KR101982987B1 - Activated carbon for high power energy storage and method for manufacture thereof - Google Patents

Abstract

The present invention relates to a method of producing activated carbon for high power energy storage and, more specifically, to a method of producing activated carbon for high power energy storage, which comprises: an impregnation step of selecting and pulverizing a cellulose-based biomass to obtain a pulverized biomass, and impregnating the pulverized biomass with an acidic aqueous solution to obtain an impregnated biomass; a charging step of charging the impregnated biomass into a furnace to obtain a charged biomass; an activation step of heating the furnace, thereby activating the charged biomass to obtain an activated biomass; a cooling step of cooling the activated biomass to obtain a cooled biomass; and a cleaning step of cleaning the cooled biomass with a cleaning solution to produce activated carbon, wherein the furnace is charged with an active gas or an inert gas therein. According to the present invention, the method can produce the activated carbon for high power energy storage, and an electric double layer capacitor can be manufactured by using the activated carbon for high power energy storage.

Description

TECHNICAL FIELD [0001] The present invention relates to an activated carbon for high energy storage,

More particularly, the present invention relates to a method for producing active carbon particulates for high-power energy storage, and more particularly, to a method for producing an activated carbon particulate phase, which comprises: impregnating an aqueous solution of a cellulosic biomass into an aqueous solution, The present invention relates to a method for producing activated carbon for high-power energy storage having chemical output characteristics.

The currently used energy storage devices are typically lead-acid batteries, lithium secondary batteries, and electric double layer capacitors (EDLC).

At this time, the energy density of the lead-acid battery and the lithium secondary battery is as high as 20 to 150 Wh / kg, but the output density is as low as 50 to 300 W / kg and the cycle life is only about 1,000 times.

However, the electric double layer capacitor has an energy density of 2,000 to 3,000 W / kg, a cycle life characteristic of 500,000 times or more, and stability, compared with a lead-acid battery and a lithium secondary battery.

In recent years, the market for electric double layer capacitors has been on the rise, and electric double layer capacitors have been used in place of conventional batteries such as smart meters.

Conventional electric double-layer capacitors include coconut shells using water vapor, phenol-based activated carbon using coke-based activated carbon and potassium hydroxide, and the like. In recent years, high power density and low resistance The demand for products that are demanding is increasing.

However, conventional coconut shells and coke-based activated carbon are formed in micropore of about 90%, which makes it difficult to transfer electrolyte ions at high output.

In addition, the conventional porous carbon material is mostly produced by steam, and thus, it is possible to manufacture only a precursor having a high fixed carbon ratio, and it is difficult to form a medium-sized hole.

Therefore, it is necessary to develop a technology capable of manufacturing a porous carbon material having a mesopore suitable for improving the output characteristics of an energy storage device.

Disclosure of Invention Technical Problem [8] Accordingly, the present invention has been made keeping in mind the above problems occurring in the prior art, and an object of the present invention is to provide a method for producing activated carbon for high-power energy storage having excellent electrochemical output characteristics as well as forming excellent mesopores by impregnating and activating cellulosic biomass in an aqueous solution The purpose is to provide.

In order to solve the above problems, the present invention provides a method for producing activated carbon for high-power energy storage, comprising the steps of: pulverizing cellulose-based biomass, impregnating the pulverized biomass into an aqueous solution; Charging the impregnated biomass into a furnace; An activation step of heating the furnace to activate the charged biomass; A cooling step of cooling the activated biomass; And washing the cooled biomass with a washing liquid to produce activated carbon, wherein the furnace is filled with an active gas or an inert gas.

In the impregnating step, the pulverized biomass is impregnated in an aqueous solution of 0.1 to 100% for 10 minutes to 120 hours, wherein the biomass and the aqueous solution are impregnated in a weight ratio of 1: 0.1 to 1:10 .

The activating step is characterized in that the furnace is heated to 100 to 1000 ° C at a heating rate of 1 to 30 ° C / min, and then the heating temperature is maintained for 5 to 120 minutes to activate the impregnated biomass .

The cooling step may be characterized in that the activated biomass is cooled to room temperature.

