KR100716032B1 - Apparatus and method for producing catalyst and Cobalt and Platinum supported catalyst using Carbon nano fibers for fuel cell - Google Patents

Abstract

The present invention relates to an apparatus and method for producing a cobalt-platinum catalyst for a fuel cell using carbon nanofibers, the composition of which includes a nitrate solution in which a plurality of carbon nanofibers are immersed and pickled to remove impurities from the carbon nanofibers Housed pickling treatment tank; An ultrasonic generator for dispersing ultrasonic waves in the carbon nanofibers soaked in the nitric acid solution to prevent entanglement between the plurality of carbon nanofibers; A thermostat containing 60 ° C. to 80 ° C. water in which the pickling treatment tank is immersed; A filter for removing nitric acid solution remaining in the carbon nanofibers soaked in the pickling treatment tank; A water washing tank containing distilled water in which the carbon nanofibers from which nitric acid solution has been removed are soaked and washed with water; A first oven member for drying the carbon nanofibers by heating the carbon nanofibers in an amount of about 100 ° C. to 150 ° C. in order to remove residual moisture of the water washed carbon nanofibers; A first bath in which the dried carbon nanofibers are immersed and acetone solvent containing platinum ions dispersed by platinum hydrate and dispersed by an ultrasonic cleaner is accommodated; A first sealing member for sealing the first bath in which the carbon nanofibers are soaked to allow the carbon nanofibers to sufficiently adsorb the platinum ions and to prevent impurities from entering; A first rotary evaporator for treating the first bath in a water bath at 65 ° C. to 100 ° C. to evaporate the acetone solvent in the first bath; A second oven member for drying the carbon nanofibers on which the platinum ions are adsorbed and dried by heating the carbon nanofibers on which the platinum ions are adsorbed at about 100 ° C. to 120 ° C .; A first hydrogen reduction device for reducing the platinum ions supported on the carbon nanofibers to platinum; A second bath in which the carbon nanofibers carrying the platinum are immersed and in which acetone solvent containing iron ions dispersed by an ultrasonic washing machine containing iron hydrate is contained; A second sealing member for sealing the second bath in which the carbon nanofibers carrying the platinum are immersed so that the carbon nanofibers adsorbing the platinum can sufficiently adsorb the iron ions and prevent impurities from entering; A second rotary evaporator for treating the second bath in a water bath at 65 ° C. to 100 ° C. to evaporate the acetone solvent in the second bath; A third oven member for heating and drying the carbon nanofibers carrying the iron ions and the platinum at about 100 ° C. to 120 ° C. to dry the carbon nano fibers in which the iron ions and the platinum are deposited; And a second hydrogen reduction device for reducing the iron ions adsorbed to the carbon nanofibers carrying the iron ions and the platinum to iron, from which high-performance, high-efficiency, high stability cobalt-platinum is formed. It is possible to produce a catalyst, there is an effect that the manufacturing cost can be reduced.

Description

Apparatus and method for producing catalyst and Cobalt and Platinum supported catalyst using Carbon nano fibers for fuel cell}

1 is a conceptual view sequentially showing a cobalt-platinum supported catalyst manufacturing apparatus for a fuel cell using carbon nanofibers according to an embodiment of the present invention.

FIG. 2 is a conceptual view illustrating the first hydrogen reduction device of FIG. 1 in detail. FIG.

3 a and b are conceptual views illustrating a cobalt-platinum supported catalyst for a fuel cell manufactured by a cobalt-platinum supported catalyst manufacturing apparatus for a fuel cell using the carbon nanofibers of FIG. 1.

Figure 4 is a flow chart sequentially showing a method for preparing a cobalt-platinum supported catalyst for a fuel cell using carbon nanofibers according to a preferred embodiment of the present invention.

<Explanation of symbols for the main parts of the drawings>

10: pickling treatment tank 20: ultrasonic generator

30: thermostat 40: filter

50: water washing treatment tank 60: first oven member

70,70 ': First and second tank 75,75': First and second sealing member

80,80 ': 1st, 2nd rotary evaporator 90,90': 2nd, 3rd oven member

95,95 ': 1st and 2nd hydrogen reduction device 951: 1st quartz tube

953: first nitrogen gas introduction unit 955: first hydrogen gas introduction unit

957: first gas exhaust 959: first heating coil

The present invention relates to a cobalt-platinum catalyst production apparatus and method for a fuel cell using carbon nanofibers.

