JPH0784608B2 - Method for producing fine palladium particles - Google Patents
Method for producing fine palladium particlesInfo
- Publication number
- JPH0784608B2 JPH0784608B2 JP5030188A JP5030188A JPH0784608B2 JP H0784608 B2 JPH0784608 B2 JP H0784608B2 JP 5030188 A JP5030188 A JP 5030188A JP 5030188 A JP5030188 A JP 5030188A JP H0784608 B2 JPH0784608 B2 JP H0784608B2
- Authority
- JP
- Japan
- Prior art keywords
- palladium
- particle size
- particles
- aqueous solution
- fine particles
- 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.)
- Expired - Lifetime
Links
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は微細なパラジウム粒子の製造方法に関するもの
である。TECHNICAL FIELD The present invention relates to a method for producing fine palladium particles.
（従来技術とその問題点） 従来、パラジウム微粒子の製造方法としては、還元剤と
してヒドラジンを用いて塩化パラジウム酸水溶液に水酸
化ナトリウムを加えて還元する方法が用いられてきた。(Prior Art and Problems Thereof) Conventionally, as a method for producing fine palladium particles, a method has been used in which hydrazine is used as a reducing agent and sodium hydroxide is added to an aqueous chloropalladic acid solution for reduction.
ところが、この方法では、還元された粒子同士が引き寄
せ合うために凝集した粒度分布の幅の広いパラジウム粒
子しか得られないという欠点を有していた。However, this method has a drawback that only reduced palladium particles attract each other and thus only agglomerated palladium particles having a wide particle size distribution can be obtained.
本発明は上記の欠点を解消せんがためになされたもので
あり、分散した、粒度分布の幅の狭い微細なパラジウム
粒子の粒径コントロール可能な製造方法を提供せんとす
るものである。The present invention has been made in order to solve the above drawbacks, and an object of the present invention is to provide a method for producing dispersed fine palladium particles having a narrow particle size distribution and capable of controlling the particle size.
（問題点を解決するための手段） 本発明は硝酸パラジウム水溶液中のパラジウムイオンを
還元してパラジウム微粒子を製造する方法において、還
元剤としてヒドロキシル（−OH）基を１個もしくは数個
含む芳香族化合物を用いることによって単分散したパラ
ジウム微粒子を得ることを特徴とするものである。(Means for Solving Problems) The present invention relates to a method for producing palladium fine particles by reducing palladium ions in an aqueous palladium nitrate solution, which is an aromatic compound containing one or several hydroxyl (—OH) groups as a reducing agent. It is characterized in that monodispersed palladium fine particles are obtained by using a compound.
而して本発明の製造方法において、ヒドロキシル（−O
H）基を１個もしくは数個含む芳香族化合物を用いる理
由は、これらの酸化還元電位が硝酸パラジウム水溶液を
還元するのに適当であると同時に粒子同士の凝集を防ぐ
働きがあるためである。Thus, in the production method of the present invention, hydroxyl (-O
The reason why the aromatic compound containing one or several H) groups is used is that these redox potentials are suitable for reducing the aqueous palladium nitrate solution and at the same time have a function of preventing the aggregation of particles.
さらに本発明において、硝酸パラジウム水溶液のpHは0.
1よりも低いと反応が遅くなり、８よりも高くても反応
が遅くなるので、0.1〜８の範囲がより好ましい。ヒド
ロキシル（−OH）基を１個もしくは数個含む芳香族化合
物のpHは1.0よりも低いと反応が極端に遅くなるので、
1.0以上がより好ましく、また、反応時の温度は10℃よ
り低いと反応が遅く、100℃を超えるとパラジウム微粒
子が凝集してくるので、10〜100℃の範囲がより好まし
い。Furthermore, in the present invention, the pH of the aqueous solution of palladium nitrate is 0.
When it is lower than 1, the reaction becomes slower and when it is higher than 8, the reaction becomes slower, so that the range of 0.1 to 8 is more preferable. If the pH of an aromatic compound containing one or several hydroxyl (-OH) groups is lower than 1.0, the reaction will be extremely slow, so
1.0 or more is more preferable, and if the temperature during the reaction is lower than 10 ° C., the reaction is slow, and if it exceeds 100 ° C., the fine palladium particles will agglomerate.