The washing solution may be characterized by being formed of distilled water, purified water and one of an alkali or acidic solution having a molar concentration of 0.01 to 5 mol / L.

In the washing step, the cooled biomass is agitated in a washing solution at a temperature ranging from room temperature to 150 ° C, and the washing is repeated 1 to 20 times.

In addition, the active carbon may have a mid-air ratio of 40% or more based on the total volume of the gun.

The high-power energy-storage activated carbon of the present invention can be characterized by being produced by the above production method.

In addition, the electric double layer capacitor of the present invention is characterized by being manufactured from the high output energy storage activated carbon.

Also, the electric double layer capacitor of the present invention is produced by mixing the high power energy storage activating carbon and the conventional commercial activated carbon at a ratio of 0.01: 99.9 wt% to 99.9: 0.01 wt%, and the conventional commercial activated carbon is YP- 50F, YP-FW, CEP21KS and MSP-20.

According to the method for producing activated carbon for high power storage of energy according to the present invention as described above, since the specific surface area is high, the adsorption amount is increased and the total pore number is increased.

In addition, since a high proportion of heavy metal balls is formed, the ions of the electrolyte smoothly move within the electrode active material structure during high-speed charge and discharge, resulting in high electrochemical output characteristics.

1 is a flowchart showing a method for producing activated carbon for high-power energy storage according to an embodiment of the present invention.
FIG. 2 is a graph showing the results of measurement of the specific surface area of activated carbon for high-power energy storage and two kinds of compatibilizing carbon (YP-50F, YP-FW) according to an embodiment of the present invention.
3 is a graph showing pore sizes and distributions of activated carbon for high-power energy storage and two types of compatibilizing carbon (YP-50F, YP-FW) according to an embodiment of the present invention.
FIG. 4 is a graph showing a CV (Cyclic Voltammetry) Curve of high-energy-storing activated carbon and two types of compatibilizing carbon (YP-50F, YP-FW) according to an embodiment of the present invention.
5 is a graph showing the capacity retention rate according to the current per unit area of the activated carbon for high-power energy storage and the two kinds of compatibilizing carbon (YP-50F, YP-FW) according to the embodiment of the present invention.
FIG. 6 is a conceptual diagram illustrating the difference in flow of electron ions according to the pore characteristics of the high-energy-storing activated carbon and the commercialized activated carbon according to the embodiment of the present invention.

Hereinafter, the description of the present invention with reference to the drawings is not limited to a specific embodiment, and various transformations can be applied and various embodiments can be made. It is to be understood that the following description covers all changes, equivalents, and alternatives falling within the spirit and scope of the present invention.

In the following description, the terms first, second, and the like are used to describe various components and are not limited to their own meaning, and are used only for the purpose of distinguishing one component from another component.

Like reference numerals used throughout the specification denote like elements.

As used herein, the singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. It is also to be understood that the terms " comprising, " " comprising, " or " having ", and the like are intended to designate the presence of stated features, integers, And should not be construed to preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, or combinations thereof.

Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries are to be interpreted as having a meaning consistent with the contextual meaning of the related art and are to be interpreted as either ideal or overly formal in the sense of the present application Do not.

Hereinafter, embodiments of the present invention will be described in more detail with reference to Figs. 1 to 6. Fig.

FIG. 1 is a flowchart showing a method for producing high-energy-use activated carbon according to an embodiment of the present invention. FIG. 2 is a graph showing the relationship between activated carbon for high-power energy storage and two types of compatibilizing carbon (YP-50F, YP FIG. 3 is a graph showing the results of measurement of specific surface area of the activated carbon for high-power energy storage and YP-50F, FIG. 4 is a graph showing a CV (Cyclic Voltammetry) Curve of high-energy-storing activated carbon and two types of compatibilizing carbon (YP-50F, YP-FW) according to an embodiment of the present invention. FIG. 6 is a graph showing the capacity retention ratio of the high-energy-storing activated carbon and the two compatibilizing carbon species (YP-50F, YP-FW) according to the present invention, Commercialization with activated carbon for energy storage It is a conceptual diagram showing the flow difference between the electron-ion of the pore properties of the carbon.

1, the method for producing activated carbon for high-power energy storage according to an embodiment of the present invention includes the steps of impregnating S100, charging S 200, activating S 300, cooling S 400, (S500).

