JPH02159306A - Production of fine platinum particles - Google Patents
Production of fine platinum particlesInfo
- Publication number
- JPH02159306A JPH02159306A JP31251888A JP31251888A JPH02159306A JP H02159306 A JPH02159306 A JP H02159306A JP 31251888 A JP31251888 A JP 31251888A JP 31251888 A JP31251888 A JP 31251888A JP H02159306 A JPH02159306 A JP H02159306A
- Authority
- JP
- Japan
- Prior art keywords
- soln
- particles
- chloroplatinic acid
- particle size
- platinum 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.)
- Pending
Links
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000002245 particle Substances 0.000 title claims abstract description 27
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000002253 acid Substances 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 239000010419 fine particle Substances 0.000 claims description 9
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 230000000717 retained effect Effects 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 8
- 239000002244 precipitate Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- BIVUUOPIAYRCAP-UHFFFAOYSA-N aminoazanium;chloride Chemical compound Cl.NN BIVUUOPIAYRCAP-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は微細な白金微粒子の製造する方法に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention relates to a method for producing fine platinum particles.
（従来技術とその問題点）
従来、白金微粒子の製造方法としては還元性ガスとして
Ｈ２やＣＯ等を用いて塩化白金酸塩酸酸性水溶液を還元
する方法が用いられてきた。(Prior art and its problems) Conventionally, as a method for producing platinum fine particles, a method has been used in which a chloroplatinate acid aqueous solution is reduced using H2, CO, or the like as a reducing gas.
ところが、この方法では析出した微粒子同士が引き寄せ
合って凝集した粒度分布の幅の広い白金微粒子しか得ら
れないという欠点を有していた。However, this method has the drawback that only fine platinum particles with a wide particle size distribution, which are formed by attracting and agglomerating the precipitated fine particles together, can be obtained.
本発明者は走査電子顕微鏡などを用いてこの原因を種々
検討したところ、この凝集作用が液のｐＨとＰｔ濃度に
依存することを発見した。The present inventor conducted various studies on the causes of this using a scanning electron microscope and discovered that this aggregation effect depends on the pH and Pt concentration of the liquid.
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、ポーラスな分散した粒度分布の幅の狭い白金粒子
の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 aims to provide a method for producing platinum particles that are porous and dispersed and have a narrow particle size distribution.
（問題点を解決するための手段）
本発明は塩化白金酸水溶液を還元して白金微粒子を製造
する方法において塩化白金酸水溶液を常温常圧にて還元
性ガスを導入して還元することにより白金微粒子を生成
する際に、Ｐｔ濃度を２０ｇ／ｉ以下かつ溶液濃度を酸
性に保ちポーラスな分散した粒度分布の幅の狭い粒子を
生成させることを特徴とするものである。(Means for Solving the Problems) The present invention is a method for producing platinum fine particles by reducing an aqueous solution of chloroplatinic acid. When producing fine particles, the Pt concentration is kept at 20 g/i or less and the solution concentration is kept acidic to produce porous, dispersed particles with a narrow particle size distribution.
而して本発明の製造方法において塩化白金酸水溶液を、
酸性側にもってくるのは、ＨｉＰｔｌ！ｓの還元時に発
生する遊離のＣＩ−の発生速度を残存しているＣｌ１−
により遅らせ、還元反応をゆっくり起こしポーラスな粒
子を生成させるためである。Therefore, in the production method of the present invention, the chloroplatinic acid aqueous solution is
What comes to the acidic side is HiPtl! The rate of generation of free CI- generated during the reduction of s is
This is to slow down the reduction reaction and generate porous particles.
また、Ｐｔ濃度を２０ｇ／ｌ以下にするのは、濃度を薄
くすることで析出Ｐｔ粒子相互間の結合力が弱まり、凝
集作用が遅くなるためである。Furthermore, the reason why the Pt concentration is set to 20 g/l or less is that by reducing the concentration, the bonding force between the precipitated Pt particles becomes weaker, and the agglomeration effect becomes slower.
なお、この酸性側にもってくる操作とＰｔ濃度を薄くす
る操作は同時に行わなければならない。Note that the operation of bringing the acidity level and the operation of reducing the Pt concentration must be performed at the same time.
いずれか一方のみでは走査電子顕微鏡で観察した結果析
出Ｐｔ粒子の凝集がみられた。When only one of them was used, agglomeration of the precipitated Pt particles was observed as a result of observation using a scanning electron microscope.
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）
白金含有量０．８ｇ／ｌをの塩化白金酸水溶液をＨＣｊ
２″ＱｐＨを１．５に調整してガラス容器に装入しこれ
を常温、常圧で撹拌しながら水素ガスでバブリングして
１０分分間光反応を行わせたところ、灰白色の沈殿が生
成した。得られた白金粒子は濾過後、充分に水で洗浄し
乾燥した後、電子顕微鏡観察を行った。(Example 1) A chloroplatinic acid aqueous solution with a platinum content of 0.8 g/l was HCj
The 2″Q pH was adjusted to 1.5 and charged into a glass container, and the mixture was stirred and bubbled with hydrogen gas at room temperature and pressure to carry out a photoreaction for 10 minutes, and a grayish white precipitate was formed. The obtained platinum particles were filtered, thoroughly washed with water, dried, and then observed with an electron microscope.
その結果この白金粒子は平均粒径５．０μｍのポーラス
で分散したものであった。As a result, the platinum particles were porous and dispersed with an average particle size of 5.0 μm.
