KR20230173530A - Method for preparing mesoporous carbon and mesoporous carbon prepared thereby - Google Patents

Abstract

Preparing a solution containing silver oxide (Ag ₂ O), mixing the solution containing silver oxide with acetylene (C ₂ H ₂ ) gas to form silver acetylide (Ag ₂ C ₂ ), and silver acetylide It provides a method for producing mesoporous carbon, which includes forming carbon containing mesopores by heating and extruding silver (Ag).

Description

Method for producing mesoporous carbon and mesoporous carbon produced thereby {METHOD FOR PREPARING MESOPOROUS CARBON AND MESOPOROUS CARBON PREPARED THEREBY}

The present invention relates to a method for producing mesoporous carbon containing mesopores and mesoporous carbon produced thereby.

A polymer electrolyte membrane fuel cell (PEMFC) uses hydrogen as fuel for the anode and air as fuel for the cathode to electrochemically generate water. Electrons move from the anode to the cathode through an electrical load, and at the cathode, oxygen combines with electrons and hydrogen cations generated from hydrogen as shown in the equation below and is reduced to produce water. The total chemical potential difference is 1.23 V under standard conditions, which is the voltage of the single cell, as shown in the equation below.

Anode: H ₂ → 2H ⁺ + 2e ^- , E _o = 0.00 V

Cathode: 1/2O ₂ + 2H ⁺ + 2e ^- → H ₂ O, E _o = 1.23 V

Total: H ₂ + 1/2O ₂ → H ₂ O, E _o = 1.23 V

To date, platinum catalysts supported on carbon are mainly used as electrode catalysts for PEMFC. Carbon carriers used in electrocatalysts generally have a high specific surface area to improve the supporting density of catalyst particles.

For example, Patent Document 1 includes a catalyst, a porous carrier supporting the catalyst, and a polymer electrolyte, the average particle diameter of the porous carrier is 20 nm to 100 nm, and the porous carrier has a pore volume with a pore diameter of 4 nm to 20 nm. An electrode catalyst layer for a fuel cell having a mode diameter of pore distribution of a porous carrier of 0.23 cm ³ /g to 0.78 cm ³ /g and 4 nm to 20 nm is described.

Patent Document 2 describes a carbon nanostructure consisting of branched rods or rings containing carbon and having a BET specific surface area of 870 m ² /g or more.

Patent Document 3 is a porous carbon material, and the specific surface area SA of mesopores with a pore diameter of 2 nm to 50 nm, measured by analyzing the nitrogen adsorption isotherm during the adsorption process by the Dollimore-Heal method, is 600 m ² /g or more and 1600 m ² /g or less and the peak intensity (IG') that exists in the range of 2650 cm ^-1 to 2700 cm ^-1 in the G'-band of the Raman spectroscopic spectrum and the peak intensity (IG') that exists in the range of 1550 cm ^-1 to 1650 cm ^-1 in the G-band A carbon carrier material for a solid polymer fuel cell in which the relative intensity ratio (IG'/IG) of the peak to the peak intensity (IG) is 0.8 to 2.2 and the peak position of the G'-band is 2660 cm ^-1 to 2670 cm ^-1 Enter.

Patent Document 2 and Patent Document 3 propose a method of producing porous carbon by blowing acetylene gas into silver nitrate (AgNO ₃ ) to produce silver acetylide and then heating the silver acetylide to produce porous carbon.

However, when synthesizing silver acetylide from silver nitrate (AgNO ₃ ), silver acetylide*silver nitrate (Ag ₂ C ₂ *AgNO ₃ ) double salt and ammonium nitrate (NH ₄ NO ₃ ) are produced together as by-products, which are stronger than silver acetylide. It has strong explosive power and is therefore very dangerous when handling it. For reference, the explosion speed of silver acetylide is 1,200 m/s, the explosion speed of silver acetylide*silver nitrate is 2,250 m/s to 3,460 m/s, and the explosion speed of ammonium nitrate is 2,500 m/s to 3,000 m/s. It is s. In addition, silver acetylide*silver nitrate double salt and ammonium nitrate oxidize the mesoporous carbon generated during silver acetylide explosion, thereby promoting a decrease in yield.

