JPS6349253A - Method for mass-producing platinum-deposited catalyst - Google Patents
Method for mass-producing platinum-deposited catalystInfo
- Publication number
- JPS6349253A JPS6349253A JP61190874A JP19087486A JPS6349253A JP S6349253 A JPS6349253 A JP S6349253A JP 61190874 A JP61190874 A JP 61190874A JP 19087486 A JP19087486 A JP 19087486A JP S6349253 A JPS6349253 A JP S6349253A
- Authority
- JP
- Japan
- Prior art keywords
- reducing agent
- chloroplatinic acid
- catalyst
- platinum
- added
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims description 18
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 26
- 239000002253 acid Substances 0.000 claims abstract description 17
- 125000003172 aldehyde group Chemical group 0.000 claims abstract description 6
- 239000004280 Sodium formate Substances 0.000 claims abstract 2
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 claims abstract 2
- 235000019254 sodium formate Nutrition 0.000 claims abstract 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 48
- 229910052697 platinum Inorganic materials 0.000 claims description 24
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 4
- 238000004220 aggregation Methods 0.000 claims description 4
- 230000002776 aggregation Effects 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 235000019253 formic acid Nutrition 0.000 claims description 4
- 239000003112 inhibitor Substances 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 2
- 239000003595 mist Substances 0.000 claims 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000007921 spray Substances 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 150000003057 platinum Chemical class 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
Description
【発明の詳細な説明】
〔発明の属する技術分野〕
この発明は、カーボンブラックなどを触媒担体として用
いた白金担持触媒の量産化方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Technical field to which the invention pertains] The present invention relates to a method for mass producing a platinum-supported catalyst using carbon black or the like as a catalyst carrier.
液相において、試薬を用いて白金塩を還元して白金担持
触媒を得るためには、還元剤の添加方法が触媒の物性、
特に白金の分散に大きく寄与している。触媒の調製量が
少量の場合には、還元剤方法はそれほど触媒物性に大き
な影響を与えないが、触媒のｖ！４製量が多くなった場
合には大きな問題としてクローズアップされてくる。In order to obtain a supported platinum catalyst by reducing a platinum salt using a reagent in the liquid phase, the method of adding the reducing agent depends on the physical properties of the catalyst,
In particular, it greatly contributes to the dispersion of platinum. When the amount of catalyst prepared is small, the reducing agent method does not have much effect on the physical properties of the catalyst, but the v! 4. If the production volume increases, it will be highlighted as a major problem.
例えば、親水処理を施した触媒担体を塩化白金酸水溶液
を十分に接触させた後に、系のＰ）（をアルカリ性にし
、還元剤が作用する温度まで系の温度を上げ、コロイド
凝集防止剤を添加しアルデヒド基を有する還元剤を徐々
に添加し塩化白金酸を還元するという方法においてその
スケールアップの検討を当業者に於いて慌討した結果、
調製量が少ない場合（約１００．９ ロット程度）には
還元剤を分液ロートで滴下していた。そこで１ ｋｇ程
度の触媒を調製する場合にも、その初期においては、分
液ロートを用いて触媒を調製する試みを行った。ところ
が滴下条件を変更しても、出来上がった触媒の物性が（
特に白金の平均結晶子径）改善されず、還元剤の滴下方
法についての改善を余儀なくされた。特に、この方法に
おいては、還元剤として蟻酸を用いると、かなり短時間
において、系内で塩化白金酸の還元がおこるために、還
元剤を集中曲番こ添加すると、白金の分散状態が悪くな
る。For example, after sufficiently contacting a hydrophilically treated catalyst carrier with an aqueous solution of chloroplatinic acid, the P) in the system is made alkaline, the temperature of the system is raised to the temperature at which the reducing agent acts, and a colloidal aggregation inhibitor is added. As a result of a flurry of studies by those skilled in the art to scale up the method of reducing chloroplatinic acid by gradually adding a reducing agent having an aldehyde group,
When the amount to be prepared was small (approximately 100.9 lots), the reducing agent was added dropwise using a separating funnel. Therefore, even when preparing a catalyst weighing about 1 kg, an attempt was made to prepare the catalyst using a separatory funnel at the initial stage. However, even if the dropping conditions were changed, the physical properties of the finished catalyst remained (
In particular, the average crystallite diameter of platinum) was not improved, and it was necessary to improve the method of dropping the reducing agent. In particular, in this method, when formic acid is used as a reducing agent, reduction of chloroplatinic acid occurs within the system in a fairly short time, so if the reducing agent is added in a concentrated manner, the dispersion state of platinum will deteriorate. .
