KR20140135440A - Activated charcoal with functional group and manufacturing method thereof via mechanic chemical process - Google Patents
Activated charcoal with functional group and manufacturing method thereof via mechanic chemical process Download PDFInfo
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- KR20140135440A KR20140135440A KR1020130055686A KR20130055686A KR20140135440A KR 20140135440 A KR20140135440 A KR 20140135440A KR 1020130055686 A KR1020130055686 A KR 1020130055686A KR 20130055686 A KR20130055686 A KR 20130055686A KR 20140135440 A KR20140135440 A KR 20140135440A
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- C—CHEMISTRY; METALLURGY
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- C01B32/00—Carbon; Compounds thereof
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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
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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
- C01B32/342—Preparation characterised by non-gaseous activating agents
Abstract
The present invention relates to a method for producing a functionalized activated carbon powder by introducing various functional groups at the edge of activated carbon, and is characterized in that the functional group-imparting substance is mixed with activated carbon in the step of pulverizing activated carbon without any special heat treatment step or firing step , And can be manufactured by a simpler method at a lower cost than the conventional surface modification method of activated carbon. In addition, it has an advantage of being able to mass-produce compared to a method using a conventional plasma.
Description
The present invention relates to an activated carbon powder into which a functional group has been introduced and a method for producing the same, and more particularly to an activated carbon powder in which a functional group is introduced through a process of mixing and pulverizing a conventional activated carbon with a functional group- .
Activated carbon is generally produced by activating carbides obtained by carbonizing raw materials such as coal or coconut shells such as lignite, bituminous coal, and coconut shells in an atmosphere of steam or steam at a high temperature in a rotary furnace or a multi-phase furnace. The activated carbon is an amorphous material composed mainly of carbon and is a porous carbonaceous material having excellent specific surface area and adsorbing ability and is used as an adsorbent for various purposes and is used not only in chemical industry such as purification, , And can be used as a catalyst or a catalyst support, particularly, as a redox catalyst for a fuel cell.
In order to improve the properties of the activated carbon that can be used in various fields, there have been developed surface modification methodologies for introducing a large number of functional groups onto the surface of activated carbon.
Among these conventional techniques, Korean Patent Laid-Open Publication No. 1990-016260 discloses a method for modifying the surface of activated carbon at a high temperature. The present invention relates to a method for attaching a functional group to the surface of an activated carbon by introducing a functional group onto the surface of the activated carbon by keeping the activated carbon at a predetermined temperature for a predetermined time under air without using an oxidizing solution. However, the above manufacturing method has a problem that enormous energy is consumed because it is maintained at a high temperature for a long time.
In order to solve the above problem, Korean Patent Laid-Open No. 10-2003-0093146 discloses a surface modification method of activated carbon using plasma. The present invention relates to a method for producing surface-modified activated carbon using atmospheric oxygen plasma, which is excellent in adsorbability against toxic gases but has limitations in application fields. In order to modify the surface of a large amount of activated carbon, There is a problem in that there is a limit to the production amount because the equipment is required and it is not economical and the time required for the processing device to be increased becomes long.
Also, as a method for modifying the surface of activated carbon using a chemical, a large amount of waste such as a washing waste liquid is generated due to an additional process for removing the residual solution not used in the post-production reforming reaction and the solution remaining on the surface of the reformed activated carbon And there is a problem that the pore structure of the activated carbon is destroyed due to an excessive chemical reaction and the adsorption capacity is lowered.
SUMMARY OF THE INVENTION Accordingly, the present invention has been made in view of the above problems, and it is an object of the present invention to provide a method for simply and efficiently producing an activated carbon powder into which functional groups having various functions are introduced.
Also, it is intended to provide an activated carbon powder which is functionalized by introducing various functional groups at the edge of activated carbon by the above-mentioned production method.
Also, there is provided a redox catalyst for a fuel cell using activated carbon powder into which a functional group having a large capacitance is introduced.
In order to solve the above-described problems, the present invention provides a method for producing a functionalized activated carbon powder comprising the following steps.
A step of pulverizing the pulverized vessel with activated carbon and a functional group-imparting substance, washing the pulverized activated carbon with an acid solution, and drying the activated carbon powder washed with the acid solution.
