JPH078807A - Production of catalyst - Google Patents
Production of catalystInfo
- Publication number
- JPH078807A JPH078807A JP5172680A JP17268093A JPH078807A JP H078807 A JPH078807 A JP H078807A JP 5172680 A JP5172680 A JP 5172680A JP 17268093 A JP17268093 A JP 17268093A JP H078807 A JPH078807 A JP H078807A
- Authority
- JP
- Japan
- Prior art keywords
- platinum
- catalyst
- carrier
- solution
- ion
- 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.)
- Pending
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000010419 fine particle Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 5
- -1 platinum ion Chemical class 0.000 abstract description 9
- 239000004094 surface-active agent Substances 0.000 abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract 1
- 238000000151 deposition Methods 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 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 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000004280 Sodium formate Substances 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、白金粒子が担体上に均
一微細に分散した触媒の製造方法に関する。TECHNICAL FIELD The present invention relates to a method for producing a catalyst in which platinum particles are uniformly and finely dispersed on a carrier.
【０００２】[0002]
【従来の技術】白金触媒の製造方法は、従来から多数知
られており、一般的には塩化白金酸水溶液にアルミナ、
カーボン等の担体を加えておき、これへギ酸、ギ酸ソー
ダ、ヒドラジン、水素化ホウ素ナトリウム等の還元剤を
加え、白金微粒子を還元させ、担体上に吸着させてい
た。なお、この際還元した白金粒子が凝集してしまい粒
子径が大きくなってしまい触媒活性が低下してしまうた
め、界面活性剤等を加えて白金粒子の凝集を防止してい
た。2. Description of the Related Art A number of methods for producing platinum catalysts have been known so far, and in general, an aqueous solution of chloroplatinic acid and alumina,
A carrier such as carbon was added in advance, and a reducing agent such as formic acid, sodium formate, hydrazine, sodium borohydride was added thereto to reduce the platinum fine particles and to adsorb on the carrier. At this time, the reduced platinum particles agglomerate to increase the particle size and reduce the catalytic activity. Therefore, a surfactant or the like is added to prevent the platinum particles from aggregating.
【０００３】[0003]
【発明が解決しようとする課題】ところが上記のように
界面活性剤を添加しても、凝集防止効果は不十分であ
り、また最終製品より界面活性剤を除去するため洗浄が
複雑になったり、加熱除去するなど手数がかかるという
問題があった。However, even if a surfactant is added as described above, the effect of preventing coagulation is insufficient, and cleaning is complicated because the surfactant is removed from the final product. There is a problem that it takes time and labor such as removing by heating.
【０００４】本発明は上記課題を解決し、界面活性剤を
用いずに、均一で微細な白金微粒子が担持した触媒の製
造方法を提供することを目的とする。An object of the present invention is to solve the above problems and to provide a method for producing a catalyst in which uniform and fine platinum fine particles are supported without using a surfactant.
【０００５】[0005]
【課題を解決するための手段】本発明は白金イオン及び
該白金イオンの還元により生成する白金微粒子が担持さ
れる担体を含む溶液中に、還元剤を加えて白金微粒子に
還元して前記担体上に担持した触媒を製造する方法にお
いて、白金イオン溶液としてジニトロジアミノ硝酸溶液
を使用し、かつ還元剤としてエタノールを使用すること
により目的は達成される。上記構成を用いることによ
り、界面活性剤を用いなくても、白金粒子が凝集せず、
担体上に白金微粒子が均一、高分散に担持された触媒が
得られることがあきらかとなった。また界面活性剤を用
いていないため、洗浄も簡単におこなわれた。According to the present invention, a reducing agent is added to a solution containing a platinum ion and a carrier on which platinum fine particles produced by reduction of the platinum ion are carried to reduce the platinum fine particles on the carrier. In a method for producing a catalyst supported on, the object is achieved by using a dinitrodiaminonitric acid solution as the platinum ion solution and ethanol as the reducing agent. By using the above configuration, without using a surfactant, the platinum particles do not aggregate,
It became clear that a catalyst was obtained in which platinum fine particles were uniformly and highly dispersed on a carrier. In addition, since no surfactant was used, cleaning was easy.
【０００６】[0006]
【実施例】白金濃度 5.8ｇ／ｌのジニトロジアミノ硝酸
溶液 850mlと98.5％のエタノール850mlを混合し、これ
へ表面積60〜 400ｍ2 ／ｇのカーボン10ｇを加え、超音
波ホモジナイザーで２分間混合した。その後該混合液を
還流装置付きの容器に入れ、80℃の温度で16時間加熱還
流し、白金イオンの還元を行った。還元終了後濾過洗浄
を濾液が中性になるまで行い、その後60℃で一晩乾燥
し、さらにチッ素気流中で 250℃で30分間乾燥すること
により、カーボン上に白金微粒子が担持された触媒が得
られた。この触媒を電子顕微鏡により観察したところ白
金粒子は担体上に均一高分散に担持されており、一酸化
炭素吸着法により求めた白金粒子の径は15〜18Åであっ
た。Example 850 ml of a dinitrodiaminonitric acid solution having a platinum concentration of 5.8 g / l and 850 ml of 98.5% ethanol were mixed, to which 10 g of carbon having a surface area of 60 to 400 m 2 / g was added, and the mixture was mixed with an ultrasonic homogenizer for 2 minutes. Then, the mixed solution was put into a container equipped with a reflux device, and heated and refluxed at a temperature of 80 ° C. for 16 hours to reduce platinum ions. After completion of the reduction, filtration and washing are performed until the filtrate becomes neutral, then dried at 60 ° C overnight, and further dried at 250 ° C for 30 minutes in a nitrogen stream to obtain a catalyst with platinum fine particles supported on carbon. was gotten. When this catalyst was observed by an electron microscope, the platinum particles were uniformly and highly dispersed on the carrier, and the diameter of the platinum particles determined by the carbon monoxide adsorption method was 15 to 18Å.
