JP2591787B2 - Method for producing ruthenium oxide fine particles - Google Patents
Method for producing ruthenium oxide fine particlesInfo
- Publication number
- JP2591787B2 JP2591787B2 JP63099117A JP9911788A JP2591787B2 JP 2591787 B2 JP2591787 B2 JP 2591787B2 JP 63099117 A JP63099117 A JP 63099117A JP 9911788 A JP9911788 A JP 9911788A JP 2591787 B2 JP2591787 B2 JP 2591787B2
- Authority
- JP
- Japan
- Prior art keywords
- ruthenium
- fine particles
- ruthenium oxide
- oxide fine
- inert gas
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/004—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は微細な酸化ルテニウム粒子の製造方法に関す
るものである。The present invention relates to a method for producing fine ruthenium oxide particles.
（従来技術とその問題点） 従来、酸化ルテニ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ルテニウム酸水溶液に
水酸化ナトリウムを加えて還元し、さらに酸化性ガス雰
囲気中で熱処理する方法が用いられてきた。(Prior art and its problems) Conventionally, as a method for producing ruthenium oxide fine particles, a method in which hydrazine is used as a reducing agent, sodium hydroxide is added to an aqueous solution of ruthenium chloride to reduce the solution, and a heat treatment is performed in an oxidizing gas atmosphere. Has been used.
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酸化ルテニウム微
粒子しか得られないという欠点を有していた。However, this method has a drawback that only fine particles of ruthenium oxide having a wide particle size distribution can be obtained in which the precipitated fine particles attract and aggregate together.
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球状の酸化ルテニ
ウム微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 in order to solve the above-mentioned drawbacks, and has as its object to provide a method for producing spherical ruthenium oxide fine particles having a narrow dispersed particle size distribution.
（問題点を解決するための手段） 本発明は、塩化ルテニウム酸水溶液を加熱して水素、
塩素、酸素及びルテニウムから成るルテニウム化合物粒
子を合成しこれを熱分解して酸化ルテニウム微粒子を製
造する方法において、塩化ルテニウム酸水溶液を圧力５
〜30kg/cm2の不活性ガス雰囲気中で100〜200℃に加熱し
て前記ルテニウム化合物微粒子を合成し、このルテニウ
ム化合物微粒子を200〜1000℃の不活性ガス雰囲気中で
熱分解することを特徴とするものである。(Means for Solving the Problems) The present invention heats an aqueous ruthenic chloride solution to produce hydrogen,
In a method for producing ruthenium compound particles composed of chlorine, oxygen and ruthenium and thermally decomposing them to produce ruthenium oxide fine particles, a ruthenium chloric acid aqueous solution is subjected to a pressure of 5%.
The method is characterized in that the ruthenium compound fine particles are synthesized by heating to 100 to 200 ° C. in an inert gas atmosphere of up to 30 kg / cm 2 , and the ruthenium compound fine particles are thermally decomposed in an inert gas atmosphere of 200 to 1000 ° C. It is assumed that.
而して本発明の製造方法において塩化ルテニウム酸水
溶液を高圧の不活性ガス雰囲気中で加熱する理由は、水
溶液の蒸発を抑えると共に加熱温度、圧力をコントロー
ルすることによりルテニウム化合物微粒子の合成速度を
コントロールし、合成（析出）したルテニウム化合物微
粒子の成長を助け、分散した、粒度分布の幅の狭いルテ
ニウム化合物微粒子を合成させるためであり加熱温度を
100〜200℃、不活性ガスの圧力を５〜30kg/cm2に限定す
る理由は100℃、5kg/cm2よりも低いと析出速度が遅く、
200℃、30kg/cm2よりも高いと析出した微粒子同士の凝
集が起こってくるためである。In the production method of the present invention, the reason for heating the ruthenic acid chloride aqueous solution in a high-pressure inert gas atmosphere is to control the synthesis rate of the ruthenium compound fine particles by suppressing the evaporation of the aqueous solution and controlling the heating temperature and pressure. The heating temperature is set to assist the growth of the synthesized (precipitated) ruthenium compound fine particles and to synthesize dispersed ruthenium compound fine particles having a narrow particle size distribution.
100 to 200 ° C., the reason to limit the pressure of the inert gas to 5~30kg / cm 2 is 100 ° C., slow lower the deposition rate than 5 kg / cm 2,
If the temperature is higher than 200 ° C. and 30 kg / cm 2 , aggregation of the precipitated fine particles occurs.