According to an embodiment of the present invention, the functional group-imparting substance may be a gas, a liquid or a solid, and when the functional group-imparting substance is a gas, the process conditions in the pulverization step are 1-200 bar, 10-10,000 rpm and 1 -100 hours, and when the functional group-imparting substance is liquid or solid, the process conditions in the pulverization step may be 10-10,000 rpm and 1-100 hours.
According to one embodiment of the present invention, the crushing vessel may be any one selected from the group consisting of a cone crusher, a double roll crusher, a disk crusher, a rotary crusher, a ball mill, a centrifugal roller mill, a ring roll mill and a centrifugal ball mill.
According to an embodiment of the present invention, the average diameter of the modified activated carbon powder that can be utilized as a material for various application fields, an adsorbent, and an oxidation-reduction catalyst of a fuel cell may be 50 nm or more.
According to an embodiment of the present invention, the functional group that is introduced at the edge of the activated carbon powder and has various functions may be selected from the group consisting of an alkyl group, an alkenyl group, an arene group, a tert-butyl group, a cyclohexyl group, a hydroxyl group, a lactone group, An amino group, an imide group, an azide group, a cyanic acid group, a nitrile group, a nitro group, a nitro group, a nitro group, a pyridine group, a phosphine group, a phosphoric acid group, a phosphonic acid group, A carboxyl group, a carboxylic acid ester group, a haloformyl group, an ether group, an ester group, a peroxy group, a hydroperoxy group, an acyl halide group, a fluoro group, a sulfone group, a sulfoxide group, a thiol group, a thiol group, a carbonyl group, an aldehyde group, A halogen atom, a nitro group, a chloro group, a bromo group, an iodo group, and combinations thereof.
The functional group-imparting substance for imparting such a functional group may be contained in an amount of 0.1 to 50 parts by weight based on 100 parts by weight of activated carbon.
The functional group-imparting substance may be at least one selected from the group consisting of nitrogen, air, hydrogen, methane, ethane, carbon monoxide, carbon dioxide, nitrogen dioxide, ammonia, florine, chlorine, hydrogen fluoride, hydrogen bromide, hydrogen chloride, hydrogen cyanide, hydrogen sulfide, But are not limited to, water, methanol, ethanol, isopropyl alcohol, sulfuric acid, nitric acid, acetic acid, n-hexane, cyclohexane, heptane, toluene, benzene, acetone, N-methylpyrrolidone, tetrahydrofuran, dimethylacetamide, Sodium hydroxide, sodium hydroxide, sodium hydrogencarbonate, sodium carbonate, potassium carbonate, sodium sulphate, nitric acid, sodium nitrate, sodium carbonate, potassium carbonate, sodium carbonate, potassium carbonate, Sodium chloride, sodium chloride, ammonium chloride, boron trioxide, boric acid, tribromoboron, aminobenzoic acid, chlorobenzoic acid Acid, bromobenzoic acid, thiolbenzoic acid, maleic acid, and mixtures thereof.
According to an embodiment of the present invention, the acid solution may be at least one selected from the group consisting of nitric acid (HNO 3 ), hydrochloric acid (HCl), hydrofluoric acid (HF), sulfuric acid (H 2 SO 4 ) The concentration of the acid solution may be 0.1-10 M.
The present invention also provides an activated carbon having a functional group, which is produced according to the above-described method, and provides a redox catalyst for a fuel cell comprising the activated carbon.
According to the present invention, modified activated carbon powder which can be used as materials for various application fields, adsorbents, oxidation catalysts for fuel cells, etc. can be manufactured at a lower cost and in a simpler manner as compared with the conventional surface modification method of activated carbon. In addition, it has an advantage of being able to mass-produce compared to a method using a conventional plasma.
1 is a scanning electron microscope (SEM) photograph of activated carbon powder according to an embodiment of the present invention.
FIG. 2 is an image of nitrogen distribution showing the distribution of nitrogen functional groups attached to the surface of activated carbon powder according to an embodiment of the present invention. FIG.
FIG. 3 is a graph of binding energy analysis measured by an XPS (X-ray Photoelectron Spectrometer) of activated carbon powder according to an embodiment of the present invention.
