KR20070092014A - Apparatus for manufacturing catalyst powder - Google Patents

Apparatus for manufacturing catalyst powder Download PDF

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Publication number
KR20070092014A
KR20070092014A KR1020060021892A KR20060021892A KR20070092014A KR 20070092014 A KR20070092014 A KR 20070092014A KR 1020060021892 A KR1020060021892 A KR 1020060021892A KR 20060021892 A KR20060021892 A KR 20060021892A KR 20070092014 A KR20070092014 A KR 20070092014A
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South Korea
Prior art keywords
tube
catalyst
solution
powder
catalyst powder
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KR1020060021892A
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Korean (ko)
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민명기
박찬희
권호진
채근석
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삼성에스디아이 주식회사
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Priority to KR1020060021892A priority Critical patent/KR20070092014A/en
Publication of KR20070092014A publication Critical patent/KR20070092014A/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/04Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18Carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/16Reducing

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Catalysts (AREA)

Abstract

A system for preparing catalyst powder that can obtain catalyst powder with a uniform particle size by spraying a catalytic solution into a tube is provided. In a system for preparing catalyst powder from a solution container(30) in which a catalytic solution is stored, the system for preparing catalyst powder comprises: a tube(10); a first tube holder(12) holding one end portion of the tube; a second tube holder(14) holding the other end portion of the tube; a spray nozzle(32) embedded in the first tube holder to spray a catalytic solution from the solution container into the tube; a reciprocating means(40) having a powder collector(42) attached to an end portion thereof such that the powder collector is movable through the second tube holder; and a heating means(20) heating the tube. The system further comprises an opening-and-closing valve(34) interposed between the spray nozzle and the solution container.

Description

촉매분말 제조장치{APPARATUS FOR MANUFACTURING CATALYST POWDER}Catalytic powder manufacturing apparatus {APPARATUS FOR MANUFACTURING CATALYST POWDER}

도 1은 본 발명에 따른 촉매합성장치의 도면;1 is a view of a catalyst synthesis apparatus according to the present invention;

도 2는 도 1의 선 II-II를 취한 단면도;2 is a cross-sectional view taken along the line II-II of FIG. 1;

도 3은 튜브로부터 건조된 촉매를 인출하는 상태를 나타낸 도면.3 is a view showing a state in which the dried catalyst is withdrawn from the tube.

< 도면의 주요부분에 대한 부호의 설명 ><Description of Symbols for Major Parts of Drawings>

10 : 튜브10: tube

12, 14 : 튜브홀더12, 14: tube holder

20 : 가열수단20: heating means

30 : 용액용기30: solution container

32 : 분사노즐32: injection nozzle

34 : 개폐밸브34: on-off valve

40 : 왕복이동수단40: reciprocating means

42 : 분말 수집기42: powder collector

본 발명은 촉매원료를 환원시켜 촉매를 제조하는 장치에 관한 것이고, 더 상세하게 일정한 촉매특성과 균일한 입도크기를 갖는 분말을 얻을 수 있는 촉매분말 제조장치에 관한 것이다. The present invention relates to an apparatus for producing a catalyst by reducing the catalyst raw material, and more particularly to a catalyst powder production apparatus that can obtain a powder having a constant catalyst characteristics and uniform particle size.

일반적으로, 연료전지 시스템은 메탄올이나 천연가스 등의 탄화수소계열의 연료 중에 포함되어 있는 수소와 공기중의 산소를 전기화학 반응에 의해서 직접 전기에너지를 얻는 발전 시스템이다. 이러한 연료전지 시스템은 전해질의 종류에 따라 크게 알칼리형, 인산형, 용융탄산염, 고체산화물형 및 고체고분자 전해질형으로 분류될 수 있다.In general, a fuel cell system is a power generation system that directly obtains electrical energy by an electrochemical reaction between hydrogen contained in a hydrocarbon-based fuel such as methanol or natural gas and oxygen in the air. Such fuel cell systems can be broadly classified into alkali type, phosphoric acid type, molten carbonate, solid oxide type and solid polymer electrolyte type according to the type of electrolyte.