Japanese Patent Publication No. 2013-109856 Japanese Patent Registration No. 5481748 International Patent Publication No. 2015/141810

One embodiment provides a method for producing mesoporous carbon that can increase the production yield of mesoporous carbon and improve work safety by suppressing the production of by-products with an explosion risk.

Another embodiment provides mesoporous carbon produced by a method for producing mesoporous carbon.

According to one embodiment, preparing a solution containing silver oxide (Ag ₂ O), mixing the solution containing silver oxide with acetylene (C ₂ H ₂ ) gas to form silver acetylide (Ag ₂ C ₂ ). A method for producing mesoporous carbon is provided, including forming carbon containing mesopores by heat-treating silver acetylide to extrude silver (Ag).

A solution containing silver oxide can be prepared by mixing silver oxide and a high concentration ammonia aqueous solution.

The concentration of the high concentration aqueous ammonia solution may be 7% by volume to 30% by volume.

Silver oxide and high-concentration ammonia aqueous solution may be mixed at a weight ratio of 1:5 to 1:40.

Silver oxide and acetylene (C ₂ H ₂ ) gas may be mixed at a weight ratio of 0.5:1 to 9:1.

The method for producing mesoporous carbon may further include vacuum drying the prepared silver acetylide at 30°C to 100°C for 10 to 48 hours.

Heat treatment can be performed by raising the temperature to 110°C to 250°C in a vacuum atmosphere at a rate of 2°C/min to 6°C/min.

The method for producing mesoporous carbon may include the step of washing the produced mesoporous carbon with nitric acid at 50°C to 85°C for 1 hour to 6 hours.

The concentration of nitric acid may be 10% to 20% by volume.

The method for producing mesoporous carbon may further include adding deionized water to the cleaned mesoporous carbon to dilute the concentration of nitric acid to 2% by volume to 5% by volume.

The method for producing mesoporous carbon may further include washing the cleaned mesoporous carbon with a low-concentration ammonia aqueous solution to pH 5 to 7.

The concentration of the low concentration aqueous ammonia solution may be 0.5% by volume to 5% by volume.

According to another embodiment, mesoporous carbon including mesopores having a specific surface area of 1,500 m ² /g to 2,300 m ² /g and a pore diameter of 3 nm to 7 nm before graphitization treatment is provided.

The mesoporous carbon may have a specific surface area of 1,000 m ² /g to 1,700 m ² /g after graphitization at 1800 ° C. or higher, and a mesopore volume of 0.5 cm ³ /g to 1.4 cm ³ /g, The total pore volume may be between 15 cm ³ /g and 30 cm ³ /g.

The method for producing mesoporous carbon according to one embodiment increases the production yield of mesoporous carbon and improves work safety by suppressing the production of explosive by-products, while lowering the frequency of explosion during synthesis, enabling synthesis in large quantities compared to the same reactor volume. do.

1 is a process flow chart showing a method for manufacturing mesoporous carbon according to one embodiment.
Figure 2 is a scanning electron microscope (SEM) photograph of the mesoporous carbon prepared in Example 1.
Figure 3 is a scanning electron microscope (SEM) photograph of the mesoporous carbon prepared in Comparative Example 1.
Figure 4 is a photograph showing the color change of silver acetylide depending on the concentration of a high-concentration ammonia aqueous solution.
Figure 5 is a graph showing the number of explosions during synthesis depending on the concentration of a high-concentration ammonia aqueous solution.

The advantages and features of the technology described hereinafter, and methods for achieving them, will become clear by referring to the implementation examples described in detail below along with the accompanying drawings. However, the implemented form may not be limited to the implementation examples disclosed below. Unless otherwise defined, all terms (including technical and scientific terms) used in this specification may be used with meanings that can be commonly understood by those skilled in the art. Additionally, terms defined in commonly used dictionaries are not to be interpreted ideally or excessively unless clearly specifically defined. When a part in the entire specification is said to “include” a certain element, this means that it may further include other elements rather than excluding other elements, unless specifically stated to the contrary.

Additionally, the singular includes the plural, unless specifically stated in the phrase.