また不活性ガス雰囲気中で熱分解する温度を200〜100
0℃に限定する理由は、200℃よりも低いと分解が遅く、
1000℃よりも高いと焼結が進行するためである。In addition, the temperature for thermal decomposition in an inert gas atmosphere is set to 200 to 100
The reason for limiting to 0 ° C is that if it is lower than 200 ° C, the decomposition is slow,
If the temperature is higher than 1000 ° C., sintering proceeds.
本発明において用いる不活性ガスとしては窒素、アル
ゴン、ヘリウムなどである。Examples of the inert gas used in the present invention include nitrogen, argon, and helium.
ここで本発明の実施例について説明する。 Here, an embodiment of the present invention will be described.
（実施例１） ルテニウム含有量7g/lの塩化ルテニウム酸水溶液（H2
RuCl6）を圧力容器オートクレーブに装入し、これを攪
拌しながら窒素ガス15kg/cm2の圧力下で130℃に昇温し
て、30分間合成反応を行わせたところ灰白色のＨ、Cl、
ＯおよびRuから成るルテニウム化合物微粒子の沈澱物が
生成した。得られた沈澱物はろ過後、充分に水で洗浄乾
燥した後、800℃のアルゴン雰囲気中で１時間熱処理し
て粒度分布測定、電子顕微鏡観察及びＸ線回折を行っ
た。(Example 1) Ruthenium chloride aqueous solution (H 2 ) having a ruthenium content of 7 g / l
RuCl 6 ) was charged into a pressure vessel autoclave, and the mixture was heated to 130 ° C. under a pressure of 15 kg / cm 2 of nitrogen gas with stirring to carry out a synthesis reaction for 30 minutes.
A precipitate of ruthenium compound fine particles consisting of O and Ru was formed. The obtained precipitate was filtered, washed sufficiently with water and dried, and then heat-treated in an argon atmosphere at 800 ° C. for 1 hour, and subjected to particle size distribution measurement, observation with an electron microscope, and X-ray diffraction.
その結果、この酸化ルテニウム微粒子は平均粒径0.6
μｍで、粒度分布は0.4〜0.8μｍに70％が入る幅の狭い
もので、球状に分散したものであった。As a result, the ruthenium oxide fine particles had an average particle size of 0.6.
μm, the particle size distribution was narrow with a width of 70% within 0.4 to 0.8 μm, and the particles were dispersed spherically.
（実施例２） ルテニウム含有量の20g/lの塩化ルテニウム酸水溶液
（H2RuCl6）を圧力容器オートクレーブを装入し、これ
を攪拌しながら窒素ガスを25kg/cm2の圧力下で180℃に
昇温して、60分間合成反応を行なわせたところ灰白色の
Ｈ、Cl、Ｏ及びRuから成るルテニウム化合物微粒子の沈
澱物が生成した。得られた沈澱物はろ過後、充分に水で
洗浄乾燥した後、500℃のアルゴン雰囲気中で１時間熱
処理して粒度分布測定、電子顕微鏡観察及びＸ線回折を
行った。Example 2 A pressure vessel autoclave was charged with an aqueous ruthenium chloride solution (H 2 RuCl 6 ) having a ruthenium content of 20 g / l, and nitrogen gas was supplied at 180 ° C. under a pressure of 25 kg / cm 2 while stirring. When the temperature was raised to 60 ° C. and the synthesis reaction was carried out for 60 minutes, an off-white precipitate of ruthenium compound fine particles composed of H, Cl, O and Ru was formed. The obtained precipitate was filtered, sufficiently washed with water and dried, and then heat-treated in an argon atmosphere at 500 ° C. for 1 hour, and subjected to particle size distribution measurement, observation with an electron microscope, and X-ray diffraction.
その結果、この酸化ルテニウム微粒子は平均粒径0.9
μｍで、粒度分布は0.7〜1.1μｍに70％が入る幅の狭い
もので、球状で分散したものであった。As a result, the ruthenium oxide fine particles had an average particle size of 0.9.
μm, the particle size distribution was narrow with a width of 70% within 0.7 to 1.1 μm, and spherical and dispersed.
（従来例） ルテニウム含有量10g/lの塩化ルテニウム酸水溶液（H
2RuCl6）をビーカー中で攪拌しながら水酸化ナトリウム
を添加し、さらにこの溶液に塩酸ヒドラジン（N2H4・2H
Cl）を徐々に添加したところ灰白色の沈澱物が生成し
た。得られたルテニウム粒子はろ過後、充分に水で洗浄
乾燥した後、500℃の酸素雰囲気中で１時間熱処理して
粒度分布測定、電子顕微鏡観察及びＸ線回折を行った。(Conventional example) Ruthenium chloride aqueous solution (H
2 RuCl 6 ) was stirred in a beaker, sodium hydroxide was added, and hydrazine hydrochloride (N 2 H 4 .2H) was added to the solution.