Specifically, the present invention relates to a process for producing a high-power energy-saving activated carbon having high electrochemical characteristics as well as forming an excellent mesopore by impregnating cellulose-based biomass into an aqueous solution and then activating the same, Carbon and electric double layer capacitors.

First, in the impregnation step (SlOO), the cellulosic biomass is selected and pulverized, and then the pulverized biomass is impregnated into the aqueous solution, wherein the aqueous solution may be formed to be acidic or basic.

More specifically, the pulverized biomass may be impregnated with 0.1 to 100% of an acidic or basic aqueous solution at a weight ratio of 1: 0.1 to 1:10 for 10 minutes to 120 hours after the pulverization of the cellulosic biomass .

Preferably, the well-dried kenaf stems are selected and pulverized, and the pulverized kenaf can be impregnated in a 20 to 85% aqueous phosphoric acid solution at a weight ratio of 1: 0.5 to 1:10 for 12 to 48 hours.

If the concentration of the aqueous solution is less than 0.1%, the biomass may not be sufficiently activated after the impregnation step. If the concentration exceeds 100%, the viscosity may increase, Resulting in a problem that may occur.

When the weight ratio of the aqueous solution is less than 0.1 part by weight, the biomass may not be sufficiently activated after the impregnation step. When the weight ratio of the aqueous solution is more than 10 parts by weight, the biomass is sufficiently impregnated, There is a problem that efficiency is not increased and it is inefficient.

In addition, if the impregnation is performed for less than 12 hours, there may arise a problem that the biomass is not sufficiently activated after the impregnation step, and when the impregnation time exceeds 48 hours, the biomass is sufficiently impregnated, There is a problem that it is inefficient.

Next, the charging step (S200) is a step of transferring the impregnated biomass into the crucible and charging it into the furnace, wherein the furnace may be formed of alumina material and the furnace interior may be filled with active or inert gas have.

Preferably, the impregnated kenaf is transferred to a crucible and then charged into the furnace. The furnace interior may be filled with at least one of nitrogen (N2), argon (Ar), and helium (He).

Alumina is characterized by high electrical insulation and does not cause dielectric breakdown, and is excellent in heat resistance, chemical resistance, strength, hardness and dielectric strength as well as high thermal conductivity.

Since the inert gas is colorless, odorless, tasteless, inert, and nonflammable, it can prevent oxidation and nitrification which may be caused by contact with air during the production of active carbon, so that it is possible to manufacture high- have.

Next, the activation step S300 is a step of heating the furnace to activate the biomass charged into the furnace. More specifically, the furnace is heated to 100 to 1000 DEG C at a heating rate of 1 to 30 DEG C / min, The heating temperature may be maintained for 5 to 120 minutes to activate the impregnated biomass.

Preferably, the furnace can be activated by heating the furnace at a heating rate of 1 to 10 ° C / min to 400 to 800 ° C, and then heating the furnace for 30 to 120 minutes to impregnate the furnace Lt; / RTI > can be activated.

At this time, when the heating rate is less than 1 ° C / min, there is a problem that the activation rate is lowered and productivity is decreased. When the heating rate is more than 30 ° C / min, thermal stress is applied to the biomass, Can occur.

Also, when the heating temperature is 100 to 1000 ° C, medium pitches having a diameter of 2 to 50 nm can be formed, and the output characteristics can be improved according to the formation of the medium pitch.

If the heating temperature is less than 100 ° C., there may arise a problem that the medium holes are not formed sufficiently. If the heating temperature is more than 1000 ° C., the medium holes may collapse and the micropore may be formed, have.

Next, the cooling step (S400) is a step of cooling the activated biomass to room temperature (15 to 25 DEG C), and more particularly, the activated biomass can be cooled at a constant rate.

Preferably, the activated kenaf can be cooled naturally to a temperature of 18 to 25 占 폚 or at a rate of 2 to 5 占 폚 / min.

At this time, it is preferable to keep the internal gas atmosphere in an inert gas atmosphere at a stable temperature of 250 deg. C or less, which will not cause additional oxidation, even when the temperature is lowered.