この発明は、親水処理を施した触媒担体を塩化白金酸水
溶液を十分に接触させた後に、系のＰＨをアルカリ性に
し、還元剤が作用する温度まで系の温度を上げ、コロイ
ド凝集防止剤を添加しアルデヒド基を有する還元剤を徐
々に添刀口し塩化白金酸を還元するという方法において
、白金担持触媒の量産を可能にする還元剤の滴下方法を
提供することを目的とする。In this invention, after sufficiently contacting a hydrophilically treated catalyst carrier with an aqueous chloroplatinic acid solution, the pH of the system is made alkaline, the temperature of the system is raised to the temperature at which a reducing agent acts, and a colloidal aggregation inhibitor is added. An object of the present invention is to provide a method for dropping a reducing agent that enables mass production of a supported platinum catalyst in a method of reducing chloroplatinic acid by gradually adding a reducing agent having an aldehyde group.
この目的は本発明によれば、親水処理を施した触媒担体
に塩化白金酸水溶液を十分に接触させた後に、系のＰＨ
をアルカリ性にし、還元剤が作用する温度まで系の温度
を上げ、コロイド凝集防止剤を添加しアルデヒド基を有
する還元剤を徐々に添加し塩化白金酸を還元するという
方法において、還元剤を霧状で滴下することにより達成
される。According to the present invention, this purpose is achieved by sufficiently contacting a hydrophilically treated catalyst carrier with an aqueous chloroplatinic acid solution, and then adjusting the pH of the system.
In this method, the reducing agent is made alkaline, the temperature of the system is raised to the temperature at which the reducing agent acts, a colloidal aggregation inhibitor is added, and a reducing agent having an aldehyde group is gradually added to reduce the chloroplatinic acid. This is accomplished by dripping.
このようにしたために触媒調製段階において、より広い
範囲に還元剤が添加され、大きな滴状で添加していた場
合と比較して、白金粒子の分散がより良くなり白金担持
触媒の量産においても、少量で調製した触媒と同様な物
性を有する高分散な白金担持触媒が得られるようになる
。This allows the reducing agent to be added over a wider area during the catalyst preparation stage, resulting in better dispersion of platinum particles compared to when it is added in large droplets, and even in the mass production of platinum-supported catalysts. A highly dispersed platinum-supported catalyst having physical properties similar to those of a catalyst prepared in a small amount can be obtained.
（実施例１）
アセチレンブラック９００ｇにｌＱｗｔ％硝酸水溶液４
０リットルを添加し、攪拌しながら、系の温度を５０°
Ｃに昇温し、この状態で約２時間攪拌した。その後、痣
過しケーキのＰＨが約７になるまで十分に脱イオン水で
洗浄した。洗浄の完了したケーキに脱イオン水４０リツ
トルを添加し分散をした。次に白金として１００ｇを含
有する塩化白金酸１０リツトルを添加し室温において攪
拌した。(Example 1) 1 Qwt% nitric acid aqueous solution 4 to 900 g of acetylene black
Add 0 liters and raise the temperature of the system to 50° while stirring.
The temperature was raised to 40°C, and the mixture was stirred in this state for about 2 hours. Thereafter, the blemish cake was thoroughly washed with deionized water until the pH of the blemish cake was approximately 7. 40 liters of deionized water was added to the washed cake for dispersion. Next, 10 liters of chloroplatinic acid containing 100 g of platinum was added and stirred at room temperature.