A fuel cell is a power generation element that converts chemical energy of fuel into electrical energy. Recently, research on using a fuel cell as a power supply source for automobiles, houses, and mobile devices has been conducted. In such fuel cells, research on electrodes, fuels, and electrolyte membranes has been actively conducted to increase energy density to improve output density and output voltage. In particular, attempts to increase the reactivity of catalysts to improve the conductivity of electrodes have been made. have. The performance of the electrode is greatly influenced by the ease of mass transfer, such as the diffusion of reactants into the catalyst bed and the discharge of reaction products, which improves as the reaction surface area of the catalyst increases. Therefore, in order to increase the reactivity of the catalyst present in the electrode, it is necessary to reduce the particle diameter of the catalyst to a size of several nm to increase the reaction surface area. In addition, the development of carriers for effective uniform dispersion of catalysts is also rapidly progressing. In particular, heterogeneous catalysts are generally unstable due to heat treatment temperature or reaction temperature during the manufacturing process, and it is a common method to disperse them in carriers.

As described above, carbon black and activated carbon have been commonly used as a carrier for catalysts to increase the reactivity of the catalyst for fuel cells. Such carbon black or activated carbon is vulnerable to oxidizing agents and has low mechanical strength. Impurity can be contained during the manufacturing process due to plugging phenomenon, easy to deteriorate, unstable under high temperature condition reaction as a porous oxide, and desorption phenomenon occurs easily due to concentration change, temperature and pressure. There is a problem that clogging may occur when the structure of the carrier is broken in the reactor is low.

The present invention has been made to solve the above-described problems, the cobalt-platinum catalyst manufacturing apparatus for fuel cells using carbon nanofibers can manufacture a high-performance, high-efficiency, high stability cobalt-platinum catalyst, the production cost can be reduced And to provide a method.

The cobalt-platinum supported catalyst manufacturing apparatus for a fuel cell using the carbon nanofiber of the present invention for achieving the above object is, in order to remove impurities of the carbon nanofiber, a plurality of carbon nanofibers are nitrate solution which is pickled and pickled Housed pickling treatment tank; An ultrasonic generator for dispersing ultrasonic waves in the carbon nanofibers soaked in the nitric acid solution to prevent entanglement between the plurality of carbon nanofibers; A thermostat containing 60 ° C. to 80 ° C. water in which the pickling treatment tank is immersed; A filter for removing nitric acid solution remaining in the carbon nanofibers soaked in the pickling treatment tank; A water washing tank containing distilled water in which the carbon nanofibers from which nitric acid solution has been removed are soaked and washed with water; A first oven member for drying the carbon nanofibers by heating the carbon nanofibers in an amount of about 100 ° C. to 150 ° C. in order to remove residual moisture of the water washed carbon nanofibers; A first bath in which the dried carbon nanofibers are immersed and acetone solvent containing platinum ions dispersed by platinum hydrate and dispersed by an ultrasonic cleaner is accommodated; A first sealing member for sealing the first bath in which the carbon nanofibers are soaked to allow the carbon nanofibers to sufficiently adsorb the platinum ions and to prevent impurities from entering; A first rotary evaporator for treating the first bath in a water bath at 65 ° C. to 100 ° C. to evaporate the acetone solvent in the first bath; A second oven member for drying the carbon nanofibers on which the platinum ions are adsorbed and heated by drying the carbon nanofibers on which the platinum ions are adsorbed at about 100 ° C. to 120 ° C .; A first hydrogen reduction device for reducing the platinum ions supported on the carbon nanofibers to platinum; A second bath in which the carbon nanofibers carrying the platinum are immersed and in which acetone solvent containing cobalt ions dispersed by ultrasonic cleaning is accommodated by cobalt hydrate; A second sealing member for sealing the second tank in which the carbon nanofibers carrying the platinum are loaded so that the carbon nanofibers adsorbing the platinum sufficiently adsorb the cobalt ions and prevent impurity incorporation; A second rotary evaporator for treating the second bath in a water bath at 65 ° C. to 100 ° C. to evaporate the acetone solvent in the second bath; A third oven member for drying the cobalt ions and the platinum-carrying carbon nanofibers by heating the cobalt ions and the platinum-carrying carbon nanofibers at about 100 ° C. to about 120 ° C .; And a second hydrogen reduction device for reducing the cobalt ions adsorbed onto the carbon nanofibers adsorbed with the cobalt ions and the platinum to cobalt.