It is also possible to forcefully collect activated biomass at temperatures of 100-300 ° C without cooling down to 15-25 ° C, but additional cooling is required after harvesting.

Next, the washing step (S500) is a step of washing the cooled biomass with a washing solution to produce activated carbon. The cooled activated kenaf is stirred in a washing solution at room temperature (15 to 25 ° C) to 150 ° C, The activated carbon can be produced by repeating the reaction 1 to 20 times.

When the acidic aqueous solution is used in the impregnation step (S100), the cleaning solution is an alkali solution. When a basic aqueous solution is used, the cleaning solution may be a solution of distilled water and an alkali or acid solution of 0.01 to 5 mol / It is preferable that it is formed of an acidic solution.

More specifically, the wash liquor may be formed of an alkali or acidic solution having a molar concentration of 0.01 to 5 mol / L, and when the wash liquor is formed of an alkali or an acidic solution, the wash liquor is 2-4 times faster Lt; / RTI >

Preferably, the cooled kenaf is agitated at 50 to 100 DEG C with a washing solution formed of distilled water, purified water and one of an alkali or acidic solution having a molar concentration of 1 to 2 mol / L, and the process is repeated 1 to 20 times To produce activated carbon.

At this time, when the washing is completed, it is preferable that the pH of the activated carbon washing solution is about 6 to 7 neutral.

According to this, as shown in the following Table 3, it can be seen that the mesopore ratio has excellent pores of 40% or more of the total pore volume.

In addition, as shown in FIG. 6, active carbon having a better flow of electron ions and superior electrochemical characteristics can be produced compared to conventional commercial activated carbon.

The activated carbon for high output energy storage according to the present invention can be used for manufacturing an electrode for a capacitor, and then an electrode for a capacitor can be processed to manufacture an electric double layer capacitor.

More specifically, it is possible to use polytetrafluoroethylene (PTFE) as a binder, Super-P of Timcal as a conductive material, and the activated carbon for high-energy storage of the present invention as an activated carbon. In this case, , Conductive material, and activated carbon may be mixed at a weight ratio of 5:10:85 to prepare a mixture.

The mixture is put into a mixture of distilled water and isopropyl alcohol at a ratio of 10: 1, and the mixture is stirred at 3,000 RPM for 30 minutes using a homogenizer. The mixture is placed in an aluminum tray and allowed to stand in an oven at 150 ° C for 12 hours.

1 to 3 ml of isopropyl alcohol is added to the dried mixture, kneaded, rolled using a hand operated roller, and pressed to a rolled mixture using a 120 ° C hot roll press to make a sheet electrode having a thickness of 150 μm .

Thereafter, a conducting paste was applied to the etched aluminum current collector having a thickness of 20 탆 to a thickness of 5 탆, the prepared sheet electrode was attached, and pressurized at 120 캜 hot roll press to manufacture a capacitor electrode.

Next, an electrode for a capacitor was processed to produce an electric double layer capacitor.

More specifically, a capacitor electrode was drilled at 12 mm to form a coin cell type electrode. Cellulose of NKK Co., Ltd., Japan was drilled at 18 mm to prepare a separator. A separator was fabricated from a coin assembly kit having a diameter of? 20 mm and a height of 3.2 mm To prepare a cell.

Then, 1 M spirobipyrrolidinium tetrafluoroborate (SBPBF4) was used as an electrolyte, and propylene carbonate was used as a solvent, and a coin type cell electric double layer capacitor was prepared using the same.

Further, in order to improve the high output density and produce high output characteristics by facilitating the movement of the electron ions in the production of the electric double layer capacitor using the commercially available activated carbon, the high output energy storage activated carbon and the conventional commercial activated carbon are mixed at a ratio of 0.01: 99.9 wt.% to 99.9: 0.01 wt.%, to prepare an electric double layer capacitor.

The commercially available activated carbon may include one or more of YP-50F, YP-FW, CEP21KS, and MSP-20, but this is only an embodiment of the present invention, and other commercially available activated carbon may be used.

