JPH01225707A - Production of fine palladium particles - Google Patents
Production of fine palladium particlesInfo
- Publication number
- JPH01225707A JPH01225707A JP5029988A JP5029988A JPH01225707A JP H01225707 A JPH01225707 A JP H01225707A JP 5029988 A JP5029988 A JP 5029988A JP 5029988 A JP5029988 A JP 5029988A JP H01225707 A JPH01225707 A JP H01225707A
- Authority
- JP
- Japan
- Prior art keywords
- palladium
- particle size
- ascorbic acid
- size distribution
- 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.)
- Granted
Links
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000002245 particle Substances 0.000 title abstract description 30
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 26
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 14
- 239000002211 L-ascorbic acid Substances 0.000 claims abstract description 11
- 235000000069 L-ascorbic acid Nutrition 0.000 claims abstract description 11
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 150000000996 L-ascorbic acids Chemical class 0.000 claims description 4
- 239000011859 microparticle Substances 0.000 claims 2
- 238000009826 distribution Methods 0.000 abstract description 13
- 150000000994 L-ascorbates Chemical class 0.000 abstract description 4
- 239000011668 ascorbic acid Substances 0.000 abstract description 3
- 235000010323 ascorbic acid Nutrition 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 15
- 239000010419 fine particle Substances 0.000 description 13
- 239000007864 aqueous solution Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 238000007865 diluting Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000001493 electron microscopy Methods 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 2
- 235000019187 sodium-L-ascorbate Nutrition 0.000 description 2
- 239000011755 sodium-L-ascorbate Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- -1 palladium ions Chemical class 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
Abstract
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。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application 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 its problems) Conventionally, as a method for producing palladium fine particles, a method has been used in which hydrazine is used as a reducing agent and sodium hydroxide is added to an aqueous solution of chloropalladic acid to reduce the solution.
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 the disadvantage that only aggregated palladium particles with a wide particle size distribution can be obtained because the reduced particles are attracted to each other.
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・−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 to solve the above-mentioned drawbacks, and it is an object of the present invention to provide a method for producing fine, dispersed palladium particles with a narrow particle size distribution, in which the particle size can be controlled. .
（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 the Problems) The present invention provides a method for producing palladium fine particles by reducing palladium ions in a palladium ammonium complex solution, by using L-ascorbic acid or L-ascorbic acid salts as a reducing agent. This method is characterized by obtaining monodispersed palladium fine particles.
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ヲ用いる理由は、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。The reason for using L-ascorbic acid or L-ascorbic acid salts in the production method of the present invention is that their redox potential is suitable for reducing the palladium ammonium complex solution, and at the same time, the reason is that L.-ascorbic acid or L-ascorbate salts are used. This is because it works to prevent agglomeration.
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。In addition, in the scope of the present invention, L-ascorbic acid and L-ascorbate salts include sodium salts, potassium salts, ammonium salts, and 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°Ｃより低いと反応が遅く、１００°Ｃを
超えるとパラジウム微粒子が凝集してくるので、１０〜
１００°Ｃの範囲がよ、り好ましい。、
ここで本発明の実施例について説明する。Furthermore, in the present invention, if the pH of the palladium ammonium complex solution is lower than 8, the precipitated particles will aggregate and 13
If the pH is higher, ammonia gas will be generated more and the reaction will be slower, so a range of 8 to 13 is more preferable.If the pH of L-ascorbic acid is lower than 0.5, the reaction will be extremely slow, so 0. More preferably 5 or more. In addition, if the reaction temperature is lower than 10°C, the reaction will be slow, and if it exceeds 100°C, palladium fine particles will aggregate, so
A range of 100°C is even more preferred. , Examples of the present invention will now be described.
（実施例１）
硝酸パラジウム液（ｐ ａ （５０ｇ／ｌ ） １００
ｄを水で希釈して１１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) Palladium nitrate solution (p a (50 g/l) 100
After diluting d with water to make an aqueous solution of 11, 28% aqueous ammonia was added to adjust the pH to 9.
また、Ｌ−アスコルビン酸１００ｇを水に溶解し５００
／ｄ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°
Ｃにし、パラジウムアンモニウム錯体溶液を撹拌しなが
らＬ−アスコルビン酸溶液を添加し、６０分間反応させ
る。In addition, dissolve 100 g of L-ascorbic acid in water and
After making an aqueous solution of /d, 28% aqueous ammonia was added to adjust the pH to 4. Here, set the temperature of these two liquids to 50°
C, add the L-ascorbic acid solution while stirring the palladium ammonium complex solution, and react 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 subjected to particle size distribution measurement and electron microscopy observation.