In the above, the first hydrogen reduction device, the first quartz tube in which the carbon nanofibers adsorbed the platinum ions are charged into the interior; A first nitrogen gas introduction part connected to the first quartz tube to supply nitrogen gas into the first quartz tube and having a first flow regulator; A first hydrogen gas introduction part connected to the first quartz tube to supply hydrogen gas into the first quartz tube and having a second flow regulator; A first gas exhaust part connected to the first quartz tube to discharge gas after a hydrogen reduction reaction; And a first heating coil installed outside the first quartz tube to heat the inside of the first quartz tube to 900 ° C. to 1200 ° C., wherein the second hydrogen reduction device includes the cobalt ion and the A second quartz tube into which carbon nanofibers adsorbed platinum are charged into the interior; A second nitrogen gas introduction part connected to the second quartz tube to supply nitrogen gas into the second quartz tube and having a third flow controller; A second hydrogen gas introduction part connected to the second quartz tube to supply hydrogen gas into the second quartz tube and having a fourth flow regulator; A second gas exhaust part connected to the second quartz tube to discharge gas after a hydrogen reduction reaction; And a second heating coil installed outside the second quartz tube and heating the inside of the second quartz tube to 500 ° C to 650 ° C.

On the other hand, cobalt-platinum supported catalyst production method for a fuel cell using the carbon nanofiber of the present invention for achieving the above object, (a) in order to remove impurities of the carbon nanofiber, the carbon nanofiber is pickled with a nitric acid solution Pickling and soaking in a treatment tank; (b) dispersing ultrasonic waves in the pickling bath of step (a) to prevent entanglement between the plurality of carbon nanofibers; (c) putting the pickling treatment tank of step (b) into a thermostatic bath containing water of 60 ° C. to 80 ° C. to boil; (d) filtering the carbon nanofibers to remove nitric acid solution remaining in the carbon nanofibers; (e) washing the carbon nanofibers with water; (f) drying the carbon nanofibers by heating the carbon nanofibers in an amount of about 100 ° C. to 150 ° C. to remove moisture remaining in the carbon nanofibers; (g) injecting the carbon nanofibers into a tank containing acetone solvent containing platinum ions dispersed by platinum hydrate; (h) sealing the water tank of step (g) to allow the carbon nanofibers to sufficiently adsorb the platinum ions; (i) treating the bath with a water bath at 65 ° C. to 100 ° C. to evaporate the acetone solvent in the bath of step (h); (j) drying the carbon nanofibers by heating the carbon nanofibers at about 100 ° C. to about 120 ° C. to dry the carbon nanofibers onto which the platinum ions are adsorbed; (k) reducing the platinum ions adsorbed on the carbon nanofibers to platinum using a first hydrogen reduction device; (l) injecting the carbon nanofibers carrying the platinum obtained in step (k) into a water bath containing acetone solvent containing cobalt ions dispersed by cobalt hydrate; (m) sealing the water tank of step (l) so that the platinum-supported carbon nanofibers can sufficiently adsorb the cobalt ions; (n) treating the water bath with a water bath at 65 ° C. to 100 ° C. to evaporate the acetone solvent in the water tank of step (m); (o) heating the carbon nanofibers carrying the cobalt ions and the platinum to a temperature of about 100 ° C. to 120 ° C. to dry the carbon nanofibers carrying the cobalt ions and the platinum; And (p) reducing the cobalt ions adsorbed onto the carbon nanofibers carrying the cobalt ions and the platinum to the cobalt using a second hydrogen reduction device.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

An apparatus for preparing a cobalt-platinum catalyst for a fuel cell using carbon nanofibers according to an embodiment of the present invention will be described.

1 is a conceptual view sequentially showing an apparatus for preparing a cobalt-platinum supported catalyst for a fuel cell using carbon nanofibers according to an embodiment of the present invention, and FIG. 2 is a conceptual view illustrating the first hydrogen reduction apparatus of FIG. 1 in detail. 3A and 3B are conceptual views illustrating a cobalt-platinum supported catalyst for a fuel cell manufactured by a cobalt-platinum supported catalyst manufacturing apparatus for a fuel cell using the carbon nanofibers of FIG. 1.