Preferably, as shown in the following Tables 4 and 5, when the mixing ratio of the high-power energy storage activated carbon is larger than a certain ratio, the electrode density is decreased due to the pore characteristics of the high-power energy storage activated carbon , it is possible to mix 10 to 30 wt% of the active carbon for high energy storage of the present invention with conventional commercial activated carbon because the performance is lowered.

Hereinafter, the present invention will be described in more detail with reference to the following examples, but they should be construed as merely illustrative of preferred embodiments of the present invention, and the examples do not limit the scope of the present invention.

[ Example ]

The well-dried kenaf stalks having a hard particle shape were selectively pulverized, and the pulverized kenaf was impregnated in a 50% aqueous solution of phosphoric acid at a weight ratio of 1: 5 for 12 to 48 hours. The impregnated kenaf was transferred into a crucible and charged into a furnace made of alumina. The furnace was heated to 600 ° C at a heating rate of 5 ° C / min and maintained for 85 minutes to activate the impregnated kenaf. The activated kenaf was spontaneously cooled to 20 ° C and washed with an alkali solution having a molar concentration of 2 mol / L to prepare activated carbon for high-power energy storage.

(PTFE) as a binder, Super-P of Timcal Co. as a conductive material, activated carbon for high-power energy storage using activated carbon, and a binder, a conductive material, and an activated carbon at a ratio of 5:10:85 By weight to prepare a mixture. The mixture was poured into a mixed solution of distilled water and isopropyl alcohol at a weight ratio of 10: 1, and then mixed using a homogenizer at 3,000 RPM for 30 minutes. The mixture was placed in an aluminum tray and allowed to stand in an oven at 150 ° C for 12 hours. 1 to 3 ml of isopropyl alcohol was added to the dried mixture, kneaded, rolled using a hand operated roller, and the rolled mixture was pressurized using a hot roll press at 120 占 폚 to make a sheet electrode having a thickness of 150 占 퐉. Thereafter, conductive paste (thickness: 5 탆) was applied to the etched aluminum current collector having a thickness of 20 탆, and then the prepared sheet electrode was attached and pressed by a hand operated roller to manufacture a capacitor electrode.

The electrode for a capacitor was drilled to a diameter of 12 mm to be processed into an electrode of a coin cell type. Cellulose of NKK Co., Ltd. of Japan was perforated with a diameter of 18 mm to prepare a separator. Using a coin assembly kit having a diameter of? 20 mm and a height of 3.2 mm, . Coin type cell electric double layer capacitors were prepared by using 1 M spirobipyrrolidinium tetrafluoroborate (SBPBF4) as electrolyte and propylene carbonate as solvent.

[ Comparative Example  One]

An electric double-layer capacitor was prepared by using YP-50F instead of activated carbon for high-power energy storage in the production of electrodes for capacitors of the Examples.

[ Comparative Example  2]

An electric double-layer capacitor was prepared by using YP-FW instead of activated carbon for high-power energy storage in the production of the electrode for a capacitor in the examples.

[ Comparative Example  3]

An electric double layer capacitor was prepared by using CEP21KS in place of activated carbon for high output energy storage in the production of electrode for a capacitor in the examples.

[ Comparative Example  4]

In the preparation of the electrode for a capacitor of the example, an electric double layer capacitor was prepared by mixing 90 wt% of YP-50F and 10 wt% of active carbon for high-power energy storage instead of activated carbon for high output energy storage.

[ Comparative Example  5]

In the preparation of the electrodes for capacitors of the examples, an electric double layer capacitor was prepared by mixing 80 wt% of YP-50F and 20 wt% of active carbon for high-power energy storage instead of activated carbon for high output energy storage.

[ Comparative Example  6]

In the preparation of the electrode for capacitors of the examples, an electric double layer capacitor was prepared by mixing 70wt% of YP-50F and 30wt% of active carbon for high-energy storage instead of high-energy storage activated carbon.

[ Comparative Example  7]

In the preparation of the capacitor electrode of the example, an electric double layer capacitor was prepared by mixing 60 wt% of YP-50F and 40 wt% of active carbon for high-energy storage instead of high-energy storage activated carbon.

[ Comparative Example  8]

In the preparation of the electrodes for capacitors of the examples, an electric double-layer capacitor was prepared by mixing 50 wt% of YP-50F and 50 wt% of high-energy-storing activated carbon instead of activated carbon for high-power energy storage.