【０００７】[0007]
【従来例】イソプロピルアルコール 250ml及び水 100ml
の混合液へ、ポリビニルアルコール２ｇを溶解した。こ
れへ白金濃度20ｇ／ｌの塩化白金酸溶液 100mlを加え、
アンモニア水でｐＨ2.2 に調整した後蒸溜水で全量を 5
00mlとした。次に該混合液へカーボン20ｇを加え、よく
混合した。その後該混合液を還流装置付きの容器に入
れ、70℃を温度で６時間加熱還流し、白金イオンの還元
を行った。その後濾過、水洗を濾液が中性となるまで行
い、さらに乾燥を行うことにより、担体上に白金粒子が
担持された触媒が得られた。この触媒の電子顕微鏡観察
を行ったところ、白金粒子径は30〜50Åであり、ところ
どころに白金粒子の凝集が見られた。[Conventional example] 250 ml of isopropyl alcohol and 100 ml of water
2 g of polyvinyl alcohol was dissolved in the mixed solution. To this, add 100 ml of chloroplatinic acid solution with a platinum concentration of 20 g / l,
Adjust the pH to 2.2 with aqueous ammonia, then add 5 to the total volume with distilled water.
It was set to 00 ml. Next, 20 g of carbon was added to the mixed solution and mixed well. Then, the mixed solution was placed in a container equipped with a reflux device, and heated at 70 ° C. under reflux for 6 hours to reduce platinum ions. Then, filtration and washing with water were carried out until the filtrate became neutral, and further drying was carried out to obtain a catalyst in which platinum particles were supported on the carrier. An electron microscopic observation of this catalyst revealed that the platinum particle diameter was 30 to 50 Å, and that platinum particle aggregation was observed here and there.
【０００８】[0008]
【発明の効果】以上説明してきたように、本発明の製造
方法を用いれば、界面活性剤の使用なしで均一で微細な
白金微粒子が担持した触媒を製造することができ、水洗
の手間が簡素化できるとともに、高活性の触媒を得る方
法としてたいへん有用である。As described above, the use of the production method of the present invention makes it possible to produce a catalyst in which uniform and fine platinum fine particles are supported without using a surfactant, and the washing with water is simple. It is very useful as a method for obtaining a highly active catalyst.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 只野 悦子 神奈川県平塚市新町２番73号 田中貴金属 工業株式会社技術開発センター内 (72)発明者 杉本 晴子 神奈川県平塚市新町２番73号 田中貴金属 工業株式会社技術開発センター内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Etsuko Tadano 2-73 Shinmachi, Hiratsuka City, Kanagawa Prefectural Technology Development Center, Tanaka Kikinzoku Kogyo Co., Ltd. (72) Haruko Sugimoto 2-73 Shinmachi, Hiratsuka, Kanagawa Prefecture Tanaka Kikinzoku Industry Development Center
Claims (1)
り生成する白金微粒子が担持される担体を含む溶液中
に、還元剤を加えて白金微粒子に還元して前記担体上に
担持した触媒を製造する方法において、白金イオン溶液
としてジニトロジアミノ硝酸溶液を使用し、かつ還元剤
としてエタノールを使用することを特徴とする高分散微
細白金粒子担持触媒の製造方法。1. A catalyst containing a platinum ion and platinum fine particles produced by reduction of the platinum ion is added to a solution containing a carrier to reduce the platinum fine particles to produce a catalyst supported on the carrier. In the method, a dinitrodiaminonitric acid solution is used as a platinum ion solution, and ethanol is used as a reducing agent, which is a method for producing a highly dispersed fine platinum particle-supported catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5172680A JPH078807A (en) | 1993-06-18 | 1993-06-18 | Production of catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5172680A JPH078807A (en) | 1993-06-18 | 1993-06-18 | Production of catalyst |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH078807A true JPH078807A (en) | 1995-01-13 |
Family
ID=15946378
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5172680A Pending JPH078807A (en) | 1993-06-18 | 1993-06-18 | Production of catalyst |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH078807A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2021094529A (en) * | 2019-12-18 | 2021-06-24 | トヨタ紡織株式会社 | Method for producing noble metal fine particle-supported catalyst, method for producing noble metal fine particles, noble metal fine particle-supported catalyst, and noble metal fine particles |
-
1993
- 1993-06-18 JP JP5172680A patent/JPH078807A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2021094529A (en) * | 2019-12-18 | 2021-06-24 | トヨタ紡織株式会社 | Method for producing noble metal fine particle-supported catalyst, method for producing noble metal fine particles, noble metal fine particle-supported catalyst, and noble metal fine particles |
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