1 is a process flow chart showing a method for manufacturing mesoporous carbon according to one embodiment. Hereinafter, a method for producing mesoporous carbon will be described in detail with reference to FIG. 1.

The method for producing mesoporous carbon according to one embodiment includes a silver oxide solution preparation step (S1), a silver acetylide formation step (S2), and a heat treatment step (S5).

In the method for producing mesoporous carbon according to one embodiment, the reaction starting material is replaced with silver oxide (Ag ₂ O) from the conventional silver nitrate (AgNO ₃ ), thereby suppressing the production of explosive by-products to produce mesoporous carbon. It increases the manufacturing yield and improves operational safety, while lowering the frequency of explosion during synthesis, making it possible to synthesize in large quantities compared to the same reactor volume.

As an example, silver acetylide (Ag ₂ C ₂ ) is prepared by reacting silver nitrate (AgNO ₃ ) with acetylene (C ₂ H ₂ ) in an aqueous ammonia solution, and then heat-treated to produce porous carbon, as shown in Scheme 1 below. same.

[Scheme 1]

5AgNO ₃ + 4NH ₄ OH + 2C ₂ H ₂ → Ag ₂ C ₂ + Ag ₂ C ₂ *AgNO ₃ + 4NH ₄ NO ₃ + 4H ₂ O

Ag ₂ C ₂ + Ag ₂ C ₂ *AgNO ₃ → 2C + 5Ag + CO ₂ + CO + N ₂

NH ₄ OH + NO ₃ → NH ₄ NO ₃

Referring to Scheme 1, when silver nitrate (AgNO ₃ ) reacts with acetylene (C ₂ H ₂ ), silver acetylide*silver nitrate (Ag ₂ C ₂ *AgNO ₃ ) double salt and ammonium nitrate (NH ₄ NO ₃ ) are produced as by-products. However, they are more explosive than silver acetylide and are therefore more dangerous when handled. In addition, silver acetylide*silver nitrate double salt and ammonium nitrate oxidize the mesoporous carbon generated during silver acetylide explosion, thereby promoting a decrease in yield.

On the other hand, the reaction for producing mesoporous carbon using silver oxide (Ag ₂ O) is shown in Scheme 2 below.

[Scheme 2]

Ag ₂ O + NH ₄ OH + C ₂ H ₂ → 2[Ag(NH ₃ ) ₂ ]OH + C ₂ H ₂ → Ag ₂ C ₂ + 2NH ₄ OH + 2NH ₃ → Ag ₂ C ₂

Referring to Scheme 2, since silver acetylide*silver nitrate (Ag ₂ C ₂ *AgNO ₃ ) double salt and ammonium nitrate (NH ₄ NO ₃ ) by-products are not generated, work safety can be improved by lowering the risk of explosion and carbon loss. By preventing this, the production yield of mesoporous carbon can be increased. In addition, ammonium hydroxide (NH ₄ OH) and ammonia (NH ₃ ) generated as by-products in Scheme 2 can be removed by vacuum drying after washing without filtration, thereby improving work stability.

However, when manufacturing mesoporous carbon using silver oxide (Ag ₂ O), when silver oxide (Ag ₂ O) is dissolved in an aqueous ammonia solution (NH ₄ OH), Ag ₃ N (an explosive substance) is formed in a low concentration aqueous ammonia solution. There is a disadvantage in that the explosion frequency increases during synthesis and the volume of the synthesis reactor must be increased when scaling up.

In order to solve this problem, the method for producing mesoporous carbon according to one embodiment is to synthesize silver oxide by dissolving silver oxide using a high-concentration ammonia aqueous solution in the step (S1) of preparing a solution containing silver oxide (Ag ₂ O). It reduces the frequency of underwater explosions and allows the synthesis of large amounts of silver acetylide in the same reactor volume.

For example, the concentration of the high-concentration ammonia aqueous solution may be 7 vol% to 30 vol%, for example, 10 vol% to 20 vol%. Here, the concentration of the ammonia aqueous solution means the percentage of the ammonia volume relative to the total volume of the ammonia aqueous solution. If the concentration of the high-concentration ammonia aqueous solution is less than 7% by volume, a small explosion may occur inside the reactor during synthesis.