이러한 연료전지 시스템은 기본적으로 전기를 생성하기 위한 단위전지가 복수개 적층되어 있는 스택을 갖고 있다. 스택은 엔드 플레이트 사이에 적층되어 있는 복수개의 단위전지가 볼트와 너트에 의해서 체결된 구조로 이루어진다. 상기 단위전지는 고분자 전해질막의 양측면에 전극이 각각 제공되어 있는 전극막 조립체(MEA)와, 상기 MEA의 양측에 각각 위치하고 유체유동용 채널이 표면에 가공되어 있는 세퍼레이터, 즉 바이폴라 플레이트로 이루어진다.Such a fuel cell system basically has a stack in which a plurality of unit cells for generating electricity are stacked. The stack has a structure in which a plurality of unit cells stacked between end plates are fastened by bolts and nuts. The unit cell includes an electrode membrane assembly (MEA) provided with electrodes on both sides of the polymer electrolyte membrane, and a separator, that is, a bipolar plate, respectively disposed on both sides of the MEA and having a fluid flow channel processed on the surface thereof.

연료전지 시스템의 발전효율은 전극에 의해서 크게 좌우된다. 이러한 전극은 일반적으로 미세한 촉매분말, 예를 들어 백금분말이 담지된 탄소분말을 결합제로 결합시킨 전극 촉매층을 포함하고 있으므로, 연료전지 시스템의 발전효율을 향상시키기 위해서는 촉매특성이 우수하고 분말 상태가 양호한 양질의 촉매분말이 요구된다. The power generation efficiency of a fuel cell system depends largely on the electrode. Such an electrode generally includes an electrode catalyst layer in which a fine catalyst powder, for example, a carbon powder on which platinum powder is supported, is bonded with a binder. Thus, in order to improve power generation efficiency of a fuel cell system, the catalyst has excellent catalyst properties and a good powder state. Good catalyst powder is required.

종래 실시예에 따르면, 촉매원료를 함유한 용액에 환원제나 계면활성제(surfactant)를 첨가한 후에 환원성 분위기 하에서 열처리함으로써 촉매분말을 얻었다. 그러나, 상술된 바와 같은 촉매분말 제조방식은 회분방식(batch manner)으로 이루어지므로, 균질의 분말을 얻는 것이 어려웠다. 즉, 분말의 입도상태를 균일하게 유지하는 것이 어려웠다.According to the conventional example, a catalyst powder was obtained by adding a reducing agent or a surfactant to a solution containing a catalyst raw material and then performing heat treatment in a reducing atmosphere. However, since the catalyst powder production method as described above is made in a batch manner, it is difficult to obtain a homogeneous powder. That is, it was difficult to keep the particle size state of powder uniform.

본 발명은 상술된 바와 같은 종래의 문제점을 해결하기 위하여 제안된 것으로, 분말의 입도상태를 양호하게 얻을 수 있는 촉매분말 제조장치를 제공하는 데 그 목적이 있다. The present invention has been proposed in order to solve the conventional problems as described above, and an object thereof is to provide a catalyst powder production apparatus that can obtain a good particle size state of the powder.

상기 목적을 달성하기 위하여 본 발명에 따르면, 촉매분말 제조장치는 관통형상의 튜브와, 상기 튜브의 일단부를 지지하는 제1튜브홀더와, 상기 튜브의 타단부를 지지하는 제2튜브홀더와, 상기 제1튜브홀더에 내장되어 촉매용액을 상기 튜브의 내부에 분사하는 분사노즐과, 상기 제2튜브홀더를 통해 이동가능한 분말 수집기가 단부에 부착되어 있는 왕복이동수단과, 상기 튜브를 가열하기 위한 가열수단으로 이루어진 것을 특징으로 한다.In order to achieve the above object, according to the present invention, a catalyst powder manufacturing apparatus includes a through-shaped tube, a first tube holder for supporting one end of the tube, a second tube holder for supporting the other end of the tube, and A injection nozzle embedded in the first tube holder for injecting a catalyst solution into the tube, a reciprocating means having a powder collector movable at the end of the tube and attached to an end thereof, and heating for heating the tube. It is characterized by consisting of means.

상기 분사노즐은 개폐밸브를 개재시킨 상태로 촉매용액이 저장되어 있는 용액 용기에 유체소통이 가능하게 연결된다. The injection nozzle is fluidly connected to the solution container in which the catalyst solution is stored with the on / off valve interposed therebetween.

상기 왕복이동수단은 실린더이고, 상기 가열수단은 열선 또는 할로겐 램프이다. 상기 가열수단에는 반사경이 제공된다.The reciprocating means is a cylinder, and the heating means is a hot wire or a halogen lamp. The heating means is provided with a reflector.

상기 촉매용액은 백금산용액이고, 필요에 따라서 나피온과 같은 이오노머 또는 카본이 함유된다.The catalyst solution is a platinum acid solution and, if necessary, contains an ionomer or carbon such as Nafion.