As shown in FIG. 1, an apparatus for preparing a cobalt-platinum supported catalyst for fuel cells using carbon nanofibers according to an embodiment includes a pickling treatment tank 10a, an ultrasonic generator 20a, a thermostat 30a, a filter 40a, and a water washing treatment. Tank 50a, first oven member 60a, first water tank 70a, first sealing member 75a, first rotary evaporator 80a, second oven member 90a, and first hydrogen Reduction device 95a, second water tank 70a ', second sealing member 75a', second rotary evaporator 80a ', third oven member 90a' and second hydrogen reduction device 95a ') Is done.

A large number of carbon nanofibers (CNFs) are introduced into the pickling treatment tank 10a, and in order to remove impurities of the carbon nanofibers (CNFs), carbon nanofibers (CNFs) are immersed in a 30% concentration of nitric acid ( HNO ₃ ) solution is contained.

A large number of carbon nanofibers (CNFs) are immersed in the nitric acid solution contained in the pickling treatment tank 10a, and the carbon nanofibers (CNFs) are pickled to remove impurities such as inorganic and organic substances, and carbon nanofibers are removed. The surface area of the fibers (CNFs) and the volume of the pores are increased to increase the adsorption capacity and dispersibility of cobalt ions and platinum ions described later.

The ultrasonic generator 20a disperses ultrasonic waves in carbon nanofibers (CNFs) immersed in nitric acid solution to prevent entanglement between a plurality of carbon nanofibers (CNFs).

The thermostatic bath 30a contains water at 60 ° C to 80 ° C, and the pickling treatment tank 10a is immersed in the water.

The filter 40a removes the nitric acid solution remaining in the carbon nanofibers (CNFs) immersed in the pickling treatment tank 10a.

The water washing tank 50a contains distilled water in which carbon nanofibers (CNFs) from which nitric acid solution has been removed are immersed and washed with water.

By this washing process, carbon nanofibers (CNFs) are returned to almost neutral conditions.

The first oven member 60a heats the carbon nanofibers CNFs at about 100 ° C. to 150 ° C. to remove residual moisture of the carbon nanofibers CNFs.

As a platinum hydrate, [Pt (NH ₃ ) ₂ (H ₂ O) ₂ Cl ₂ ] Br ₂ was introduced into the first tank 70a to contain acetone solvent containing platinum ions (Pt ²⁺ ) dispersed by ultrasonic waves. The carbon nanofibers (CNFs) dried in the acetone solvent are soaked.

The above [Pt (NH ₃ ) ₂ (H ₂ O) ₂ Cl ₂ ] Br ₂ is one embodiment of the platinum hydrate, and may vary depending on the embodiment.

The first sealing member 75a seals the first water tank 70a in which the carbon nanofibers CNFs are immersed in order to allow the carbon nanofibers CNFs to sufficiently adsorb platinum ions and to prevent impurity incorporation.

The first rotary evaporator 80a treats the first bath 70a in water at 65 ° C to 100 ° C to evaporate the acetone solvent in the first bath 70a.

The second oven member 90a heats the carbon nanofibers CNFs at about 100 ° C. to about 120 ° C. in order to dry the carbon nanofibers CNFs on which platinum ions are adsorbed.

The first hydrogen-reduction device (95a) causes a reduction of the platinum supported on carbon nanofibers (CNFs) on (Pt ^{2 +)} with platinum (Pt).

As illustrated in FIG. 5, the first hydrogen reduction device 95a includes a first quartz tube 951a, a first nitrogen gas introduction unit 953a, a first hydrogen gas introduction unit 955a, and a first gas exhaust unit ( 957a) and the first heating coil 959a are preferably included.

A first quartz tube (951a) is a platinum ion is adsorbed carbon nanofibers (CNFs ⁺ Pt ² +) that is charged into the interior, thus the first quartz tube, the specimen mounting convenience when using the (951a), and facilitates the gas injection In addition, the specimen inside can be easily observed.

The first nitrogen gas introduction unit 953a is connected to the first quartz tube 951a to supply nitrogen gas into the first quartz tube 951 and includes a first flow regulator.

The first hydrogen gas inlet 955a is connected to the first quartz tube 951a to supply hydrogen gas into the first quartz tube 951 and includes a second flow regulator.

Preferably, the first and second flow rate regulators are MFCs.

The first gas exhaust portion 957a is connected to the first quartz tube 951a to discharge the gas after the hydrogen reduction reaction.