Silver oxide and a high-concentration ammonia aqueous solution may be mixed at a weight ratio of 1:5 to 1:40, for example, 1:10 to 1:30. If the weight ratio of silver oxide and high-concentration ammonia solution is less than 1:5, silver oxide may precipitate or silver nitride may be generated.

In the silver acetylide forming step (S2), a solution containing silver oxide and acetylene (C ₂ H ₂ ) gas are mixed to form silver acetylide (Ag ₂ C ₂ ).

Silver oxide and acetylene (C ₂ H ₂ ) gas may be mixed at a weight ratio of 0.5:1 to 9:1, for example, 1:1 to 3:1. If the weight ratio of silver oxide and acetylene gas exceeds 9:1, the yield of mesoporous carbon may decrease.

Optionally, after the silver acetylide formation reaction, the supernatant of the solution may be removed and diluted (S3).

Removal of the supernatant can be performed to shorten the drying time and suppress side reactions caused by dissolved [Ag(NH ₃ ) ₂ ]OH].

For dilution, remove the supernatant and add deionized water to reach pH 7 to 9. If the pH after dilution is 9 or higher, the carbon yield may be reduced due to dissolved [Ag(NH ₃ ) ₂ ]OH] during heat treatment.

Additionally, the optionally prepared silver acetylide can be vacuum dried (S4).

In Scheme 2, ammonium hydroxide (NH ₄ OH) and ammonia (NH ₃ ), which are by-products generated during the silver acetylide formation reaction, can be removed through vacuum drying.

Vacuum drying may be performed at 30°C to 100°C for 10 to 48 hours, for example, the vacuum drying temperature may be performed at 50°C to 90°C. If the vacuum drying temperature is less than 30 ℃, the drying time may be long, and if it exceeds 100 ℃, some of the silver acetylide inside may react and be ejected out of the reactor, or the reaction may be terminated by temperature without reaching the completion point of drying, causing carbon Yields decrease, and recovery of carbon may be difficult. If the vacuum drying time is less than 10 hours, the yield of the produced carbon may decrease due to incomplete drying.

In the heat treatment step (S5), silver acetylide is heat treated to extrude silver (Ag) to form carbon containing mesopores.

Heat treatment may be performed by raising the internal temperature of the reactor to 110°C to 250°C at a rate of 2°C/min to 6°C/min.

If the temperature of the heat treatment is less than 110 ℃, separation of silver acetylide does not occur, which reduces the yield of mesoporous carbon and may impair safety during carbon recovery. If it exceeds 250 ℃, silver particles and silver oxides generated after the reaction may occur. Burning this mesoporous carbon may reduce yield.

Optionally, the prepared mesoporous carbon may be washed and then diluted (S6).

Mesoporous carbon manufactured using silver oxide can be cleaned with an aqueous nitric acid solution.

Here, the concentration of nitric acid may be 10 vol% to 20 vol%. Here, the concentration of nitric acid means the percentage of nitric acid volume relative to the total volume of nitric acid aqueous solution. If the concentration of nitric acid is less than 10 vol%, silver particles may not be removed, and if it exceeds 20 vol%, it may be difficult to remove nano silver oxide particles contained in the mesopores of the carbon.

Cleaning may be carried out at 50°C to 85°C for 1 hour to 6 hours, for example at 60°C to 80°C for 1 hour to 4 hours. If the cleaning temperature is less than 50°C, it may be difficult to remove silver (Ag) in the mesopores of the carbon, and if it exceeds 85°C, nitric acid may evaporate. If the cleaning time is less than 1 hour, it may be difficult to remove silver particles.

Dilution can be accomplished by adding deionized water to dilute the nitric acid concentration to 2% to 5%. If dilution conditions exceed 5%, silver oxide residues may remain.

Optionally, the cleaned and diluted mesoporous carbon can be filtered and washed (S7).

As an example, in filtration, the washed and diluted mesoporous carbon can be separated using paper filter paper.

Additionally, in washing, silver oxide present in the pores of the mesoporous carbon after heat treatment can be removed with low-concentration ammonia water. Washing is repeated with filtration until the pH of the filtrate of the mesoporous carbon reaches 5 to 7.