이하, 첨부도면을 참조하여 본 발명에 대해 설명한다.Hereinafter, the present invention will be described with reference to the accompanying drawings.

도 1은 본 발명에 따른 촉매분말 제조장치를 도시한 도면이고, 도 2는 도 1의 선 II-II를 취한 단면도이고, 도 3은 본 발명에 따라서 제조된 촉매분말의 인출상태를 나타낸 도면이다.1 is a view showing a catalyst powder production apparatus according to the present invention, Figure 2 is a cross-sectional view taken line II-II of Figure 1, Figure 3 is a view showing the withdrawal state of the catalyst powder prepared according to the present invention. .

먼저, 촉매분말을 제조하기 위하여 촉매용액을 준비한다. 상기 촉매용액은 촉매원료를 산성용액에 용해시킨 용액이다. 상기 촉매용액에는 필요에 따라서 증류수, 에탄올, 알콜 및 아세톤으로 이루어진 그룹으로부터 선택되는 적어도 하나의 용매가 첨가될 수 있다. 이러한 촉매용액은 용액 용기(30; 도 1 참조)에 저장될 수 있다. 상기 촉매용액은 예를 들어 백금산용액으로 구성될 수 있다.First, a catalyst solution is prepared to prepare a catalyst powder. The catalyst solution is a solution in which the catalyst raw material is dissolved in an acid solution. At least one solvent selected from the group consisting of distilled water, ethanol, alcohol and acetone may be added to the catalyst solution as necessary. This catalyst solution may be stored in the solution vessel 30 (see FIG. 1). The catalyst solution may be composed of, for example, a platinum acid solution.

본 발명에 따르면, 상술된 촉매용액으로부터 촉매분말을 제조하기 위한 장치(100)는 도 1에 도시된 바와 같이, 관통구조를 갖는 튜브(10)와, 튜브(10)의 일단부를 지지하는 제1튜브홀더(12)와, 튜브(10)의 타단부를 지지하는 제2튜브홀더(14)를 갖는다. According to the present invention, the apparatus 100 for producing the catalyst powder from the catalyst solution described above, as shown in Figure 1, the tube 10 having a through structure and the first end of the one end of the tube 10, The tube holder 12 and the second tube holder 14 supporting the other end of the tube 10 are provided.

튜브(10)의 주변에는 이를 가열하기 위한 가열수단(20)이 제공된다. 가열수단(20)은 튜브(10)의 주변을 감고 있는 열선 또는 튜브(20)의 주변을 둘러싸고 있 는 복수개의 할로겐 램프와 같은 발열체로 이루어질 수 있다. 이때, 가열수단(20)에 의한 가열효과를 향상시키기 위하여, 가열수단(20)으로부터 발산되는 열이 튜브(10)를 향해서 반사될 수 있도록 작용하는 반사경이 튜브(20)의 주변에 제공될 수도 있다. At the periphery of the tube 10 is provided heating means 20 for heating it. The heating means 20 may be made of a heating element, such as a heating wire wound around the periphery of the tube 10 or a plurality of halogen lamps surrounding the periphery of the tube 20. At this time, in order to improve the heating effect by the heating means 20, a reflecting mirror may be provided around the tube 20 so that the heat emitted from the heating means 20 can be reflected toward the tube 10. have.

제2튜브홀더(14)의 하부에는 길이가변동작이 가능한 왕복이동수단(40)이 제공되고, 왕복이동수단(40)의 단부에는 분말 수집기(42)가 제공된다. 왕복이동수단(40)은 실린더로 구성될 수 있다. 분말 수집기(42)는 판상의 구조를 갖는다. 예를 들어, 분말 수집기(42)는 튜브(10)의 내부면 구조에 따라서 원판 또는 사각판 구조로 이루어질 수 있다. 분말 수집기(42)는 왕복이동수단(40)의 길이가변동작에 의해서 제2튜브홀더(14)를 통해서 튜브(10)의 내부로 진입하거나 또는 이로부터 외부로 배출될 수 있다.The lower portion of the second tube holder 14 is provided with a reciprocating means 40 capable of variable length operation, the powder collector 42 is provided at the end of the reciprocating means 40. The reciprocating means 40 may be configured as a cylinder. The powder collector 42 has a plate-like structure. For example, the powder collector 42 may have a disc or square plate structure according to the inner surface structure of the tube 10. The powder collector 42 may enter or exit the inside of the tube 10 through the second tube holder 14 by the variable length operation of the reciprocating means 40.