The first heating coil 959a is installed outside the first quartz tube 951a to heat the temperature inside the first quartz tube 951a to 900 ° C to 1200 ° C.

Meanwhile, cobalt hydrate (Co (CH ₃ CO ₂ ) ₂ .4H ₂ O) is added to the second tank 70a ', and acetone containing cobalt ions (Co ²⁺ ) dispersed by ultrasonic waves. The solvent is accommodated, and carbon nanofibers (CNFs + Pt) carrying platinum are immersed in this acetone solvent.

Cobalt acetate hydrate (Co (CH ₃ CO ₂ ) ₂ · 4H ₂ O) is an embodiment of the cobalt hydrate, and of course may vary depending on the embodiment.

The second sealing member 75a 'allows the carbon nanofibers (CNFs + Pt) loaded with platinum to sufficiently adsorb cobalt ions and the carbon nanofibers (CNFs + Pt) loaded with platinum to prevent impurity incorporation. The second bath 70a 'soaked is sealed.

The second rotary evaporator (80a ') is a water bath treatment of the second water tank (70a') from 65 ℃ to 100 ℃ to evaporate the acetone solvent in the second water tank (70a ').

The third oven member (90a ') is a cobalt ion, and for the platinum to the dried to the carbon nanofibers (CNFs + Pt + Co ²⁺⁾ supported thereon, the cobalt ions and the platinum-supported carbon nanofibers (CNFs Co + Pt + ^{2 +} ) Is heated to about 100 to 120 ℃.

The second hydrogen-reduction device (95a ') is thereby reduced to the cobalt ion (Co ²⁺⁾ adsorbed by the carbon nanofibers (CNFs + Pt + ^2, Co ⁺⁾ as cobalt (Co).

The second hydrogen reduction device 95a 'is preferably configured to include a second quartz tube, a second nitrogen gas introduction portion, a second hydrogen gas introduction portion, a second gas exhaust portion, and a second heating coil.

Since the second hydrogen reduction device 95a 'is substantially the same as the configuration of the first hydrogen reduction device 95a described above, only the characteristic effects of the second hydrogen reduction device 95a' will be described below. do.

The second heating coil is installed outside the second quartz tube to heat the temperature inside the second quartz tube to 500 ° C to 650 ° C.

Hereinafter, the operation of the second embodiment of the present invention having the above-described configuration will be described.

Referring to FIGS. 1 and 2, first, carbon nanofibers (CNFs) are prepared to remove impurities in the carbon nanofibers (CNFs) in order to remove a plurality of carbon nanofibers (CNFs) at 30% concentration of nitric acid. The solution is placed in a pickling treatment tank 10a containing the solution and dispersed for about 40 minutes to prevent entanglement between a plurality of carbon nanofibers (CNFs) using the ultrasonic generator 20a.

Carbon nanofibers (CNFs) in the dispersed nitric acid solution are boiled in a thermostat 30a at 60 ° C. to 80 ° C. for about 2 days to be pickled.

The pickled carbon nanofibers (CNFs) are immersed in a water treatment tank (50a) to remove the nitric acid solution remaining in the carbon nanofibers (CNFs) through a filter (40a) and to be almost neutral as distilled water. Is processed.

After washing with water, carbon nanofibers (CNFs) are heated to 100 ° C to 150 ° C in the first oven member 60a to remove residual moisture.

An acetone solvent is accommodated in the first bath 70a, platinum hydrate is added to the acetone solvent, the acetone solvent is dispersed by an ultrasonic cleaner for about 5 minutes, and dried carbon nanofibers (CNFs) are added to the acetone solvent.

The carbon nanofibers (CNFs) seal the first water tank (70a) with the first sealing member (75a) so as to sufficiently adsorb the platinum ions contained in the acetone solvent. While on the air.

Sufficiently platinum ion by carbon nanofibers adsorb (CNFs ⁺ Pt ² +) is in the first rotary Yves When Po radar processing water bath at 65 ℃ until 100 ℃ through (80a), the first tank (70a) Acetone solvent is evaporated.

The carbon nanofibers (CNFs + Pt ²⁺ ) on which the platinum ion remains after the acetone solvent is evaporated are heated to about 100 ° C. to 120 ° C. using the second oven member 90a. Keep this state for two days.