次にこれに、０．１Ｍの炭酸す） ＩＪウム水溶液１９
．５リツトルを添加し攪拌をした。この後に系の温度を
約５０°０まで昇温した。昇温完了後 ３Ｑｗｔ％の過
酸化水素水を１リツトル添加し約５分間攪拌した。これ
にひきつづき０．１ Ｍの蟻酸水溶液１３リツトルをス
プレーを用いて霧状にして約２時間かけて徐々に添加し
た。蟻酸を児全に添加後さらに攪拌をした。以上の操作
が完了後、反応物を濾過し、さらに、脱イオン水で十分
に洗浄した。洗浄の終点は、塩素と硝酸銀が反応して塩
化銀が生成する反応を利用して決定した。Next, add 0.1M carbonate (IJ) aqueous solution 19
．． 5 liters was added and stirred. After this, the temperature of the system was raised to about 50°0. After the temperature was raised, 1 liter of 3Qwt% hydrogen peroxide solution was added and stirred for about 5 minutes. Subsequently, 13 liters of a 0.1 M aqueous formic acid solution was atomized using a sprayer and gradually added over about 2 hours. After adding formic acid to the mixture, the mixture was further stirred. After the above operations were completed, the reaction product was filtered and further washed thoroughly with deionized water. The end point of cleaning was determined using the reaction between chlorine and silver nitrate to produce silver chloride.
調製の完了した触媒を分析した結果、白金の担持量は、
約１０．５％であり、Ｘ線回折により白金の平均結晶子
径を分析した結果、白金の（１１１）面でのピークの値
より担持白金の平均結晶子径は約３０！であることがわ
かった。As a result of analyzing the prepared catalyst, the amount of platinum supported was
The average crystallite diameter of platinum was analyzed by X-ray diffraction, and based on the value of the peak on the (111) plane of platinum, the average crystallite diameter of the supported platinum was approximately 30! It turned out to be.
白金粒子の分散性の悪い触媒は熱処理すると。Catalysts with poor dispersibility of platinum particles can be heat treated.
さらに分散性が悪くなる（白金のシンタリングが起こり
易いため）ことが、当業者においてすでにわかっていた
ために、念のために得られた触媒を９００°Ｃ１窒素雰
囲気で約２時間処理して、白金のシンタリング状態をみ
てみた。その結果、Ｘ線回折の結果では、予想していた
ように白金のシンタリングが殆ど起っておらず白金がア
セチレンブラック担体上に良く分散していることが証明
された。Since those skilled in the art already knew that the dispersibility would further worsen (because sintering of platinum easily occurs), the obtained catalyst was treated in a nitrogen atmosphere at 900° C. for about 2 hours just to be sure. I looked at the sintering condition of platinum. As a result, the results of X-ray diffraction showed that almost no sintering of platinum occurred, as expected, and that platinum was well dispersed on the acetylene black carrier.
さらに、電子顕微鏡により、触媒を直接観察した結果、
やはり、白金は小さいままで良く分散していることがわ
かった。Furthermore, as a result of direct observation of the catalyst using an electron microscope,
As expected, it was found that platinum remained small and well dispersed.
（比較例）
比較のため、実施例１と同じ触媒調製法において、還元
剤の添加を分液ロートを用いて触媒の調製を行った。他
の条件は、実施例１と同じである。(Comparative Example) For comparison, a catalyst was prepared using the same catalyst preparation method as in Example 1, using a separating funnel to add a reducing agent. Other conditions are the same as in Example 1.
出来上がった触媒について実施例１と同じにＸ線回折、
熱処理、電子顕微鏡観察を行ったが、その結果はどれも
予想どおりに白金の分散性が悪いという結果をもたらし
た。特に電子顕微鏡による観察では、多くの白金の集落
が観察された。The finished catalyst was subjected to X-ray diffraction in the same manner as in Example 1.
Heat treatment and electron microscope observation were performed, but as expected, the results showed that platinum had poor dispersibility. In particular, many platinum colonies were observed when observed using an electron microscope.
