KR20120079850A - Platinium-palladium composite catalyst having a new structure and method for manufacturing the same - Google Patents
Platinium-palladium composite catalyst having a new structure and method for manufacturing the same Download PDFInfo
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- KR20120079850A KR20120079850A KR1020100138938A KR20100138938A KR20120079850A KR 20120079850 A KR20120079850 A KR 20120079850A KR 1020100138938 A KR1020100138938 A KR 1020100138938A KR 20100138938 A KR20100138938 A KR 20100138938A KR 20120079850 A KR20120079850 A KR 20120079850A
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000003054 catalyst Substances 0.000 title claims abstract description 43
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000011734 sodium Substances 0.000 claims abstract description 7
- 239000002608 ionic liquid Substances 0.000 claims abstract description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 3
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 3
- 241000257465 Echinoidea Species 0.000 claims abstract 2
- 101150003085 Pdcl gene Proteins 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 238000005054 agglomeration Methods 0.000 claims 1
- 230000002776 aggregation Effects 0.000 claims 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract 1
- 229910052700 potassium Inorganic materials 0.000 abstract 1
- 239000011591 potassium Substances 0.000 abstract 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- FRZPYEHDSAQGAS-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;trifluoromethanesulfonate Chemical compound [O-]S(=O)(=O)C(F)(F)F.CCCC[N+]=1C=CN(C)C=1 FRZPYEHDSAQGAS-UHFFFAOYSA-M 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 3
- 229960005070 ascorbic acid Drugs 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 235000019253 formic acid Nutrition 0.000 description 3
- 235000000069 L-ascorbic acid Nutrition 0.000 description 2
- 239000002211 L-ascorbic acid Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- -1 chloride Palladium compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000003058 platinum compounds Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
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- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
Description
본 발명은 Pt 및 Pd 성분을 포함하는 백금-팔라듐 복합체 촉매 및 그 제조 방법에 관한 것으로, 보다 상세하게는, Pt 성분과 Pd 성분이 입자 내부에 고르게 분산되며, 별 모양의 구조를 갖는 백금-팔라듐 복합체 촉매 및 그 제조 방법에 관한 것이다.The present invention relates to a platinum-palladium composite catalyst comprising a Pt and a Pd component and a method for preparing the same, and more particularly, to a platinum-palladium having a star-shaped structure in which the Pt component and the Pd component are evenly dispersed inside the particles. A composite catalyst and a method for producing the same.
종래에 연료 전지 및 자동차 배가스 처리 분야에서는, 일반적으로 전지 성능 또는 배가스 처리능을 향상시키기 위해 산화 환원 반응을 촉진하기 위한 촉매를 사용하여 왔다. 현재 이러한 촉매로는 주로 백금 성분을 포함하는 백금 촉매가 사용되고 있으나, 백금 촉매는 가격이 비싸기 때문에, 이를 사용할 경우 최종 제품의 생산 가격이 높아진다는 문제점이 있다. 따라서, 백금 촉매를 대체할 수 있는 대체 촉매 개발에 대한 연구가 지속되고 있다.Background Art Conventionally, in the fuel cell and automotive exhaust gas treatment field, catalysts for promoting redox reactions have generally been used to improve cell performance or flue gas treatment capacity. Currently, a platinum catalyst including a platinum component is mainly used as the catalyst, but since the platinum catalyst is expensive, there is a problem in that the production price of the final product is increased. Therefore, research on the development of an alternative catalyst that can replace the platinum catalyst is continuing.
본 발명은 상기와 같은 문제점을 해결하기 위한 것으로, 백금 촉매에 비해 제조 단가가 상대적으로 저렴하며, 우수한 촉매 성능을 갖는 신규한 구조의 백금-팔라듐 복합체 촉매 및 그 제조방법을 제공한다.The present invention is to solve the above problems, and provides a novel structure of the platinum-palladium composite catalyst and a method for producing the same, the production cost is relatively low compared to the platinum catalyst, and has excellent catalytic performance.
이를 위해, 본 발명은, 일 측면에서, 백금 성분과 팔라듐 성분이 입자 내부에 고르게 분산되며, 별 모양의 구조를 갖는 백금-팔라듐 복합체 촉매를 제공한다.
To this end, the present invention provides a platinum-palladium composite catalyst having, in one aspect, a platinum component and a palladium component evenly dispersed inside the particles and having a star shape.
