface dish for pre-freezing treatment, and freeze-drying after the pre-freezing is carried out until the sample is completely solidified;
(3) Collecting the freeze-dried sample obtained in the step (2), placing the freeze-dried sample into a surface dish, placing the surface dish into a muffle furnace for pretreatment of carbon materials, heating to 200 ℃ at a heating rate of 2 ℃ per minute, preserving heat for 1 hour, continuously heating to 250 ℃ at the heating rate of 2 ℃ per minute, preserving heat for 1 hour, and then cooling;
(4) Placing the pretreated carbon material in the step (3) into a quartz boat, placing the quartz boat into a tube furnace for further carbonization, heating to 900 ℃ at a heating rate of 2 ℃ per minute, keeping the temperature for one hour, cooling, and keeping the nitrogen atmosphere in the carbonization process;
in the step (1), the temperature of the mixed and dissolved tannic acid, urotropine and distilled water is 22 ℃;
the pre-freezing treatment condition in the step (2) is that the cold trap temperature is-60 ℃ and 2 hours.
2. The method for preparing a carbon foam material using tannic acid according to claim 1, wherein in the step (1), the mass ratio of tannic acid, urotropine and distilled water is 1:1:4.
3. The method for preparing a carbon foam using tannic acid according to claim 1, wherein the lyophilization time in step (2) is 8 hours.
4. The method for producing a carbon foam using tannic acid according to claim 1, wherein in the step (4), the nitrogen flow rate is 100ml/min.
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