以上の説明から明らかなようにこの発明によれば、白金
担持触媒を量産するにあたり、還元剤をスプレーなどの
方法により霧状にして添加するようにしたために、反応
系の中で還元剤がより広い範囲に添加できるようになり
、大量の触媒を調製した場合においても、少量の場合と
同様な高分散な白金担持触媒が得られる。As is clear from the above description, according to the present invention, when mass producing platinum-supported catalysts, the reducing agent is added in atomized form by a method such as spraying, so that the reducing agent is more concentrated in the reaction system. It can now be added over a wide range, and even when a large amount of catalyst is prepared, a highly dispersed platinum-supported catalyst similar to that obtained when a small amount is prepared can be obtained.
Claims (4)
十分に接触させた後に、系のＰＨをアルカリ性にし、還
元剤が作用する温度まで系の温度を上げ、コロイド凝集
防止剤を添加しアルデヒド基を有する還元剤を除々に添
加し塩化白金酸を還元、担持する方法により白金担持触
媒を量産する過程において、前記還元剤を霧状に添加す
ることを特徴とする白金担持触媒の量産方法。(1) After sufficiently contacting a chloroplatinic acid aqueous solution with a hydrophilically treated catalyst carrier, the pH of the system is made alkaline, the temperature of the system is raised to the temperature at which the reducing agent acts, and a colloidal aggregation inhibitor is added. A method for mass producing a supported platinum catalyst, which comprises adding the reducing agent in the form of mist during the process of mass producing a supported platinum catalyst by gradually adding a reducing agent having an aldehyde group to reduce and support chloroplatinic acid. .
白金酸の還元試薬として、蟻酸を用いることを特徴とす
る白金担持触媒の量産方法。(2) A method for mass production of a supported platinum catalyst, characterized in that in the method according to claim 1, formic acid is used as a reducing reagent for chloroplatinic acid.
白金酸の還元試薬として、蟻酸ナトリウムを用いること
を特徴とする白金担持触媒の量産方法。(3) A method for mass production of a supported platinum catalyst, characterized in that, in the method according to claim 1, sodium formate is used as a reducing reagent for chloroplatinic acid.
剤をスプレーにより霧状に添加することを特徴とする白
金担持触媒の量産方法。(4) A method for mass production of a supported platinum catalyst according to claim 1, characterized in that the reducing agent is added in the form of a mist by spraying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61190874A JPS6349253A (en) | 1986-08-14 | 1986-08-14 | Method for mass-producing platinum-deposited catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61190874A JPS6349253A (en) | 1986-08-14 | 1986-08-14 | Method for mass-producing platinum-deposited catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6349253A true JPS6349253A (en) | 1988-03-02 |
| JPH0463733B2 JPH0463733B2 (en) | 1992-10-12 |
Family
ID=16265188
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61190874A Granted JPS6349253A (en) | 1986-08-14 | 1986-08-14 | Method for mass-producing platinum-deposited catalyst |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6349253A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1061145A1 (en) * | 1999-06-18 | 2000-12-20 | W.C. Heraeus GmbH & Co. KG | Process of producing high purity platinum from a hexachloroplatinate solution |
| KR20230006471A (en) | 2021-07-01 | 2023-01-10 | 이시후꾸 긴조꾸 고오교 가부시끼가이샤 | Manufacturing method of platinum cobalt chrome alloy supported carbon catalyst for fuel cell |
-
1986
- 1986-08-14 JP JP61190874A patent/JPS6349253A/en active Granted
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1061145A1 (en) * | 1999-06-18 | 2000-12-20 | W.C. Heraeus GmbH & Co. KG | Process of producing high purity platinum from a hexachloroplatinate solution |
| US6315811B1 (en) | 1999-06-18 | 2001-11-13 | W. C. Heraeus Gmbh & Co. Kg | Method for producing platinum |
| KR20230006471A (en) | 2021-07-01 | 2023-01-10 | 이시후꾸 긴조꾸 고오교 가부시끼가이샤 | Manufacturing method of platinum cobalt chrome alloy supported carbon catalyst for fuel cell |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0463733B2 (en) | 1992-10-12 |
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