（実施例２）
白金含有量１．０ｇ／ｌの塩化白金酸水溶液をＨＣＩで
ｐＨを４，０に調整してガラス容器に装入し、これを常
温常圧で撹拌しながら水素ガスでバブリングして１５分
分間光反応を行わせたところ、灰白色の沈殿が生成した
。得られた白金微粒子は濾過後、充分に水で洗浄し乾燥
した後、電子顕微鏡観察を行った。(Example 2) A chloroplatinic acid aqueous solution with a platinum content of 1.0 g/l was adjusted to pH 4.0 with HCI, charged into a glass container, and bubbled with hydrogen gas while stirring at room temperature and pressure. When the photoreaction was carried out for 15 minutes, a grayish white precipitate was formed. The obtained platinum fine particles were filtered, thoroughly washed with water, dried, and then observed with an electron microscope.
その結果この白金微粒子は平均粒径３．０μｍのポーラ
スで分散したものであった。As a result, the platinum fine particles were porous and dispersed with an average particle size of 3.0 μm.
（従来例１）
白金含有量１０ｇ／ｌの塩化白金酸アンモニウム水溶液
をビーカー中で撹拌しなからＮａＯＨを添加し、さらに
この溶液に塩酸ヒドラジン（Ｎ２Ｈ。(Conventional Example 1) An aqueous solution of ammonium chloroplatinate having a platinum content of 10 g/l was stirred in a beaker, then NaOH was added, and hydrazine hydrochloride (N2H) was added to this solution.
・２Ｈ（１）を徐々に添加したところ灰白色の沈殿物が
生成した。得られた白金粒子は濾過後、充分に水で洗浄
し乾燥した後、粒度分布測定及び電子顕微鏡観察を行っ
た。- When 2H(1) was gradually added, a grayish white precipitate was formed. The obtained platinum particles were filtered, thoroughly washed with water, dried, and then subjected to particle size distribution measurement and electron microscope observation.
その結果、この白金粒子は平均粒径６．２０μｍで粒度
分布の幅の広い凝集したものであった。As a result, the platinum particles were agglomerated with an average particle size of 6.20 μm and a wide particle size distribution.
（従来例２）
白金含有量５０ｇ／ｌの高濃度な塩化白金酸水溶液をｐ
Ｈを３及び１２に調整してガラス容器に装入し、これを
常温、常圧で撹拌しながら、水素ガスでバブリングして
３０分間還元反応を行わせたところ、反応は進行せず、
沈殿は生成しなかった。(Conventional Example 2) A highly concentrated chloroplatinic acid aqueous solution with a platinum content of 50 g/l was
H was adjusted to 3 and 12 and charged into a glass container, and while stirring at room temperature and normal pressure, hydrogen gas was bubbled to carry out the reduction reaction for 30 minutes, but the reaction did not proceed.
No precipitate formed.
（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、塩化
白金酸水溶液を還元して白金微粒子を製造する方法にお
いて、塩化白金酸水溶液を常温常圧で還元性ガスを導入
して還元する際にｐｔｍ度を２０ｇ／Ｉ！以下かつ溶液
ｐＨを酸性に保つことにより、従来法では得られなかっ
た分散した粒度分布の幅の狭いポーラスな微細な白金微
粒子を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 is a method for producing platinum fine particles by reducing a chloroplatinic acid aqueous solution, in which a reducing gas is introduced into the chloroplatinic acid aqueous solution at room temperature and normal pressure. When reducing it, the PTM degree is 20g/I! By keeping the pH of the solution below acidic, it is possible to produce fine, porous platinum particles with a narrow dispersed particle size distribution that could not be obtained using conventional methods, making it an epoch-making product that can replace conventional manufacturing methods. I can say that.
出願人 田中貴金属工業株式会社Applicant: Tanaka Kikinzoku Kogyo Co., Ltd.
Claims (1)
して還元することにより白金微粒子を製造する方法にお
いて、Ｐｔ濃度を２０ｇ／ｌ（０．１モル）以下かつ溶
液ｐＨを酸性に保ち粒子を生成させることを特徴とする
白金微粒子の製造方法。1. In a method for producing platinum fine particles by introducing a reducing gas into a chloroplatinic acid aqueous solution at room temperature and normal pressure to reduce it, the Pt concentration is set to 20 g/l (0.1 mol) or less and the solution pH is made acidic. A method for producing platinum fine particles, characterized by producing retained particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31251888A JPH02159306A (en) | 1988-12-09 | 1988-12-09 | Production of fine platinum particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31251888A JPH02159306A (en) | 1988-12-09 | 1988-12-09 | Production of fine platinum particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02159306A true JPH02159306A (en) | 1990-06-19 |
Family
ID=18030190
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31251888A Pending JPH02159306A (en) | 1988-12-09 | 1988-12-09 | Production of fine platinum particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02159306A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS514692A (en) * | 1974-07-03 | 1976-01-14 | Toyoda Machine Works Ltd | CHOSHIAGE KAKOHOHO |
| JPS544692A (en) * | 1977-06-03 | 1979-01-13 | Grace W R & Co | Device for separating sheet from continuous strip |
-
1988
- 1988-12-09 JP JP31251888A patent/JPH02159306A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS514692A (en) * | 1974-07-03 | 1976-01-14 | Toyoda Machine Works Ltd | CHOSHIAGE KAKOHOHO |
| JPS544692A (en) * | 1977-06-03 | 1979-01-13 | Grace W R & Co | Device for separating sheet from continuous strip |
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