[ Comparative Example  9]

In the preparation of the electrodes for capacitors of the Examples, an electric double layer capacitor was prepared by mixing 30 wt% of YP-50F and 70 wt% of active carbon for high-energy storage instead of high-energy storage activated carbon.

[ Comparative Example  10]

An electric double layer capacitor was prepared by mixing 90 wt% of CEP21KS and 10 wt% of active carbon for high energy storage instead of high power energy storage activated carbon at the time of manufacturing the capacitor electrode of the embodiment.

[ Comparative Example  11]

In the preparation of the electrodes for capacitors of the Examples, an electric double layer capacitor was prepared by mixing 80 wt% of CEP21KS and 20 wt% of active carbon for high energy storage instead of high power energy storage activated carbon.

[ Comparative Example  12]

In the preparation of the electrode for a capacitor of the Example, an electric double layer capacitor was prepared by mixing 70 wt% of CEP21KS and 30 wt% of active carbon for high energy storage instead of high power energy storage activated carbon.

[ Comparative Example  13]

An electric double layer capacitor was prepared by mixing 60wt% of CEP21KS and 40wt% of active carbon for high energy storage, instead of high power energy storage activated carbon, in the capacitor electrode of the embodiment.

[ Comparative Example  14]

An electric double layer capacitor was prepared by mixing 50 wt% of CEP21KS and 50 wt% of active carbon for high energy storage instead of high power energy storage activated carbon for the capacitor electrode of the embodiment.

[ Comparative Example  15]

In the preparation of the electrode for a capacitor according to the embodiment, an electric double layer capacitor was prepared by mixing 30 wt% of CEP21KS and 70 wt% of active carbon for high energy storage instead of high power energy storage activated carbon.

[ Test Example  One] Activated carbon  Analysis of pore characteristics

In order to analyze the pore characteristics of the prepared activated carbon, the examples, Comparative Examples 1 and 2 were deaerated at 573 K for 6 hours while maintaining the residual pressure at 10 -3 torr or less, and then adsorbed to the isothermal adsorption apparatus (BELSORP-max, BEL JAPAN, (N2) gas was measured at 77 K according to the relative pressure (P / P0), and the specific surface area of activated carbon was calculated. The results are shown in FIG.

According to Fig. 2, it is confirmed that the adsorption amount of nitrogen (N ₂ ) gas according to the comparative example 1 and 2 is superior to that according to the comparative example (P / P ₀ ).

Further, the calculation results are shown in Table 1 below.

Samples BET
[m ² / g] Total pore volume
[cm ³ / g] Micropore volume
[cm ³ / g] Mesopore volume
[cm ³ / g] Fraction of Mesopore volume [%] Comparative Example 1 1777 0.83 0.66 0.17 20.5 Comparative Example 2 1818 0.91 0.65 0.26 28.6 Example 1939 3.18 0.38 2.80 88.0

Table 1 is a table showing the results of active carbon pore analysis, and it can be confirmed that the examples have higher specific surface area than Comparative Examples 1 and 2. Thus, it was confirmed that the total pore volume of the Example was three times or more higher than that of Comparative Examples 1 and 2.

Also, in Comparative Examples 1 and 2, although the micropore volume has a higher distribution than the mesopore volume, it can be confirmed that the mesopore volume of the embodiment is much higher than the micropore volume.

From the viewpoint of the mesopore volume fraction (Mesopore volume / total pore volume X 100), it can be confirmed that the mesopore volume ratio is four times higher than that of Comparative Example 1 and three times higher than that of Comparative Example 2, Of the total pore volume is 40% or more of the total pore volume.

Therefore, it can be seen that the medium pitch is formed at a high ratio in the embodiment, and thus the electrolyte of the embodiment smoothly moves within the electrode active material structure during the high-speed charge and discharge, compared with the electrolytes of the comparative examples 1 and 2, It can be seen that it has higher electrochemical output characteristics than Examples 1 and 2.

 Further, according to Fig. 3, the pore sizes of Comparative Examples 1 and 2 are mostly distributed in a range of 2 nm or less, but in the embodiment, the pore distribution at 2 to 50 nm is high and the pore sizes exceeding 100 nm are distributed in large numbers Able to know.