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 found to be almost spherical, with an average particle size of 0.7 μm and a particle size distribution of 0.5 to 1.0 μm.
It was sharp with a percentage.
（実施例２）
硝酸パラジウム液（Ｐ ｄ （５０ｇ／ Ｅ ） ）
５０ｍ１を水で希釈して１１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) Palladium nitrate solution (P d (50 g/E))
After diluting 50ml with water to make an aqueous solution of 11, 28%
of ammonia water to adjust the pH to 11.
また、Ｌ−アスコルビン酸５０ｇを水に溶解し５００戚
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°Ｃに
し、パラジウムアンモニウム錯体溶液を撹拌しながらＬ
−アスコルビン酸溶液を添加し、３０分間反応させる。In addition, after dissolving 50 g of L-ascorbic acid in water to make a 500 aqueous solution, 28% ammonia water was added to adjust the pH.
=6. Here, the temperature of these two liquids was set to 30°C, and while stirring the palladium ammonium complex solution, L
- Add ascorbic acid solution and allow to react 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 subjected to particle size distribution measurement and electron microscopy observation.
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０．２μｍ１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 almost spherical, with an average particle size of 0.2 μm, and a particle size distribution of 70% between 0.1 and 0.4 μm.
It was a sharp item with a .
（実施例３）
硝酸パラジウム液（Ｐ ｄ （５０ｇ／ ｌ ） ）
１００ ｒｕｓｔを水で希釈して１２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) Palladium nitrate solution (P d (50 g/l))
After diluting 100 rust with water to make an aqueous solution of 12, 28% aqueous ammonia was added to adjust the pH to 10.
また、Ｌ−アスコルビン酸ナトリウム１００ｇヲ１水に
溶解し１ｆｆｉの水溶液にする。ここでこの２液の温度
を７０°Ｃにしパラジウムアンモニウム錯体溶液を撹拌
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。Also, dissolve 100 g of sodium L-ascorbate in 1 water to make 1 ffi aqueous solution. Here, the temperature of these two liquids was set to 70°C, and sodium L-ascorbate was added while stirring the palladium ammonium complex solution.
Let it react for a minute.
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 subjected to particle size distribution measurement and electron microscopy observation.
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 found to be almost spherical, with an average particle size of 1.2 μm, and a particle size distribution of 70% between 1.0 and 1.5 μm.
It was a sharp item with a .
（従来例）
硝酸パラジウム液（Ｐ ｄ （５０ｇ／ ｌ ） ）
１００ ｍｌを水で希釈して１ｊ２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) Palladium nitrate solution (Pd (50g/l))
After diluting 100 ml with water to make an aqueous solution of 1j2,
Add sodium hydroxide to adjust pH=8.
さらにこの液を撹拌しながら８０％の抱水ヒドラジン水
溶液５０ｍｋを添加後、５０°Ｃで２時間撹拌した。Further, while stirring this liquid, 50 mk of an 80% aqueous hydrazine hydrate 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 palladium fine particles were filtered, washed, and subjected to particle size distribution measurement and electron microscope observation.
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０．３〜１０ａｍと幅が広く
、凝集したものであった。As a result, the palladium fine particles were amorphous, had an average particle diameter of 1.8 μm, had a wide particle size distribution of 0.3 to 10 am, and were aggregated.
（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 clear from the above explanation, the production method of the present invention uses L-ascorbic acid or L-ascorbic acid salts as a reducing agent in the method of producing palladium fine particles by reducing a palladium ammonium complex solution. By this,
Since it is possible to produce fine palladium particles with a narrow particle size distribution that is monodisperse, which cannot be obtained using conventional methods, by controlling the particle size, it can be said to be an epoch-making method that can replace conventional production methods.
Claims (1)
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。A method for producing palladium microparticles by reducing a palladium ammonium complex solution, the method comprising obtaining monodispersed palladium microparticles by using L-ascorbic acid or L-ascorbic acid salts as a reducing agent. .
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 true JPH01225707A (en) | 1989-09-08 |
| JPH0784606B2 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) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019131415A (en) * | 2018-01-29 | 2019-08-08 | 住友金属鉱山株式会社 | Method for recovering selenium from copper electrolytic slime |
-
1988
- 1988-03-03 JP JP5029988A patent/JPH0784606B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019131415A (en) * | 2018-01-29 | 2019-08-08 | 住友金属鉱山株式会社 | Method for recovering selenium from copper electrolytic slime |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0784606B2 (en) | 1995-09-13 |
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