Alumina boat charged with (952a) after a piece of platinum ions are uniformly adsorbed carbon nanofibers (CNFs ⁺ Pt ² +) alumina boat (952a) to into the first quartz tube (951a) of the first hydrogen-reduction device (95a) After purging at a temperature increase rate of 5 ° C./min to 900 ° C. to 1200 ° C. under a nitrogen gas atmosphere. At this time, the nitrogen gas is supplied into the first quartz tube 951a through the first nitrogen gas introduction unit 953a.

When the temperature inside the first quartz tube 951a reaches 900 ° C to 1200 ° C, hydrogen gas is supplied through the first hydrogen gas introduction unit 955a for 1 hour to perform hydrogen reduction.

After purging again with a nitrogen gas atmosphere until the temperature drops below 200 ° C, the alumina boat 952a is taken out of the first quartz tube 951a, and platinum adsorbed onto carbon nanofibers (CNFs + Pt ²⁺ ). Ions (Pt ²⁺ ) are reduced to platinum (Pt) to produce carbon nanofibers (CNFs + Pt) on which platinum is adsorbed.

On the other hand, acetone solvent is accommodated in the second water tank 70a ', cobalt hydrate is added to the acetone solvent, and carbon nanofibers (CNFs + Pt) loaded with platinum after dispersing the acetone solvent for about 5 minutes by an ultrasonic cleaner. Is added to acetone solvent.

Platinum-adsorbed carbon nanofibers (CNFs + Pt) seal the second water tank (70a ') with the second sealing member (75a') to sufficiently adsorb cobalt ions. Hold on standby for two days.

When carbon nanofibers (CNFs + Pt) sufficiently adsorbed cobalt ions are subjected to water bath treatment from 65 ° C to 100 ° C through the second rotary evaporator 80a ', the second water tank 70a' Acetone solvent is evaporated.

The carbon nanofibers (CNFs + Pt + Co ²⁺ ) carrying the cobalt ions and platinum remaining after the acetone solvent is evaporated are heated to about 100 ° C. to 120 ° C. using the third oven member 90a '. Keep this state for two days.

Evenly spread the carbon nanofibers (CNFs + Pt + Co ²⁺ ) loaded with cobalt ions and platinum on the alumina boat, and load the alumina boat into the second quartz tube of the second hydrogen reduction device (95a ') Purging is carried out under nitrogen gas atmosphere up to 650 ℃. At this time, the nitrogen gas is supplied into the second quartz tube through the second nitrogen gas introduction portion.

When the temperature inside the second quartz tube reaches 500 ° C to 650 ° C, hydrogen gas is supplied through the second hydrogen gas introduction portion for one hour to perform hydrogen reduction.

After purging again with a nitrogen gas atmosphere until the temperature drops below 200 ° C, the alumina boat is taken out of the second quartz tube and cobalt ions (Co ²⁺ ) adsorbed on carbon nanofibers (CNFs + Pt + Co ²⁺ ) ) Is reduced to cobalt (Co) to complete a cobalt-platinum supported catalyst for fuel cells using carbon nanofibers (CNFs) of the present invention.

As described above, the cobalt-platinum supported catalyst for fuel cell manufactured by the cobalt-platinum supported catalyst manufacturing apparatus for fuel cell using the carbon nanofiber of the present invention is illustrated in FIGS.

Meanwhile, FIG. 4 illustrates a method for preparing a cobalt-platinum supported catalyst for a fuel cell using carbon nanofibers according to a preferred embodiment of the present invention.

5 is a flowchart sequentially illustrating a method for preparing a cobalt-platinum supported catalyst for a fuel cell using carbon nanofibers according to a preferred embodiment of the present invention.

As shown in FIG. 5, the method for preparing a cobalt-platinum supported catalyst for a fuel cell using the carbon nanofiber of the present embodiment includes a pickling treatment step, an ultrasonic dispersion step, a boiling step in a thermostat, a filtration step, and a water washing treatment. A step, a heat drying step, a step of putting in an acetone solvent, a sealing step, a water bath treatment step, a heat drying step, a hydrogen reduction step, a step of putting in an acetone solvent, a sealing step, a water bath A treatment step, a heat drying step, and a hydrogen reduction step.

In step (a), the carbon nanofibers are immersed in a pickling tank containing nitric acid solution to remove impurities from the carbon nanofibers.

In step (b), ultrasonic waves are dispersed in the pickling bath of step (a) to prevent entanglement between the plurality of carbon nanofibers.