Therefore, in the case of the embodiment, since a high proportion of the mesopores is formed and the micropores and the mesopores are distributed at an appropriate ratio, the electrolytes of the examples are higher in the electrode active material structure than the electrolytes of the comparative examples 1 and 2 It can be seen that the examples have higher electrochemical output characteristics than those of Comparative Examples 1 and 2.

[ Test Example  2] Activated carbon  Electrochemical Characteristic Analysis 1

CV (Cyclic Voltammetry) test was carried out at a scanning speed of 50-500 mV / sec using a French bio logic science instrument (VSP-300) for the Examples and Comparative Examples 1 and 2, preferably 400 mV / sec (Cyclic Voltammetry) test was performed at a scanning speed of 10 m / sec. The results are shown in Fig.

According to FIG. 4, when the CV (Cyclic Voltammetry) is measured at a scanning speed of 400 mV / sec, the graph of the embodiment shows a shape closer to a rectangle than that of the graphs of Comparative Examples 1 and 2.

As a result, it can be seen that the embodiment has higher capacity and efficiency as compared with Comparative Examples 1 and 2.

[ Test Example  3] Activated carbon  Electrochemical Characterization 2

For Examples and Comparative Examples 1 and 2, discharge and charge tests were conducted by charging and discharging by a constant current method using a charge and discharge device (MACCOR 4300K DESKTOP) manufactured by MACCOR, USA.

In this case, the driving voltage was 0 to 2.5 V and the applied current density was 100 to 100 cycles per 100 to 500 mA / cm 2. The electrostatic capacity of the electric double layer capacitor was calculated by the following equation in the 100th constant current discharge.

Capacitance (F) = Δtdicharge · I / ΔV

The calculated value according to the above formula is shown in Fig.

5, it was confirmed that the capacity retention rate of Comparative Examples 1 and 2 was reduced by 10% or more from the time when the current per unit area was applied at a current density of 150 mA / cm 2 compared with the Example.

However, in the case of the example, it was confirmed that the capacity retention ratio was as high as 8 to 9% even at a current density of 300 mA / cm 2.

As a result, it was confirmed that the output characteristics of the electric double-layer capacitors of the Examples were superior to those of the electric double-layer capacitors of Comparative Examples 1 and 2.

[ Test Example  4] Depending on the power density Non-capacity  Measure 1

For Comparative Examples 1 to 9 and Examples, charging and discharging were carried out by a constant current method using a MACCOR 4300K DESKTOP, manufactured by MACCOR, USA, in order to measure a specific capacity according to the output density.

At this time, the driving voltage from 0 to 2.5V, the applied current density was measured by 10cycle under the condition of 1 ~ 10A g ^-1, 10 second measurement of the capacitance of the electric double layer capacitor at a constant current discharge, and the output density by the following equation And the calculated values are shown in [Table 2].

Specific Capacitance (F g ^-1 ) = Δ tdischarge · I / ΔV · (m ⁺ + m ^- )

(m +): mass of the active material of the cathode

(m ^- ): mass of the active material of the anode

Samples Specific Capacitance [F g ^-1 ] 1A g ^-1 3A g ^-1 5A g ^-1 7A g ^-1 10A g ^-1 Comparative Example 1 15.46 11.92 8.79 5.96 3.48 Comparative Example 4 21.48 17.87 15.40 11.78 8.25 Comparative Example 5 23.05 19.89 17.35 14.82 11.11 Comparative Example 6 26.98 24.26 21.69 19.11 15.19 Comparative Example 7 25.56 23.64 22.55 20.23 17.16 Comparative Example 8 24.32 23.45 22.64 20.85 17.30 Comparative Example 9 23.68 21.98 20.87 18.93 16.95 Example 20.73 18.96 18.01 16.67 14.87

Table 2 shows the specific capacity according to the output density in the YP-50F blend production. It can be seen from the above that the cost amount according to the output density of Comparative Example 6 is the highest, and therefore, it can be seen that the cost amount when 30 wt% of the high-energy storage activating carbon is added to the commercially available activated carbon YP-50F is the highest .