본 발명의 백금-팔라듐 복합체 촉매는 입자 직경이 대략 5 내지 50nm 정도이며, 바람직하게는 5 내지 40nm, 더 바람직하게는 10 내지 30nm정도이다.
The platinum-palladium composite catalyst of the present invention has a particle diameter of about 5 to 50 nm, preferably 5 to 40 nm, more preferably about 10 to 30 nm.
또한, 본 발명의 백금-팔라듐 복합체 촉매는 이방성(anisotropic)을 가지는 다수의 침상 가지들이 입자의 중심으로부터 성장한 형상을 가진다.
In addition, the platinum-palladium composite catalyst of the present invention has a shape in which a plurality of needle-shaped branches having anisotropic growth from the center of the particles.
다른 측면에서, 본 발명은 백금 성분과 팔라듐 성분을 이온성 액체(ionic liquid) 내에서 공환원(coreduction)시키는 단계를 포함하는 백금-팔라듐 촉매 제조 방법을 제공한다.In another aspect, the present invention provides a method for preparing a platinum-palladium catalyst comprising the step of coreducing a platinum component and a palladium component in an ionic liquid.
본 발명의 백금-팔라듐 복합체 촉매는 백금 성분과 팔람듐 성분이 입자 내부에 고르게 분산되어 있어, 우수한 촉매 활성을 가지며, 침상 가지들이 포함된 별 모양의 구조로, 넓은 반응 표면적을 확보할 수 있다.In the platinum-palladium composite catalyst of the present invention, the platinum component and the palladium component are uniformly dispersed in the particles, thus having excellent catalytic activity, and having a star-shaped structure including needle branches, thereby ensuring a wide reaction surface area.
도 1은 본 발명의 제조 방법에 의해 제조된 백금-팔라듐 복합체 촉매를 촬영한 SEM 사진이며,
도 2는 본 발명의 백금-팔라듐 복합체 촉매 내의 성분 분포를 보여주는 STEM X-레이 맵 이미지이며,
도 3은 본 발명의 비교예에 의해 제조된 입자들을 촬영한 SEM 사진이다.1 is a SEM photograph of the platinum-palladium composite catalyst prepared by the production method of the present invention,
2 is a STEM X-ray map image showing the component distribution in the platinum-palladium composite catalyst of the present invention,
Figure 3 is a SEM photograph of the particles produced by the comparative example of the present invention.
이하, 본 발명을 보다 구체적으로 설명한다.
Hereinafter, the present invention will be described more specifically.
본 발명자들은 백금 촉매를 대체할 수 있는 새로운 촉매를 제조하기 위한 연구를 거듭한 결과, 백금 성분과 팔라듐 성분을 이온성 액체(ionic liquid) 내에서 공환원(coreduction)시킴으로써, 신규한 구조의 백금-팔라듐 복합체 촉매를 제조할 수 있음을 확인하고, 본 발명을 완성하였다.
The present inventors have conducted extensive research to produce a new catalyst that can replace the platinum catalyst. As a result, core structure of the platinum and palladium components in an ionic liquid can be reduced, thereby providing a novel structure of platinum- It was confirmed that the palladium composite catalyst can be prepared, and completed the present invention.
본 발명의 백금-팔라듐 복합체 촉매의 제조는, 백금 성분과 팔라듐 성분을 포함하는 재료 물질을 이온성 액체 내에서 공환원시키는 단계를 포함하여 이루어진다.
The preparation of the platinum-palladium composite catalyst of the present invention comprises the step of co-reducing a material material comprising a platinum component and a palladium component in an ionic liquid.
이때 상기 백금 성분을 포함하는 재료 물질로는, 예를 들면, 염화백금산칼륨(K2PtCl4)과 같은 백금 화합물이 사용될 수 있으며, 상기 팔라듐 성분을 포함하는 재료 물질로는, 예를 들면, 염화팔라듐산나트륨(Na2PdCl4)과 같은 팔라듐 화합물이 사용될 수 있다.
In this case, as a material material containing the platinum component, for example, a platinum compound such as potassium chloride (K 2 PtCl 4 ) may be used, and as the material material containing the palladium component, for example, chloride Palladium compounds such as sodium palladium (Na 2 PdCl 4 ) can be used.