FIG. 4 is a graph showing current-voltage characteristics of an activated carbon powder according to an embodiment of the present invention measured in an electrolyte solution of 0.1 M KOH. FIG.
5 is a graph showing current-voltage characteristics measured 1000 times in order to confirm the stability of activated carbon powder according to an embodiment of the present invention.
6 is a graph showing current-voltage characteristics of an activated carbon powder according to an embodiment of the present invention measured in a 5.5 M KOH electrolyte.
Hereinafter, the present invention will be described in more detail.
One aspect of the present invention relates to a method for producing a functionalized activated carbon powder by introducing various functional groups at the edges of activated carbon powder, and is characterized by comprising the following steps.
Pulverizing the pulverized vessel with activated carbon and a functional group-imparting substance,
Washing the pulverized activated carbon with an acid solution,
Drying the activated carbon powder washed with the acid solution.
At this time, coconut-based activated carbon, coal-based activated carbon, fiber-based activated carbon and the like can be used as the activated carbon.
The functional group-imparting substance for functionalizing the activated carbon may be gas, liquid or solid. When the functional group-imparting substance is a gas, the pulverization step process condition is preferably 1-200 bar, 10-10,000 rpm, and 1-100 hours When the functional group-imparting substance is liquid or solid, the pulverization step is preferably performed at 10-10,000 rpm for 1-100 hours.
Since the present invention is characterized by incorporating a functional group-imparting substance in the step of pulverizing activated carbon without a special heat treatment process or a firing process, the edges of the activated carbon are further functionalized under the above-mentioned pulverizing process conditions.
Particularly, when the functional group-imparting substance is a gas, the optimal conditions may vary depending on the kind thereof, but it is preferable that the pressure is set at a pressure of 1-200 bar.
The pulverizing vessel may be any one selected from the group consisting of a cone crusher, a double roll crusher, a disk crusher, a rotary crusher, a ball mill, a centrifugal roller mill, a ring roll mill and a centrifugal ball mill. Or more.
The functional group may be an alkyl group, an alkenyl group, an arene group, a tert-butyl group, a cyclohexyl group, a hydroxyl group, a lactone group, a lactam group, an ether group, A nitro group, a nitro group, a pyridine group, a phosphine group, a phosphoric acid group, a phosphonic acid group, a sulfone group, a sulfonic acid group, a sulfoxide group, a thiol group, a sulfide group, a carbonyl group, an aldehyde group, A group consisting of a carboxylic acid group, a carboxylic acid ester group, a haloformyl group, an ether group, an ester group, a peroxy group, a hydroperoxy group, an acyl halide group, a fluoro group, a chloro group, a bromo group, . ≪ / RTI >
The functional group-imparting substance may be at least one selected from the group consisting of nitrogen, air, hydrogen, methane, ethane, carbon monoxide, carbon dioxide, nitrogen dioxide, ammonia, florine, chlorine, hydrogen fluoride, hydrogen bromide, hydrogen chloride, hydrogen cyanide, hydrogen sulfide, But are not limited to, water, methanol, ethanol, isopropyl alcohol, sulfuric acid, nitric acid, acetic acid, n-hexane, cyclohexane, heptane, toluene, benzene, acetone, N-methylpyrrolidone, tetrahydrofuran, dimethylacetamide, Sodium hydroxide, sodium hydride, sodium hydrogen carbonate, sodium carbonate, potassium carbonate, sodium sulfate, sodium nitrate, sodium chloride, sodium chloride, potassium carbonate, , Ammonium chloride, boron trioxide, boric acid, tribromoboron, aminobenzoic acid, chlorobenzoic acid, bromo Benzoic acid, benzoic acid, thiolbenzoic acid, and maleic acid.
In addition, the present invention wherein the grinding in order to remove a metal component contained in the activated carbon, the solution and removing the acid solution, wherein the acid is nitric acid (HNO 3), hydrochloric acid (HCl), hydrofluoric acid (HF), sulfuric acid (H 2 SO 4 ) and aqua regia. The concentration of the acid solution is preferably 0.1-10 M, and when the concentration is less than 0.1 M, the metal component is not sufficiently removed even if the reaction is carried out for a long period of time.