제1튜브홀더(12)에는 튜브(10)의 내부를 향해서 촉매용액을 분사하기 위한 분사노즐(32)이 내장된다. 분사노즐(32)은 튜브(10)의 외부에 위치하는 용액 용기(30)에 유체소통이 가능하게 연결된다. 바람직하게, 분사노즐(32)과 용액 용기(30) 사이에는 개폐밸브(34)가 제공될 수 있다.The first tube holder 12 includes a spray nozzle 32 for injecting a catalyst solution toward the inside of the tube 10. The injection nozzle 32 is fluidly connected to the solution container 30 located outside the tube 10. Preferably, an on-off valve 34 may be provided between the injection nozzle 32 and the solution container 30.

이하, 본 발명에 따른 촉매분말 제조장치의 작동에 대하여 설명한다.Hereinafter, the operation of the catalyst powder production apparatus according to the present invention will be described.

먼저, 용액 용기(30)는 분사노즐(32)에 유체소통이 가능하게 연결되고, 분말 수집기(420는 튜브(10)의 내부, 바람직하게 제2튜브홀더(14)에 인접하는 튜브(10)의 내측 하부에 위치한다. 그리고, 가열수단(20)이 동작하여 튜브(10) 내부를 소 정 온도, 예를 들어 약 150~500℃ 정도의 온도로 가열한다.First, the solution container 30 is fluidly connected to the injection nozzle 32, and the powder collector 420 is inside the tube 10, preferably the tube 10 adjacent to the second tube holder 14. The heating means 20 is operated to heat the inside of the tube 10 to a predetermined temperature, for example, about 150 to 500 ° C.

이 후에, 개폐밸브(34)의 개방동작에 의해서 용액 용기(30)로부터 배출되는 촉매용액은 분사노즐(32)의 분사동작에 의해서 튜브(10)의 내부에 분무형태로 분사된다. 이때, 분무형태의 촉매용액은 튜브(10) 내부에 균일하게 분포되어 있으므로 촉매용액들 사이의 엉킴현상은 발생하지 않는다.Thereafter, the catalyst solution discharged from the solution container 30 by the opening operation of the opening / closing valve 34 is sprayed into the tube 10 in the form of a spray by the injection operation of the injection nozzle 32. At this time, the catalyst solution in the spray form is uniformly distributed in the tube 10, so that no entanglement between the catalyst solutions occurs.

분사노즐(32)에서 분사되는 촉매용액이 제2튜브홀더(14)를 향해서 진행하는 동안 튜브(10) 내부의 온도에 의해서 촉매용액에 함유되어 있는 휘발성이 높은 용액은 증발하게 되며, 결과적으로 균일한 입도의 촉매분말이 얻어진다.While the catalyst solution injected from the injection nozzle 32 is directed toward the second tube holder 14, the highly volatile solution contained in the catalyst solution is evaporated by the temperature inside the tube 10, and as a result, it is uniform. One particle catalyst powder is obtained.

이러한 촉매분말은 분말 수집기(42) 상에 축적된다.This catalyst powder accumulates on the powder collector 42.

상술된 과정을 통해서 분말 수집기(42) 상에 소정량의 촉매분말이 축적되면 왕복이동수단(40)의 하강동작에 의해서 분말 수집기(42)가 튜브(10)의 내부로부터 외부로 인출됨으로써, 균일한 입도를 갖는 촉매분말(A)을 얻을 수 있다.When a predetermined amount of catalyst powder is accumulated on the powder collector 42 through the above-described process, the powder collector 42 is drawn out from the inside of the tube 10 to the outside by the lowering operation of the reciprocating means 40. A catalyst powder (A) having a particle size can be obtained.

상기 촉매용액이 백금산용액인 경우에는 튜브(10) 내부는 약 200℃ 정도의 온도로 유지된다. 이때, 분사노즐(32)을 통해서 튜브(10) 내부에 분사되는 분무형태의 백금산용액에 함유되어 있는 백금 촉매는 휘발성이 높은 용액이 증발하면서 환원되어 백금분말로 변환된다. 이러한 백금분말의 입도는 균일하게 유지될 수 있다.When the catalyst solution is a platinum acid solution, the inside of the tube 10 is maintained at a temperature of about 200 ℃. At this time, the platinum catalyst contained in the spray-type platinum acid solution sprayed into the tube 10 through the injection nozzle 32 is reduced while the highly volatile solution is evaporated and converted into platinum powder. The particle size of such platinum powder can be kept uniform.