Cl) was slowly added to produce an off-white precipitate. The obtained ruthenium particles were filtered, thoroughly washed with water and dried, and then heat-treated for 1 hour in an oxygen atmosphere at 500 ° C., and subjected to particle size distribution measurement, observation with an electron microscope, and X-ray diffraction.
その結果、この酸化ルテニウム粒子は平均粒径8.5μ
ｍで、粒度分布は0.5〜15μｍで幅の広い凝集したもの
であった。As a result, the ruthenium oxide particles had an average particle size of 8.5 μm.
m, the particle size distribution was 0.5 to 15 μm and broad agglomerates.
（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
ルテニウム酸水溶液を加熱して水素、塩素、酸素及びル
テニウムから成るルテニウム化合物粒子を合成し、これ
を熱分解して酸化ルテニウム微粒子を製造する方法にお
いて、塩化ルテニウム酸水溶液を圧力５〜30kg/cm2の不
活性ガス雰囲気中で100〜200℃に加熱して前記ルテニウ
ム化合物微粒子を合成し、このルテニウム化合物微粒子
を200〜1000℃の不活性ガス雰囲気中で熱分解すること
により，、従来法では得られなかった分散した、粒度分
布の幅の狭い球状の微細な酸化ルテニウム微粒子を製造
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 description, the production method of the present invention synthesizes ruthenium compound particles composed of hydrogen, chlorine, oxygen and ruthenium by heating an aqueous ruthenic acid solution, and thermally decomposes them to oxidize them. In the method for producing ruthenium microparticles, the ruthenium compound microparticles are synthesized by heating the ruthenium chloric acid aqueous solution to 100 to 200 ° C. in an inert gas atmosphere at a pressure of 5 to 30 kg / cm 2 , and the ruthenium compound microparticles are heated to 200 to 200 ° C. Thermal decomposition in an inert gas atmosphere at 1000 ° C enables the production of dispersed, fine-grained ruthenium oxide particles with a narrow particle size distribution that could not be obtained by the conventional method. It can be said to be an epoch-making thing.
Claims (1)
塩素、酸素及びルテニウムから成るルテニウム化合物微
粒子を合成し、これを熱分解して酸化ルテニウム微粒子
を作りこれを熱分解して酸化ルテニウム微粒子を製造す
る方法において、塩化ルテニウム酸水溶液を圧力５〜30
kg/cm2の不活性ガス雰囲気中で100〜200℃に加熱して前
期ルテニウム化合物微粒子を合成し、このルテニウム化
合物微粒子を200〜1000℃の不活性ガス雰囲気中で熱分
解することを特徴とする酸化ルテニウム微粒子の製造方
法。1. An aqueous ruthenic chloride solution is heated to form hydrogen,
In a method of synthesizing ruthenium compound fine particles composed of chlorine, oxygen and ruthenium, pyrolyzing them to form ruthenium oxide fine particles, and thermally decomposing them to produce ruthenium oxide fine particles, a ruthenium chloride aqueous solution is subjected to a pressure of 5 to 30.
The method is characterized in that the ruthenium compound fine particles are synthesized by heating to 100 to 200 ° C. in an inert gas atmosphere of kg / cm 2 , and the ruthenium compound fine particles are thermally decomposed in an inert gas atmosphere of 200 to 1000 ° C. Of producing fine ruthenium oxide particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63099117A JP2591787B2 (en) | 1988-04-21 | 1988-04-21 | Method for producing ruthenium oxide fine particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63099117A JP2591787B2 (en) | 1988-04-21 | 1988-04-21 | Method for producing ruthenium oxide fine particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01270521A JPH01270521A (en) | 1989-10-27 |
| JP2591787B2 true JP2591787B2 (en) | 1997-03-19 |
Family
ID=14238851
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63099117A Expired - Lifetime JP2591787B2 (en) | 1988-04-21 | 1988-04-21 | Method for producing ruthenium oxide fine particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2591787B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574097B (en) * | 2019-02-01 | 2021-11-16 | 江苏欣诺科催化剂有限公司 | Preparation method of trichloro-hexa-amino ruthenium |
-
1988
- 1988-04-21 JP JP63099117A patent/JP2591787B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01270521A (en) | 1989-10-27 |
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