In step (c), the pickling bath of step (b) is boiled in a constant temperature bath containing water of 60 ℃ to 80 ℃.

In step (d), the carbon nanofibers are filtered to remove the nitric acid solution remaining in the carbon nanofibers.

In step (e), the carbon nanofibers are washed with water.

In step (f), the carbon nanofibers are heated to about 100 ° C to 150 ° C and dried to remove moisture remaining in the carbon nanofibers.

In the step (g), the carbon nanofibers are introduced into a tank containing acetone solvent containing platinum ions dispersed by platinum hydrate.

In step (h), the tank of step (g) is sealed to allow carbon nanofibers to sufficiently adsorb platinum ions.

In step (i), the water bath is subjected to a water bath at 65 ° C to 100 ° C in order to evaporate the acetone solvent in the water tank of step (h).

In the step (j), in order to dry the carbon nanofibers onto which platinum ions are adsorbed, the carbon nanofibers are heated to about 100 ° C to 120 ° C and dried.

In step (k), platinum ions adsorbed on the carbon nanofibers are reduced to platinum using a hydrogen reduction apparatus.

In step (l), the carbon nanofibers carrying the platinum obtained in step (k) are added to a bath containing acetone solvent containing cobalt ions dispersed by cobalt hydrate.

In step (m), the tank of step (l) is sealed to allow carbon nanofibers loaded with platinum to sufficiently adsorb cobalt ions.

In step (n), the water bath is subjected to a water bath at 65 ° C to 100 ° C to evaporate the acetone solvent in the water tank of step (m).

In step (o), in order to dry the carbon nanofibers carrying cobalt ions and platinum, the carbon nanofibers carrying cobalt ions and platinum are heated and dried to about 100 ° C to 120 ° C.

In step (p), cobalt ions adsorbed to the carbon nanofibers carrying cobalt ions and platinum are reduced to cobalt using a second hydrogen reduction device.

The cobalt-platinum supported catalyst for a fuel cell using carbon nanofibers is completed by the above steps.

As described above, although preferred embodiments of the present invention have been described, those skilled in the art will be able to variously modify or modify the present invention without departing from the spirit and scope of the invention as set forth in the claims below. It can be modified.

According to the apparatus for preparing a cobalt-platinum catalyst for a fuel cell using the carbon nanofiber of the present invention as described above, the following effects are obtained.

Pickling of the nitric acid solution allows more cobalt ions and platinum ions to be supported on the surface of the carbon nanofiber carrier, and can produce high performance, high efficiency, high stability cobalt-platinum supported catalysts and reduce manufacturing costs. have.

Claims (3)