도 1에는 이와 같은 방법으로 제조된 본 발명의 촉매를 배율을 달리하여 촬영한 사진들이 도시되어 있으며, 도 2에는 본 발명의 촉매 내의 성분 분포를 보여주는 이미지가 도시되어 있다.
1 shows photographs taken at different magnifications of the catalyst of the present invention prepared in this manner, and FIG. 2 shows an image showing the distribution of components in the catalyst of the present invention.
도 1을 통해 알 수 있듯이, 본 발명의 촉매는 별 모양 또는 성게 모양과 유사한 형태의 입자 형태를 갖는다. 보다 구체적으로는, 본 발명의 촉매는 이방성(anisotropic)을 가지는 다수의 침상 가지들의 뭉쳐진 형태, 바람직하게는 침상 가지가 입자의 중심으로부터 성장한 형상을 가진다. 또한, 촉매 입자의 전체 크기는 대략 5 내지 50nm 정도이며, 바람직하게는 5 내지 40nm, 더 바람직하게는 10 내지 30nm정도로 형성되었다.
As can be seen from Figure 1, the catalyst of the present invention has a particle form of a star or sea urchin-like form. More specifically, the catalyst of the present invention has an agglomerated form of a plurality of acicular anisotropic needles, preferably a needle branch is grown from the center of the particle. In addition, the total size of the catalyst particles is about 5 to 50 nm, preferably 5 to 40 nm, more preferably 10 to 30 nm.
한편, 도 2를 통해, 본 발명의 촉매에 있어서, 백금 성분과 팔라듐 성분이 촉매 입자 내부에 고르게 분산되어 있음을 확인할 수 있다.
On the other hand, it can be seen from FIG. 2 that in the catalyst of the present invention, the platinum component and the palladium component are evenly dispersed in the catalyst particles.
이하에서는 본 발명의 구체적인 실시예를 통해 본 발명을 보다 구체적으로 설명하기로 한다.
Hereinafter, the present invention will be described in more detail with reference to specific examples of the present invention.
실시예Example
마그네틱 바와 응축기를 구비한 둥근 플라스크에 증류수 8cc, 1-부틸-3-메틸이미다졸리움 트리플루오로메탄설포네이트 1.5cc, 폴리비닐피롤리돈(분자량 58000, PolyVinylPyrrolidone, PVP) 105mg, L-아스코르브산 60mg 및 포름산 1.5cc를 순차적으로 주입하고, 교반하면서 온도를 97℃까지 승온하였다.In a round flask equipped with a magnetic bar and a condenser, 8 cc of distilled water, 1.5 cc of 1-butyl-3-methylimidazolium trifluoromethanesulfonate, 105 mg of polyvinylpyrrolidone (molecular weight 58000, PolyVinylPyrrolidone, PVP), L-ascorbic acid 60 mg and 1.5 cc of formic acid were injected sequentially, and the temperature was heated up to 97 degreeC, stirring.
그런 다음, Na2PdCl4 15mg(0.051mmol)과 K2PtCl4 32mg(0.077mmol)을 3cc 증류수를 녹여 상기 플라스크에 주입하고, 4시간 동안 반응시킨 후, 상온으로 냉각시켰다. 그 결과, 도 1에 도시된 바와 같은 신규한 구조의 백금-팔라듐 복합체 촉매를 수득하였다.
Then, 15 mg (0.051 mmol) of Na 2 PdCl 4 and 32 mg (0.077 mmol) of K 2 PtCl 4 were dissolved in 3 cc distilled water, injected into the flask, and reacted for 4 hours, followed by cooling to room temperature. As a result, a platinum-palladium composite catalyst having a novel structure as shown in FIG. 1 was obtained.
비교예 Comparative example
마그네틱 바와 응축기를 구비한 둥근 플라스크에 증류수 8cc, 1-부틸-3-메틸이미다졸리움 트리플루오로메탄설포네이트 2cc, 폴리비닐피롤리돈(분자량 58000, PolyVinylPyrrolidone, PVP) 105mg, L-아스코르브산 60mg 및 포름산 1.5cc를 순차적으로 주입하고, 교반하면서 온도를 97℃까지 승온하였다.In a round flask equipped with a magnetic bar and condenser, 8 cc of distilled water, 2 cc of 1-butyl-3-methylimidazolium trifluoromethanesulfonate, 105 mg of polyvinylpyrrolidone (molecular weight 58000, PolyVinylPyrrolidone, PVP), 60 mg of L-ascorbic acid And 1.5 cc of formic acid were sequentially injected, and the temperature was raised to 97 ° C. while stirring.