In the above step, when the metal component remains in a trace amount depending on the functional group-imparting substance, the activated carbon, the pulverizer, etc., the present step of treating with an acid solution may be omitted or the step of treating with an acid solution may be carried out before the step of pulverizing It is also possible.
Hereinafter, the present invention will be described in more detail with reference to the drawings, examples and experimental examples. It will be apparent to those skilled in the art, however, that these examples and test examples are provided to further illustrate the present invention and that the scope of the present invention is not limited thereby.
Production Example 1
Conventionally, 5 g of activated carbon was put into a metal grinding vessel, air was removed from the grinding vessel by using a vacuum pump, nitrogen was introduced at 10 bar and pulverized at 500 rpm for 48 hours. To remove the metal of the pulverized activated carbon powder, it was washed with 1 M hydrochloric acid and lyophilized to prepare nitrogen-doped activated carbon powder.
Experimental Example 1
The surface of the nitrogen-introduced activated carbon powder according to Preparation Example 1 was measured using a scanning electron microscope (SEM). The results are shown in FIG. 1 and FIG.
FIG. 1 is an image of the surface of the activated carbon powder taken by SEM. FIG. 2 is an image showing nitrogen using EDX to identify a nitrogen functional group introduced into the surface of the activated carbon powder, The combined nitrogen functionality was indicated in green.
As a result, it can be seen that sufficient nitrogen functional groups were uniformly attached to the activated carbon powder into which the nitrogen functional group prepared according to Production Example 1 was introduced.
Experimental Example 2
The chemical composition of the activated carbon powder to which the nitrogen functional group according to Preparation Example 1 was introduced was analyzed by photoelectron spectroscopy (XPS).
As a result, as shown in FIG. 3, it can be confirmed that a large amount of nitrogen functional groups exist on the surface of the activated carbon powder prepared according to Production Example 1.
Experimental Example 3
The activity of the activated carbon powder to which the nitrogen functional group according to Preparation Example 1 was introduced was measured by cyclic voltammetry (CV) using 0.1 M KOH electrolyte.
FIG. 4 shows the result of measurement under an oxygen atmosphere. It was confirmed that the oxygen reduction peak was measured at -0.2 V and the electrochemical activity was high. FIG. 5 shows the result of 1000 repeated measurements under an oxygen atmosphere, It can be understood that the stability is excellent when it is used as a catalyst of a fuel cell.
Experimental Example 4
In order to measure the electrochemical activity of the activated carbon powder having the nitrogen functional group according to Preparation Example 1, a cyclic voltammetry (CV) was performed using a 5.5 M KOH electrolyte. As a result, , And Table 1 shows the capacitance according to the voltage.
As shown in FIG. 6 and Table 1, the capacitance of 224.9 F / g at a voltage of 10 mV was shown, which indicates that the activated carbon powder according to Preparation Example 1 is carbon, have.
Claims (13)
Washing the pulverized activated carbon with an acid solution; And
And drying the activated carbon powder washed with the acid solution.
Wherein the functional group-imparting substance is a gas, a liquid, or a solid.
Wherein when the functional group-imparting substance is a gas, the pulverizing step is performed at 1-200 bar at 10-10000 rpm for 1-100 hours.
Wherein when the functional group-imparting substance is a liquid or a solid, the pulverization is performed at 10-10000 rpm for 1-100 hours.
Wherein the pulverizing container is any one selected from the group consisting of a cone crusher, a double roll crusher, a disk crusher, a rotary crusher, a ball mill, a centrifugal roller mill, a ring roll mill and a centrifugal ball mill. .
Wherein the activated carbon powder has an average diameter of 50 nm to 100 占 퐉.
The functional group may be an alkyl group, an alkenyl group, an arene group, a tert-butyl group, a cyclohexyl group, a hydroxyl group, a lactone group, a lactam group, an ether group, A nitro group, a nitro group, a pyridine group, a phosphine group, a phosphoric acid group, a phosphonic acid group, a sulfone group, a sulfonic acid group, a sulfoxide group, a thiol group, a sulfide group, a carbonyl group, an aldehyde group, Selected from the group consisting of a carboxylic acid ester group, a carboxylic acid ester group, a haloformyl group, an ether group, an ester group, a peroxy group, a hydroperoxy group, an acyl halide group, a fluoro group, a chloro group, a bromo group, Wherein the activated carbon powder is one of the following.