한편, 백금산용액에 나피온과 같은 이오노머를 혼합시킨 후 분사노즐(32)을 통해서 튜브(10) 내부에 분사시키면, 백금촉매가 코팅된 나피온을 얻을 수 있다. 이러한 나피온에서 백금촉매는 균일한 입도를 갖고 또한 균일하게 분포하게 되므로 양질의 나피온을 얻게 된다.On the other hand, after mixing the ionizer, such as Nafion in the platinum acid solution and sprayed into the tube 10 through the injection nozzle 32, it is possible to obtain a platinum catalyst coated Nafion. In this Nafion, the platinum catalyst has a uniform particle size and is uniformly distributed, thereby obtaining a good Nafion.

또한, 상기 백금산용액에 카본을 혼합시키면 마찬가지의 효과로서 담지촉매를 얻을 수 있다.In addition, when carbon is mixed with the platinum acid solution, a supported catalyst can be obtained with the same effect.

본 발명에 따르면, 촉매용액을 튜브 내부에 분무형태로 분사시킴으로써 균일한 입도를 갖는 촉매분말을 얻을 수 있다.According to the present invention, a catalyst powder having a uniform particle size can be obtained by spraying the catalyst solution in the form of a spray inside the tube.

Claims (8)

촉매용액이 저장되어 있는 용액 용기로부터 촉매분말을 제조하기 위한 장치에 있어서,An apparatus for producing a catalyst powder from a solution vessel in which a catalyst solution is stored, 튜브와;A tube; 상기 튜브의 일단부를 지지하는 제1튜브홀더와;A first tube holder supporting one end of the tube; 상기 튜브의 타단부를 지지하는 제2튜브홀더와;A second tube holder supporting the other end of the tube; 상기 제1튜브홀더에 내장되어 상기 용액 용기로부터 촉매용액을 상기 튜브의 내부에 분사하는 분사노즐과;An injection nozzle embedded in the first tube holder for injecting a catalyst solution from the solution container into the tube; 상기 제2튜브홀더를 통해 이동가능한 분말 수집기가 단부에 부착되어 있는 왕복이동수단과;Reciprocating means having a powder collector moveable through the second tube holder attached to an end thereof; 상기 튜브를 가열하기 위한 가열수단으로 이루어진 것을 특징으로 하는 촉매분말 제조장치.Catalyst powder manufacturing apparatus, characterized in that consisting of a heating means for heating the tube. 제1항에 있어서,The method of claim 1, 상기 분사노즐과 상기 용액 용기 사이에 개재되어 있는 개폐밸브를 더 포함하는 것을 특징으로 하는 촉매분말 제조장치.Catalyst powder manufacturing apparatus further comprises an on-off valve interposed between the injection nozzle and the solution container. 제1항에 있어서,The method of claim 1, 상기 왕복이동수단은 실린더인 것을 특징으로 하는 촉매분말 제조장치.The catalyst powder manufacturing apparatus, characterized in that the reciprocating means is a cylinder. 제1항에 있어서,The method of claim 1, 상기 가열수단은 열선 또는 할로겐 램프인 것을 특징으로 하는 촉매분말 제조장치.The heating means is a catalyst powder production apparatus, characterized in that the hot wire or halogen lamp. 제4항에 있어서,The method of claim 4, wherein 상기 가열수단에는 반사경이 제공되어 있는 것을 특징으로 하는 촉매분말 제조장치.Catalytic powder production apparatus, characterized in that the heating means is provided with a reflector. 제1항에 있어서,The method of claim 1, 상기 촉매용액은 백금산용액인 것을 특징으로 하는 촉매분말 제조장치.Catalyst catalyst production apparatus, characterized in that the catalyst solution is a platinum acid solution. 제6항에 있어서,The method of claim 6, 상기 촉매용액에는 나피온이 함유되어 있는 것을 특징으로 하는 촉매분말 제조장치.The catalyst powder production apparatus characterized in that the catalyst solution contains Nafion. 제6항 또는 제7항에 있어서,The method according to claim 6 or 7, 상기 촉매용액에는 카본이 함유되어 있는 것을 특징으로 하는 촉매분말 제조장치.The catalyst powder production apparatus, characterized in that the catalyst solution contains carbon.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101025219B1 (en) * 2007-10-25 2011-03-31 주식회사 효성 Process for preparing phosphotungstic acid powder with an atomizer

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101025219B1 (en) * 2007-10-25 2011-03-31 주식회사 효성 Process for preparing phosphotungstic acid powder with an atomizer

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