그런 다음, Na2PdCl4 57mg을 주입하고, 4시간동안 반응시켰다. 생성된 Pd의 입자 크기는 약 8~9nm였으며, 이중 2cc를 취하여 다른 반응기에 옮겨 Pt와의 추가 반응을 실시하였다. 추가 반응은 상기 제조된 Pd 용액 2cc에, 증류수 6cc, 1-부틸-3-메틸이미다졸리움 트리플루오로메탄설포네이트 1.5cc, 폴리비닐피롤리돈(분자량 58000, PolyVinylPyrrolidone, PVP) 35mg, L-아스코르브산 60mg 및 포름산 1cc를 주입하고, 온도를 97℃로 승온하여 수행하였다. K2PtCl4 27mg을 3cc 증류수에 녹여 주입하였으며, 3시간동안 반응시켰다.Then, 57 mg of Na 2 PdCl 4 was injected and reacted for 4 hours. The particle size of the produced Pd was about 8-9 nm, of which 2 cc was taken and transferred to another reactor for further reaction with Pt. Further reaction was carried out by adding 6 cc of distilled water, 1.5 cc of 1-butyl-3-methylimidazolium trifluoromethanesulfonate, 35 mg of polyvinylpyrrolidone (molecular weight 58000, PolyVinylPyrrolidone, PVP) 60 mg of ascorbic acid and 1 cc of formic acid were charged, and the temperature was raised to 97 캜. 27 mg of K 2 PtCl 4 was dissolved in 3cc distilled water, and reacted for 3 hours.
도 3에는 이와 같은 방법으로 제조된 입자들의 SEM 사진이 도시되어 있다. 도 3을 통해 알 수 있듯이, 비교예의 경우, 백금과 팔라듐이 서로 혼합되지 않고, 동일 성분들끼리 뭉쳐져 2 ~ 3nm 정도의 백금 입자와 이보다 큰 팔라듐 입자가 각각 형성되는 것으로 확인되었다.3 shows an SEM photograph of the particles produced in this manner. As can be seen from FIG. 3, in the comparative example, platinum and palladium were not mixed with each other, and the same components were gathered together to form platinum particles of about 2 to 3 nm and larger palladium particles.
Claims (7)
이방성(anisotropic)을 가지는 다수의 침상 가지들이 뭉쳐진 형태로 형성된 백금-팔라듐 복합체 촉매.
Platinum component and palladium component are dispersed evenly inside the particle,
Platinum-palladium composite catalyst formed in the form of a plurality of needles having anisotropic agglomeration.
상기 백금-팔라듐 촉매는 별 모양 또는 성게 모양의 입자 형태인 백금-팔라듐 복합체 촉매.
The method of claim 1,
The platinum-palladium catalyst is a platinum-palladium composite catalyst in the form of star or sea urchin particles.
상기 다수의 침상 가지들은 입자의 중심으로부터 성장한 형상을 갖는 백금-팔라듐 복합 촉매.
The method of claim 1,
The plurality of needle-shaped branches are platinum-palladium composite catalyst having a shape grown from the center of the particle.
상기 백금-팔라듐 복합 촉매는 입자 크기가 5 내지 50nm인 백금-팔라듐 복합 촉매.
The method of claim 1,
The platinum-palladium composite catalyst is a platinum-palladium composite catalyst having a particle size of 5 to 50nm.
A method of producing a platinum-palladium catalyst comprising the step of coreducing a material comprising a platinum component and a material comprising a palladium component in an ionic liquid.
상기 백금 성분을 포함하는 재료는 염화백금산칼륨(K2PtCl4)인 백금-팔라듐 촉매 제조 방법.
The method of claim 5,
The material containing the platinum component is a platinum-palladium catalyst production method is potassium chloride (K 2 PtCl 4 ).
상기 팔라듐 성분을 포함하는 재료는 염화팔라듐산나트륨(Na2PdCl4)인 백금-팔라듐 촉매 제조 방법.The method of claim 5,
A material comprising the palladium component is sodium palladium chloride (Na 2 PdCl 4 ).
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