The concentration of the low concentration aqueous ammonia solution may be 0.5% by volume to 5% by volume. If the concentration of the ammonia solution is less than 0.5% by volume, silver oxide may not be removed, and if it exceeds 5% by volume, the pH of the carbon may increase.

According to another embodiment, mesoporous carbon includes mesopores as it is produced by the method described above.

Mesopores can be pores with a pore diameter of 3 nm to 7 nm.

The mesoporous carbon may have a specific surface area before graphitization of 1,500 m ² /g to 2,300 m ² /g, for example, 1,800 m ³ /g to 2,100 m ³ /g. If the specific surface area of mesoporous carbon before graphitization is less than 1,500 m ² /g, the weight may increase because silver or silver oxide particles are not removed during acid treatment.

Graphitization treatment of mesoporous carbon may be performed, for example, by raising the temperature to 1,800°C to 2,400°C at a rate of 2°C/min to 5°C/min and then heat treating it for 2 to 8 hours.

The mesoporous carbon may have a specific surface area of 1,000 m ² /g to 1,700 m ² /g after graphitization treatment. If the specific surface area of mesoporous carbon is less than 1,000 m ² /g after graphitization treatment, the volume of mesopores may become small due to excessive graphitization.

After the mesoporous carbon is graphitized, the mesopore volume may be 0.5 cm ³ /g to 1.4 cm ³ /g, for example, 0.6 cm ³ /g to 1.2 cm ³ /g. If the mesopore volume is less than 0.5 cm ³ /g, silver oxide particles within the mesopores may not be properly removed.

Additionally, the total pore volume of the mesoporous carbon after graphitization may be 15 cm ³ /g to 30 cm ³ /g, for example, 18 cm ³ /g to 25 cm ³ /g.

Here, the total pore volume is the cumulative value of the logarithmic derivative pore volume (dV/d (logD)) at each pore size. The mode size of the pores in the carbon carrier can be determined by, for example, the pore size (D) and the log derivative pore volume (dV/d) of the carbon carrier obtained by the Barrett-Joyner-Halenda (BJH) method. The logarithmic derivative in the pore size distribution curve showing the relationship between logD)) can be determined based on the pore size representing the maximum value of pore volume. When the BJH method is applied, the pore size distribution curve can be obtained, for example, by the following procedure. In nitrogen gas at 77.4 K (boiling point of nitrogen), the nitrogen gas adsorption amount (ml/g) of the carbon carrier is measured at each pressure P while gradually increasing the nitrogen gas pressure P (mmHg). Then, the value obtained by dividing the pressure P (mmHg) by the saturated vapor pressure of nitrogen gas P0 (mmHg) is set as the relative pressure P/P0, and the amount of nitrogen gas adsorption for each relative pressure P/P0 is plotted. Thus, the adsorption isotherm is obtained. Then, the pore size distribution of the carbon carrier is obtained from the adsorption isotherm according to the BJH method. In this way, a pore size distribution curve can be obtained. Here, for the BJH method, reference may be made to, for example, published literature (J. Am. Chem. Soc., 1951, Vol. 73, p. 373 to 380).

Below, specific embodiments of the invention are presented. However, the examples described below are only for illustrating or explaining the invention in detail, and should not limit the scope of the invention.

[Manufacture example: Manufacture of mesoporous carbon]

(Example 1)

A solution containing silver oxide was prepared by adding 27.2 g of silver oxide (Ag ₂ O) to 600 ml of ammonia aqueous solution (NH ₄ OH) with a concentration of 15% by volume. Silver oxide and acetylene (C ₂ H ₂ ) are mixed and reacted at a weight ratio of 2:1.

After the reaction, the supernatant is removed and diluted three times to prepare silver acetylide.

The prepared silver acetylide is vacuum dried at 80°C for 12 hours, then heated to 230°C at a rate of 4°C/min to prepare mesoporous carbon.

The prepared mesoporous carbon is washed with nitric acid (HNO ₃ ) at a concentration of 15% by volume for 2 hours at 70°C to remove silver particles, and then diluted to 3% by adding deionized water. Then, additional cleaning is performed at 70°C for 1 hour.