[ Test Example  5] Depending on power density Non-capacity  Measure 2

For Comparative Examples 3, 10 to 15 and Examples, charging and discharging were carried out by a constant current method using a MACCOR 4300K DESKTOP (a MACCOR 4300K DESKTOP) manufactured by MACCOR, USA, in order to measure a specific capacity according to power density.

At this time, the driving voltage from 0 to 2.5V, the applied current density was measured by 10cycle under the condition of 1 ~ 10A g ^-1, 10 second measurement of the capacitance of the electric double layer capacitor at a constant current discharge, and the output density by the following equation And the calculated values are shown in [Table 3].

Specific Capacitance (F g ^-1 ) = Δ tdischarge · I / ΔV · (m ⁺ + m ^- )

(m ⁺ ): mass of the active material of the cathode

(m ^- ): mass of the active material of the anode

Samples Specific Capacitance [F g ^-1 ] 1A g ^-1 3A g ^-1 5A g ^-1 7A g ^-1 10A g ^-1 Comparative Example 3 23.64 17.59 12.75 8.48 4.16 Comparative Example 10 28.54 26.35 21.56 17.64 13.88 Comparative Example 11 31.27 27.32 23.87 20.77 16.31 Comparative Example 12 33.23 31.05 28.93 25.14 22.12 Comparative Example 13 31.13 29.26 27.87 25.84 23.45 Comparative Example 14 29.56 27.33 26.55 25.76 23.68 Comparative Example 15 27.87 25.75 25.95 23.59. 22.34 Example 20.73 18.96 18.01 16.67 14.87

Table 3 is a table showing the specific capacity according to the output density in the production of CEP21KS blend, and it can be seen that the cost amount according to the output density of Comparative Example 12 is the highest. Therefore, it can be seen that the highest cost is obtained when 30 wt% of high-energy-storing activated carbon is added to commercially available activated carbon CEP21KS.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention may be embodied in many other specific forms without departing from the spirit or essential characteristics thereof. The embodiments described above are therefore to be considered in all respects as illustrative and not restrictive.

Claims (10)

A method for producing activated carbon for high power energy storage,
A step of pulverizing the cellulosic biomass and impregnating the pulverized biomass into an aqueous solution;
Charging the impregnated biomass into a furnace;
An activation step of heating the furnace to activate the charged biomass;
A cooling step of cooling the activated biomass;
And washing the cooled biomass with a washing solution to produce activated carbon,
The furnace includes:
The interior is filled with an active or inert gas,
In the impregnating step,
The pulverized biomass is impregnated in an acidic or basic aqueous solution having a concentration of 0.1 to 100% for 10 minutes to 120 hours, wherein the biomass and the aqueous solution are impregnated at a weight ratio of 1: 0.1 to 1:10,
Wherein,
The furnace is heated to a temperature of 100 to 1000 ° C. at a heating rate of 1 to 30 ° C./min and then the heating temperature is maintained for 5 to 120 minutes to activate the impregnated biomass,
The cleaning liquid,
An alkali or acidic solution having a molar concentration of 0.01 to 5 mol / L,
Wherein the acid solution is used as an alkaline solution when the acidic aqueous solution is used in the impregnation step and the acidic solution is used when a basic aqueous solution is used in the impregnation step.
delete delete The method according to claim 1,
The cooling step includes:
Wherein the activated biomass is cooled to room temperature.
delete The method according to claim 1,
The cleaning step comprises:
Wherein the cooled biomass is agitated in a washing solution at a temperature ranging from room temperature to 150 ° C., and the process is repeatedly performed 1 to 20 times.
The method according to claim 1,
The activated carbon,
Wherein the medium-to-high air ratio is greater than or equal to 40% of the total volume of the gun.
A high output energy storage activated carbon produced by the method of any one of claims 1, 4, 6 and 7.
An electric double layer capacitor according to claim 8, which is produced by the high-energy-storing activated carbon.
10. The method of claim 9,
Wherein the electric double layer capacitor comprises:
Wherein the high power energy storage activated carbon and the conventional commercially available activated carbon are mixed at a ratio of 0.01: 99.9 wt% to 99.9: 0.01 wt%.

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