In order to remove impurities of the carbon nanofibers, a pickling treatment tank in which a plurality of carbon nanofibers are immersed and housed in a nitric acid solution to be pickled; An ultrasonic generator for dispersing ultrasonic waves in the carbon nanofibers soaked in the nitric acid solution to prevent entanglement between the plurality of carbon nanofibers; A thermostat containing 60 ° C. to 80 ° C. water in which the pickling treatment tank is immersed; A filter for removing nitric acid solution remaining in the carbon nanofibers soaked in the pickling treatment tank; A water washing tank containing distilled water in which the carbon nanofibers from which nitric acid solution has been removed are soaked and washed with water; A first oven member for drying the carbon nanofibers by heating the carbon nanofibers in an amount of about 100 ° C. to 150 ° C. in order to remove residual moisture of the water washed carbon nanofibers; A first bath in which the dried carbon nanofibers are immersed and acetone solvent containing platinum ions dispersed by platinum hydrate and dispersed by an ultrasonic cleaner is accommodated; A first sealing member for sealing the first bath in which the carbon nanofibers are soaked to allow the carbon nanofibers to sufficiently adsorb the platinum ions and to prevent impurities from entering; A first rotary evaporator for treating the first bath in a water bath at 65 ° C. to 100 ° C. to evaporate the acetone solvent in the first bath; A second oven member for drying the carbon nanofibers on which the platinum ions are adsorbed and heated by drying the carbon nanofibers on which the platinum ions are adsorbed at about 100 ° C. to 120 ° C .; A first hydrogen reduction device for reducing the platinum ions supported on the carbon nanofibers to platinum; A second bath in which the carbon nanofibers carrying the platinum are immersed and in which acetone solvent containing cobalt ions dispersed by ultrasonic cleaning is accommodated by cobalt hydrate; A second sealing member for sealing the second tank in which the carbon nanofibers carrying the platinum are loaded so that the carbon nanofibers adsorbing the platinum sufficiently adsorb the cobalt ions and prevent impurity incorporation; A second rotary evaporator for treating the second bath in a water bath at 65 ° C. to 100 ° C. to evaporate the acetone solvent in the second bath; A third oven member for drying the cobalt ions and the platinum-carrying carbon nanofibers by heating the cobalt ions and the platinum-carrying carbon nanofibers at about 100 ° C. to about 120 ° C .; And Manufacture of a cobalt-platinum supported catalyst for a fuel cell using a carbon nanofiber comprising a; a second hydrogen reduction device for reducing the cobalt ion adsorbed on the cobalt ion and the carbon nanofiber carrying the platinum to cobalt; Device. The method of claim 1, The first hydrogen reduction device, A first quartz tube into which the carbon nanofibers on which the platinum ions are adsorbed are charged; A first nitrogen gas introduction part connected to the first quartz tube to supply nitrogen gas into the first quartz tube and having a first flow regulator; A first hydrogen gas introduction part connected to the first quartz tube to supply hydrogen gas into the first quartz tube and having a second flow regulator; A first gas exhaust part connected to the first quartz tube to discharge gas after a hydrogen reduction reaction; And And a first heating coil installed outside the first quartz tube to heat the inside of the first quartz tube to 900 ° C to 1200 ° C. The second hydrogen reduction device, A second quartz tube into which carbon nanofibers adsorbed the cobalt ions and platinum are charged; A second nitrogen gas introduction part connected to the second quartz tube to supply nitrogen gas into the second quartz tube and having a third flow controller; A second hydrogen gas introduction part connected to the second quartz tube to supply hydrogen gas into the second quartz tube and having a fourth flow regulator; A second gas exhaust base connected to the second quartz tube to discharge gas after a hydrogen reduction reaction; And Cobalt-platinum supported for fuel cells using carbon nanofibers, comprising: a second heating coil installed outside the second quartz tube to heat the inside of the second quartz tube to 500 ℃ to 650 ℃; Catalyst production apparatus. (a) immersing the carbon nanofibers in a pickling bath containing nitric acid solution to remove impurities of the carbon nanofibers; (b) dispersing ultrasonic waves in the pickling bath of step (a) to prevent entanglement between the plurality of carbon nanofibers; (c) putting the pickling treatment tank of step (b) into a thermostatic bath containing water of 60 ° C. to 80 ° C. to boil; (d) filtering the carbon nanofibers to remove nitric acid solution remaining in the carbon nanofibers; (e) washing the carbon nanofibers with water; (f) drying the carbon nanofibers by heating the carbon nanofibers in an amount of about 100 ° C. to 150 ° C. to remove moisture remaining in the carbon nanofibers; (g) injecting the carbon nanofibers into a tank containing acetone solvent containing platinum ions dispersed by platinum hydrate; (h) sealing the water tank of step (g) to allow the carbon nanofibers to sufficiently adsorb the platinum ions; (i) treating the bath with a water bath at 65 ° C. to 100 ° C. to evaporate the acetone solvent in the bath of step (h); (j) drying the carbon nanofibers by heating the carbon nanofibers at about 100 ° C. to about 120 ° C. to dry the carbon nanofibers onto which the platinum ions are adsorbed; (k) reducing the platinum ions adsorbed on the carbon nanofibers to platinum using a first hydrogen reduction device; (l) injecting the carbon nanofibers carrying the platinum obtained in step (k) into a water bath containing acetone solvent containing cobalt ions dispersed by cobalt hydrate; (m) sealing the water tank of step (l) so that the platinum-supported carbon nanofibers can sufficiently adsorb the cobalt ions; (n) treating the water bath with a water bath at 65 ° C. to 100 ° C. to evaporate the acetone solvent in the water tank of step (m); (o) heating the carbon nanofibers carrying the cobalt ions and the platinum to a temperature of about 100 ° C. to 120 ° C. to dry the carbon nanofibers carrying the cobalt ions and the platinum; And (p) reducing the cobalt ions adsorbed to the cobalt ions and the platinum-carrying carbon nanofibers using a second hydrogen reduction device to cobalt; fuel using carbon nanofibers, comprising: Method for preparing a cobalt-platinum supported catalyst for batteries.

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