After washing the mesoporous carbon, washing and filtration are repeated with a 1% aqueous ammonia solution or deionized water until the pH of the filtrate of the mesoporous carbon reaches 6 to remove any remaining silver oxide.

Dry in an oven at 100°C to obtain mesoporous carbon.

(Comparative Example 1)

Mesoporous carbon was manufactured in the same manner as Example 1, except that silver nitrate (AgNO ₃ ) was used instead of silver oxide (Ag ₂ O).

[Experimental Example 1: Characteristic analysis of mesoporous carbon]

As a result of measuring the pore diameter, mesopore volume, and specific surface area of the mesoporous carbon prepared in Example 1, the pore diameter was 3.7 nm, the pore volume (V2-5nm) was 0.68 cm ³ /g, and the specific surface area was It is 1,947 m ² /g.

In addition, the mesoporous carbon prepared in Example 1 was graphitized by raising the temperature to 1,800°C at a rate of 5°C/min and then heat treating it for 2 hours. The pore volume (V2-5nm) is 0.84 cm ³ /g, the specific surface area is 1,516 m ² /g, and the BJH (dV/d log(D)) total pore volume is 21 cm ³ /g to 22 cm ³ /g. It was confirmed that it was.

Scanning electron microscope (SEM) photographs of the mesoporous carbon prepared in Example 1 and Comparative Example 1 are shown in Figures 2 and 3, respectively.

Referring to Figures 2 and 3, it can be seen that it is a mesoporous carbon having a nanostructure with a diameter of 30 nm to 50 nm.

In Example 1 and Comparative Example 1, the amount of carbon that can theoretically be generated per 1 g of silver oxide (Ag ₂ O) and silver nitrate (AgNO ₃ ) and the amount of carbon actually generated are summarized in Table 1. At this time, the theoretical value assumes that the silver (Ag) of the material is 100% synthesized into silver acetylide (Ag ₂ C ₂ ) and that there are no side reactions.

matter theoretical creation
amount of carbon actual creation
amount of carbon Carbon
Loss (%) Comparative Example 1 AgNO ₃ 0.7g 0.025 g 96.5% Example 1 Ag ₂ O 0.103 g 0.095 g 7.8%

Referring to Table 1, it can be seen that in the case of silver nitrate (AgNO ₃ ) in Comparative Example 1, carbon is oxidized by silver acetylide * silver nitrate double salt and ammonium nitrate by-product, resulting in a decrease in yield, and in the case of silver oxide (Ag ₂ O) in Example 1 ), it can be seen that carbon loss can be prevented as these by-products are not generated.

[Experimental Example 2: Analysis of reaction explosion frequency]

When converting silver oxide (Ag ₂ O) into Ag(NH ₃ ) ₂ OH, check the difference in explosion frequency that occurs during synthesis depending on the concentration of ammonia solution.

(Example 2)

A solution containing silver oxide is prepared by mixing 13.6 g of silver oxide (Ag ₂ O), 930 ml of deionized water, and 70 ml of a 28 volume % aqueous ammonia solution (NH ₄ OH). Silver oxide and acetylene (C ₂ H ₂ ) are mixed and reacted at a weight ratio of 2:1.

(Example 3)

A solution containing silver oxide is prepared by mixing 13.6 g of silver oxide (Ag ₂ O), 910 ml of deionized water, and 90 ml of 28 vol% aqueous ammonia solution (NH ₄ OH). At this time, the volume concentration of ammonia aqueous solution (NH ₄ OH) is 2.5 volume%. Silver oxide and acetylene (C ₂ H ₂ ) are mixed and reacted at a weight ratio of 2:1.

(Example 4)

A solution containing silver oxide is prepared by mixing 13.6 g of silver oxide (Ag ₂ O), 720 ml of deionized water, and 280 ml of 28 vol% aqueous ammonia solution (NH ₄ OH). At this time, the volume concentration of ammonia aqueous solution (NH ₄ OH) is 6.6 volume%. Silver oxide and acetylene (C ₂ H ₂ ) are mixed and reacted at a weight ratio of 2:1.

Figure 4 is a photograph showing the color change of silver acetylide depending on the concentration of a high-concentration ammonia aqueous solution.

