JPH0784606B2 - Method for producing fine palladium particles - Google Patents
Method for producing fine palladium particlesInfo
- Publication number
- JPH0784606B2 JPH0784606B2 JP5029988A JP5029988A JPH0784606B2 JP H0784606 B2 JPH0784606 B2 JP H0784606B2 JP 5029988 A JP5029988 A JP 5029988A JP 5029988 A JP5029988 A JP 5029988A JP H0784606 B2 JPH0784606 B2 JP H0784606B2
- Authority
- JP
- Japan
- Prior art keywords
- palladium
- particles
- particle size
- ascorbic acid
- 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Ｌ−アスコルビン酸又はＬ−アス
コルビン酸塩類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) In the method for producing palladium fine particles by reducing palladium ions in a palladium ammonium complex solution, the present invention uses L-ascorbic acid or L-ascorbates as a reducing agent. It is characterized in that monodispersed palladium fine particles are obtained.
而して本発明の製造方法において、Ｌ−アスコルビン酸
又は、Ｌ−アスコルビン酸塩類を用いる理由は、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, the reason for using L-ascorbic acid or L-ascorbic acid salts is that their redox potential is suitable for reducing the palladium ammonium complex solution and at the same time the particles are aggregated. This is because it has the function of preventing
また、本発明の請求範囲においてＬ−アスコルビン酸及
びＬ−アスコルビン酸塩類としては、ナトリウム塩、カ
リウム塩、アンモニウム塩等を問わない。Further, in the claims of the present invention, the L-ascorbic acid and L-ascorbic acid salts may be sodium salts, potassium salts, ammonium salts or the like.
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く、Ｌ−アスコルビ
ン酸のpHは0.5よりも低いと反応が極端に遅くなるの
で、0.5以上がより好ましい。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 are aggregated, and when it is higher than 13, the generation of ammonia gas is increased and the reaction is delayed, so that the range of 8 to 13 is more preferable. If the pH of L-ascorbic acid is lower than 0.5, the reaction becomes extremely slow, so 0.5 or more is more preferable. The reaction temperature is 10
When the temperature is lower than 0 ° C, the reaction is slow, and when the temperature is higher than 100 ° C, the fine palladium particles are aggregated. Therefore, the range of 10 to 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、Ｌ−アスコルビン酸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＝４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Ｌ−アスコルビ
ン酸溶液を添加し、60分間反応させる。Further, 100 g of L-ascorbic acid is dissolved in water to prepare a 500 ml aqueous solution, and 28% ammonia water is added to adjust the pH to 4. Here, the temperature of these two solutions is set to 50 ° C., the L-ascorbic acid solution is added to the palladium ammonium complex solution while stirring, and the mixture is reacted 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0.7μｍ、粒度分布は0.5〜1.0μｍ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 0.7 μm, and the particle size distribution was as sharp as 70% in 0.5 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、Ｌ−アスコルビン酸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Ｌ−アスコルビン
酸溶液を添加し、30分間反応させる。Further, 50 g of L-ascorbic acid is dissolved in water to prepare a 500 ml aqueous solution, and 28% ammonia water is added to adjust pH = 6. Here, the temperature of the two liquids is set to 30 ° C., the L-ascorbic acid solution is added to the palladium ammonium complex solution while stirring, and the mixture is 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0.2μｍ、粒度分布は0.1〜0.4μｍ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 0.2 μm, and the particle size distribution was as sharp as 70% in 0.1 to 0.4 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、Ｌ−アスコルビン酸ナトリウム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70℃にし
パラジウムアンモニウム錯体溶液を攪拌しながらＬ−ア
スコルビン酸ナトリウムを添加し、120分間反応させ
る。Further, 100 g of sodium L-ascorbate is dissolved in water to obtain an aqueous solution of 1. Here, the temperature of the two liquids is adjusted to 70 ° C., sodium L-ascorbate is added to the palladium ammonium complex solution while stirring, and the mixture is reacted for 120 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1.2μｍ、粒度分布は1.0〜1.5μｍ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 1.2 μm, and the particle size distribution was as sharp as 70% in 1.0 to 1.5 μm.
（従来例） 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、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 nitrate 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Ｌ−アスコルビ
ン酸又はＬ−アスコルビン酸塩類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 apparent from the above description, the production method of the present invention uses L-ascorbic acid or L-ascorbates as a reducing agent in the method of producing palladium fine particles by reducing a palladium ammonium complex solution. By
Since 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, it can be said to be an epoch-making thing that can replace the conventional production method.
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Ｌ−アスコルビン酸又はＬ−アスコルビン酸塩類を
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 monodispersed palladium fine particles are obtained by using L-ascorbic acid or L-ascorbic acid salts as a reducing agent. Method for producing fine palladium particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5029988A JPH0784606B2 (en) | 1988-03-03 | 1988-03-03 | Method for producing fine palladium particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5029988A JPH0784606B2 (en) | 1988-03-03 | 1988-03-03 | Method for producing fine palladium particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01225707A JPH01225707A (en) | 1989-09-08 |
| JPH0784606B2 true JPH0784606B2 (en) | 1995-09-13 |
Family
ID=12855016
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5029988A Expired - Lifetime JPH0784606B2 (en) | 1988-03-03 | 1988-03-03 | Method for producing fine palladium particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0784606B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6933151B2 (en) * | 2018-01-29 | 2021-09-08 | 住友金属鉱山株式会社 | How to recover selenium from copper electrolytic slime |
-
1988
- 1988-03-03 JP JP5029988A patent/JPH0784606B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01225707A (en) | 1989-09-08 |
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