ここで本発明の実施例について説明する。Examples of the present invention will now be described.
（実施例１） 硝酸パラジウム液〔Pd（50g/）〕100mlを水で希釈し
て１の水溶液とした後、28％のアンモニア水を加えて
pH＝１に調整する。Example 1 100 ml of palladium nitrate solution [Pd (50 g /)] was diluted with water to give an aqueous solution of 1, and 28% aqueous ammonia was added.
Adjust to pH = 1.
また、ヒドロキノン100gを水に溶解し、500mlの水溶液
とした後、28％のアンモニア水を加えてpH＝７に調整す
る。ここで、この２液の温度を30℃にし、硝酸パラジウ
ム水溶液を攪拌しながらヒドロキノン水溶液を添加し、
30分間反応させる。得られたパラジウム微粒子は濾過、
洗浄して、粒度分布測定及び電子顕微鏡観察を行った。Further, 100 g of hydroquinone is dissolved in water to make 500 ml of an aqueous solution, and then 28% ammonia water is added to adjust the pH to 7. Here, the temperature of the two liquids is set to 30 ° C., and the aqueous solution of hydroquinone is added while stirring the aqueous solution of palladium nitrate,
Incubate for 30 minutes. The obtained palladium fine particles are filtered,
After washing, particle size distribution measurement and electron microscope observation were performed.
その結果、このパラジウム微粒子はほぼ球状で、平均粒
経が0.3μｍ、粒度分布は0.1〜0.3μｍに70％が入るシ
ャープなものであった。As a result, the palladium fine particles were almost spherical, and the average particle size was 0.3 μm, and the particle size distribution was as sharp as 70% in 0.1 to 0.3 μm.
（実施例２） 硝酸パラジウム液〔Pd（50g/）〕50mlを水で希釈して
１の水溶液とした後、28％のアンモニア水を加えてpH
＝３に調整する。(Example 2) 50 ml of palladium nitrate solution [Pd (50 g /)] was diluted with water to give an aqueous solution of 1, and then 28% ammonia water was added to adjust the pH.
Adjust to = 3.
また、ヒドロキノン50gを水に溶解し500mlの水溶液とし
た後、28％のアンモニア水を加えてpH＝６に調整する。
ここで、この２液の温度を50℃にし、硝酸パラジウム水
溶液を攪拌しながらヒドロキノン水溶液を添加し、60分
間反応させる。Also, after dissolving 50 g of hydroquinone in water to make 500 ml of an aqueous solution, 28% ammonia water is added to adjust pH = 6.
Here, the temperature of the two liquids is set to 50 ° C., the aqueous solution of hydroquinone is added to the aqueous solution of palladium nitrate while stirring, and the reaction is performed for 60 minutes.
得られたパラジウム微粒子は濾過、洗浄して、粒度分布
測定及び電子顕微鏡観察を行った。The obtained palladium fine particles were filtered and washed, and the particle size distribution was measured and observed with an electron microscope.
その結果、このパラジウム微粒子はほぼ球状で平均粒径
が0.5μｍ、粒度分布は0.3〜0.7μｍに70％が入るシャ
ープなものであった。As a result, the palladium fine particles were substantially spherical and had an average particle size of 0.5 μm, and the particle size distribution was as sharp as 70% in 0.3 to 0.7 μm.
（実施例３） 硝酸パラジウム液〔Pd（50g/）〕100mlを水で希釈し
て１の水溶液とした後、28％のアンモニア水を加えて
pH＝５に調整する。(Example 3) 100 ml of palladium nitrate solution [Pd (50 g /)] was diluted with water to give an aqueous solution of 1, and 28% aqueous ammonia was added.
Adjust to pH = 5.
また、ピロガロール100gを水に溶解し500mlの水溶液に
する。ここでこの２液の温度を40℃にし硝酸パラジウム
水溶液を攪拌しながらピロガロール水溶液を添加し30分
間反応させる。In addition, 100 g of pyrogallol is dissolved in water to make an aqueous solution of 500 ml. Here, the temperature of the two liquids is set to 40 ° C., and the aqueous solution of pyrogallol is added while stirring the aqueous solution of palladium nitrate, and the reaction is performed for 30 minutes.