Referring to FIG. 4, it can be seen that when synthesized with an ammonia aqueous solution having a concentration of 1.9 vol% or more as in Example 2, a color difference occurs in the final product of silver acetylide. In addition, when synthesizing silver acetylide using an aqueous ammonia solution with a concentration of 1.9% by volume or more as in Example 2 and using silver oxide (Ag ₂ O) as the starting material, it was confirmed that explosions occurred six times during the synthesis. On the other hand, it was confirmed that when the concentration of ammonia aqueous solution was increased as in Examples 3 and 4, the number of explosions during synthesis was reduced.

These results are summarized in Figure 5. Figure 5 is a graph showing the number of explosions during synthesis depending on the concentration of a high-concentration ammonia aqueous solution. Referring to FIG. 5, it can be seen that when synthesizing silver acetylide (Ag ₂ C ₂ ) in large quantities using silver oxide (Ag ₂ O), the volume and safety of the reactor can be improved by using a high concentration aqueous ammonia solution.

Although the preferred embodiments of the present invention have been described in detail above, the above-described embodiments are presented as specific examples of the present invention, and the present invention is not limited thereto, and the scope of the present invention is defined by the claims described later. Various modifications and improvements made by those skilled in the art using the basic concept of the present invention defined in also fall within the scope of the present invention.

Claims (15)

Preparing a solution containing silver oxide (Ag ₂ O),
Mixing the solution containing the silver oxide with acetylene (C ₂ H ₂ ) gas to form silver acetylide (Ag ₂ C ₂ ), and
Forming carbon containing mesopores by heat-treating the silver acetylide to eject silver (Ag)
Method for producing mesoporous carbon, including. In paragraph 1:
A method of producing mesoporous carbon, wherein the solution containing the silver oxide is prepared by mixing the silver oxide and a high concentration ammonia aqueous solution. In paragraph 2,
A method for producing mesoporous carbon, wherein the concentration of the high-concentration ammonia aqueous solution is 7% by volume to 30% by volume. In paragraph 2,
A method for producing mesoporous carbon, wherein the silver oxide and the high-concentration ammonia aqueous solution are mixed at a weight ratio of 1:5 to 1:40. In paragraph 1:
A method for producing mesoporous carbon, wherein the solution containing silver oxide and the acetylene (C ₂ H ₂ ) gas are mixed at a weight ratio of 0.5:1 to 9:1. In paragraph 1:
The method for producing mesoporous carbon further includes vacuum drying the prepared solution containing silver acetylide at 30°C to 100°C for 10 to 48 hours. In paragraph 1:
A method for producing mesoporous carbon, wherein the heat treatment is carried out by raising the temperature to 110°C to 250°C at a rate of 2°C/min to 6°C/min. In paragraph 1:
The method for producing mesoporous carbon further includes the step of washing the prepared mesoporous carbon with nitric acid at 50° C. to 85° C. for 1 hour to 6 hours. In paragraph 8:
A method for producing mesoporous carbon, wherein the concentration of nitric acid is 10 vol% to 20 vol%. In paragraph 8:
The method for producing mesoporous carbon further includes adding deionized water to the cleaned mesoporous carbon to dilute the concentration of nitric acid to 2% by volume to 5% by volume. In paragraph 8:
The method for producing mesoporous carbon further includes the step of washing the cleaned mesoporous carbon with a low-concentration ammonia aqueous solution to pH 5 to 7. In paragraph 11:
A method for producing mesoporous carbon, wherein the concentration of the low-concentration aqueous ammonia solution is 0.5 vol% to 5 vol%. Manufactured by the method for producing mesoporous carbon according to claim 1,
The specific surface area before graphitization is 1,500 m ² /g to 2,300 m ² /g,
Comprising mesopores with a pore diameter of 3 nm to 7 nm,
Mesoporous carbon. In paragraph 13:
The mesoporous carbon has a specific surface area of 1,000 m ² /g to 1,700 m ² /g after graphitization at 1800 ° C. or higher,
the volume of the mesopores is 0.5 cm ³ /g to 1.4 cm ³ /g,
Mesoporous carbon. In paragraph 14:
The mesoporous carbon has a total pore volume of 15 cm ³ /g to 30 cm ³ /g.