JPH0784609B2 - Method for producing fine palladium particles - Google Patents
Method for producing fine palladium particlesInfo
- Publication number
- JPH0784609B2 JPH0784609B2 JP5030288A JP5030288A JPH0784609B2 JP H0784609 B2 JPH0784609 B2 JP H0784609B2 JP 5030288 A JP5030288 A JP 5030288A JP 5030288 A JP5030288 A JP 5030288A JP H0784609 B2 JPH0784609 B2 JP H0784609B2
- Authority
- JP
- Japan
- Prior art keywords
- palladium
- particles
- particle size
- fine
- aqueous solution
- 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
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 Its Problems) Conventionally, as a method for producing fine palladium particles, a method has been used in which sodium hydroxide is added to an aqueous solution of chloropalladic acid using hydrazine as a reducing agent 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） 本発明はパラジウムアンモニウム錯体溶液中のパラジウ
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 the Problems) The present invention relates to a method for producing palladium fine particles by reducing palladium ions in a palladium ammonium complex solution, wherein 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 group 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パラジウムアンモニウム
錯体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 an aromatic compound containing one or several H) groups is used is that these redox potentials are suitable for reducing the palladium ammonium complex solution and at the same time have a function of preventing aggregation of particles. .
さらに本発明において、パラジウムアンモニウム錯体溶
液のpHは８よりも低いと析出した粒子が凝集し、13より
高いとアンモニアガスの発生が多くなり、反応が遅くな
るので、８〜13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。Further, in the present invention, when the pH of the palladium ammonium complex solution is lower than 8, the precipitated particles agglomerate, and when it is higher than 13, the generation of ammonia gas is increased and the reaction becomes slow, so that the range of 8 to 13 is more preferable. . The pH of aromatic compounds containing one or several hydroxyl (-OH) groups is
If it is lower than 1.0, the reaction becomes extremely slow, so 1.0 or more is more preferable, and if the temperature at the time of reaction is lower than 10 ° C, the reaction is slow, and if it exceeds 100 ° C, the fine palladium particles start to aggregate. The range of -100 ° C is more preferable.
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＝９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 = 9.
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＝３に調整す
る。ここで、この２液の温度を30℃にし、パラジウムア
ンモニウム錯体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, 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 3. Here, the temperature of the two liquids is set to 30 ° C., the aqueous solution of hydroquinone is added to the palladium ammonium complex solution 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0.8μｍ、粒度分布は0.6〜1.0μｍ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 0.8 μm, and the particle size distribution was as sharp as 70% in 0.6 to 1.0 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
＝11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 ＝ 11.
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＝７に調整する。
ここで、この２液の温度を50℃にし、パラジウムアンモ
ニウム錯体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。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 = 7.
Here, the temperature of the two liquids is set to 50 ° C., the aqueous solution of hydroquinone is added to the palladium ammonium complex solution while stirring, and they are reacted 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0.5μｍ、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＝10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 = 10.
また、ピロガロール100gを水に溶解し１の水溶液にす
る。ここでこの２液の温度を60℃にしパラジウムアンモ
ニウム錯体溶液を攪拌しながらピロガロール水溶液を添
加し90分間反応させる。In addition, 100 g of pyrogallol is dissolved in water to prepare an aqueous solution of 1. Here, the temperature of the two liquids is set to 60 ° C., and the aqueous solution of pyrogallol is added to the palladium ammonium complex solution while stirring and the reaction is performed for 90 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1.0μｍ、粒度分布は0.8〜1.2μｍ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 1.0 μm, and the particle size distribution was sharp such that 70% was included in 0.8 to 1.2 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おこなった。The obtained fine palladium 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パラジ
ウムアンモニウム錯体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。(Effect 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 a palladium ammonium complex solution, wherein one or several hydroxyl (-OH) groups are used as a reducing agent. By using an aromatic compound containing, fine palladium particles having a narrow monodispersed particle size distribution, which could not be obtained by the conventional method, can be produced by controlling the particle size, and thus an alternative method to the conventional production method can be obtained. It can be said that it is a term.
Claims (1)
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パラジウム微粒子の製造
方法。1. A method for producing palladium fine particles by reducing a palladium ammonium complex solution, wherein palladium fine particles monodispersed 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 |
|---|---|---|---|
| JP5030288A JPH0784609B2 (en) | 1988-03-03 | 1988-03-03 | Method for producing fine palladium particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5030288A JPH0784609B2 (en) | 1988-03-03 | 1988-03-03 | Method for producing fine palladium particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01225710A JPH01225710A (en) | 1989-09-08 |
| JPH0784609B2 true JPH0784609B2 (en) | 1995-09-13 |
Family
ID=12855101
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5030288A Expired - Lifetime JPH0784609B2 (en) | 1988-03-03 | 1988-03-03 | Method for producing fine palladium particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0784609B2 (en) |
-
1988
- 1988-03-03 JP JP5030288A patent/JPH0784609B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01225710A (en) | 1989-09-08 |
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