得られたパラジウム微粒子は濾過、洗浄して、粒度分布
測定及び電子顕微鏡観察を行った。The obtained palladium fine particles were filtered and washed, and the particle size distribution was measured and observed with an electron microscope.
その結果、このパラジウム微粒子はほぼ球状で平均粒径
が0.6μｍ、粒度分布は0.4〜0.8μｍに70％が入るシャ
ープなものであった。As a result, the palladium fine particles were substantially spherical and had an average particle size of 0.6 μm, and the particle size distribution was as sharp as 70% in 0.4 to 0.8 μm.
（従来例） 塩化パラジウム液〔Pd（50g/）〕100mlを水で希釈し
て１の水溶液とした後、水酸化ナトリウムを加えてpH
＝８に調整する。(Conventional example) 100 ml of palladium chloride solution [Pd (50 g /)] was diluted with water to give an aqueous solution of 1, and sodium hydroxide was added to adjust the pH.
Adjust to = 8.
さらにこの液を攪拌しながら80％の抱水ヒドラジン水溶
液50mlを添加後、50℃で２時間攪拌した。Furthermore, while stirring this solution, 50 ml of an 80% hydrazine hydrate aqueous solution was added, and the mixture was stirred at 50 ° C. for 2 hours.
得られたパラジウム微粒子は濾過、洗浄して粒度分布測
定及び電子顕微鏡観察を行った。The obtained palladium fine particles were filtered and washed, and the particle size distribution was measured and observed with an electron microscope.
その結果、このパラジウム微粒子は不定形で、平均粒径
が1.8μｍ、粒度分布は0.3〜10μｍと幅が広く、凝集し
たものであった。As a result, the fine palladium particles were amorphous and had a wide average particle size of 1.8 μm and a particle size distribution of 0.3 to 10 μm, and were agglomerated.
（発明の効果） 上記の説明で明らかなように本発明の製造方法は硝酸パ
ラジウム水溶液を還元してパラジウム微粒子を製造する
方法において、還元剤としてヒドロキシル（−OH）基を
１個もしくは数個含む芳香族化合物を用いることによ
り、従来法では得られなかった単分散した粒度分布の幅
の狭い微細なパラジウム粒子を粒径をコントロールして
製造できるので、従来の製造方法にとって代わることの
できる画期的なものと言える。(Effects of the Invention) As is clear from the above description, the production method of the present invention is a method of producing palladium fine particles by reducing an aqueous palladium nitrate solution, and contains one or several hydroxyl (-OH) groups as a reducing agent. By using an aromatic compound, it is possible to produce fine palladium particles with a narrow monodispersed particle size distribution, which could not be obtained by the conventional method, by controlling the particle size. It can be said that
Claims (1)
ム微粒子を製造する方法において、還元剤としてヒドロ
キシル（−OH）基を１個もしくは数個含む芳香族化合物
を用いることによって単分散したパラジウム微粒子を得
ることを特徴とするパラジウム微粒子の製造方法。1. A method for producing palladium fine particles by reducing an aqueous solution of palladium nitrate, wherein monodispersed palladium fine particles are obtained by using an aromatic compound containing one or several hydroxyl (—OH) groups as a reducing agent. A method for producing fine palladium particles, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5030188A JPH0784608B2 (en) | 1988-03-03 | 1988-03-03 | Method for producing fine palladium particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5030188A JPH0784608B2 (en) | 1988-03-03 | 1988-03-03 | Method for producing fine palladium particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01225709A JPH01225709A (en) | 1989-09-08 |
| JPH0784608B2 true JPH0784608B2 (en) | 1995-09-13 |
Family
ID=12855071
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5030188A Expired - Lifetime JPH0784608B2 (en) | 1988-03-03 | 1988-03-03 | Method for producing fine palladium particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0784608B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111069622A (en) * | 2018-10-18 | 2020-04-28 | 株式会社则武 | Core-shell particles and use thereof |
-
1988
- 1988-03-03 JP JP5030188A patent/JPH0784608B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01225709A (en) | 1989-09-08 |
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