Wherein the functional group-imparting substance is contained in an amount of 0.1 to 50 parts by weight based on 100 parts by weight of activated carbon.
The functional group-imparting substance may be selected from the group consisting of nitrogen, air, hydrogen, methane, ethane, carbon monoxide, carbon dioxide, nitrogen dioxide, ammonia, florine, chlorine, hydrogen fluoride, hydrogen bromide, hydrogen chloride, hydrogen cyanide, hydrogen sulfide, But are not limited to, methanol, ethanol, isopropyl alcohol, sulfuric acid, nitric acid, acetic acid, n-hexane, cyclohexane, heptane, toluene, benzene, acetone, N-methylpyrrolidone, tetrahydrofuran, dimethylacetamide, , Ethyl acetate, methyl ethyl ketone, xylenes, dichlorobenzene, dichloromethane, chloroform, carbon tetrachloride, bromine, sodium hydroxide, potassium hydroxide, sodium hydride, sodium hydrogenphosphate, sodium carbonate, potassium carbonate, sodium nitrate, sodium chloride, Ammonium, boron trioxide, boric acid, tribromoboron, aminobenzoic acid, chlorobenzoic acid, bromobenzoic acid The method of the acid, a thiol acid and benzo functional group, characterized in that any one of selected from the group consisting of maleic acid introduced into the activated carbon.
Wherein the acid solution is at least one selected from the group consisting of nitric acid (HNO 3 ), hydrochloric acid (HCl), hydrofluoric acid (HF), sulfuric acid (H 2 SO 4 ) .
Wherein the concentration of the acid solution is 0.1-10 M.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104891473A (en) * | 2015-05-24 | 2015-09-09 | 西北大学 | Preparation method of nitrogen-doped carbon material |
| CN109796003A (en) * | 2019-03-21 | 2019-05-24 | 哈尔滨工业大学 | A kind of coal base hard carbon Surface Oxygen functional group orientation regulation method for storing up sodium cathode |
| KR20200097079A (en) | 2019-02-07 | 2020-08-18 | 박갑동 | Preparing Method of Acitvated Carbon Using Vegetable Sponge |
| CN114316510A (en) * | 2021-11-22 | 2022-04-12 | 江西师范大学 | Method for preparing sulfonic group-containing bimetallic composite polymer nano material |
| CN115504453A (en) * | 2022-09-20 | 2022-12-23 | 北京化工大学 | Method for treating fluorine-containing greenhouse gas and co-producing carbon fluoride material by using mechanochemistry |
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- 2013-05-16 KR KR1020130055686A patent/KR20140135440A/en not_active Application Discontinuation
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104891473A (en) * | 2015-05-24 | 2015-09-09 | 西北大学 | Preparation method of nitrogen-doped carbon material |
| KR20200097079A (en) | 2019-02-07 | 2020-08-18 | 박갑동 | Preparing Method of Acitvated Carbon Using Vegetable Sponge |
| CN109796003A (en) * | 2019-03-21 | 2019-05-24 | 哈尔滨工业大学 | A kind of coal base hard carbon Surface Oxygen functional group orientation regulation method for storing up sodium cathode |
| CN109796003B (en) * | 2019-03-21 | 2022-03-25 | 哈尔滨工业大学 | Coal-based hard carbon surface oxygen functional group directional regulation and control method for sodium storage cathode |
| CN114316510A (en) * | 2021-11-22 | 2022-04-12 | 江西师范大学 | Method for preparing sulfonic group-containing bimetallic composite polymer nano material |
| CN114316510B (en) * | 2021-11-22 | 2023-10-10 | 江西师范大学 | Method for preparing sulfonic group-containing bimetal composite polymer nano material |
| CN115504453A (en) * | 2022-09-20 | 2022-12-23 | 北京化工大学 | Method for treating fluorine-containing greenhouse gas and co-producing carbon fluoride material by using mechanochemistry |
| CN115504453B (en) * | 2022-09-20 | 2024-02-02 | 北京化工大学 | Method for combining fluorine-containing greenhouse gas with fluorocarbon material by mechanochemical treatment |
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