JP3545658B2 - Method for producing iridium nitrate solution - Google Patents
Method for producing iridium nitrate solution Download PDFInfo
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- JP3545658B2 JP3545658B2 JP28901999A JP28901999A JP3545658B2 JP 3545658 B2 JP3545658 B2 JP 3545658B2 JP 28901999 A JP28901999 A JP 28901999A JP 28901999 A JP28901999 A JP 28901999A JP 3545658 B2 JP3545658 B2 JP 3545658B2
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- iridium
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- nitrate solution
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Description
【０００１】
【発明の属する技術分野】
本発明は、触媒の原料、あるいはイリジウム化合物合成時の出発物質となる硝酸イリジウム溶液の製造方法に関するものである。
【０００２】
【従来の技術】
従来、硝酸イリジウム溶液を工業的に製造する方法としては、公知の文献がなかった。関連する技術として、次のように硝酸ロジウム溶液を製造する方法が知られている。すなわち、塩化ロジウム溶液にアルカリ性溶液を加えて水酸化ロジウムの沈殿を生成させ、該沈殿を硝酸に溶解して硝酸ロジウム溶液とする方法である。しかし、この方法では、塩化ロジウムから水酸化ロジウムへの転換が不十分なため最終生成物の硝酸ロジウム溶液に不純物がやや多く混在してしまうという問題点が有った。そして、この問題点は、この方法を硝酸イリジウム溶液の製造方法として転用したとしても同様に生じる問題点と考えられる。加えて、塩化イリジウムから水酸化イリジウムへの転換率は、塩化ロジウムから水酸化ロジウムへの転換率をかなり下回ることもわかった。
【０００３】
【発明が解決しようとする課題】
本発明は、上記の状況に鑑み、不純物の極少ない硝酸イリジウム溶液を高い収率で製造するための新規の方法を提供することを目的とする。
【０００４】
【課題を解決するための手段】
本発明者は技術の現状に鑑みて鋭意研究を重ねた結果、３価の塩化イリジウムイオン［ ＩｒＣｌ６］３−は、置換不活性であり、水酸化イリジウムＩｒ（ ＯＨ）３への転換が著しく困難であるのに対し、４価の［ ＩｒＣｌ６］２−は比較的活性であるので、水酸化物への転換が可能である点に着目し、塩化イリジウムを［ ＩｒＣｌ６］２−の形に保つことによって水酸化イリジウムを経由して硝酸イリジウムの合成ができることを見いだし、本発明を完成するに至った。
【０００５】
即ち、本発明は、以下の硝酸イリジウムの製造方法を提供するものである。
本発明は、塩化イリジウム溶液に酸化剤を加える工程と、該溶液にアルカリ性溶液を加えて水酸化イリジウムとする工程と、沈殿を濾別し水洗と濾過をくりかえす工程と、硝酸を加えて加熱して反応させる工程とからなる硝酸イリジウム溶液の製造方法である。
【０００６】
【発明の実施の形態】
塩化イリジウム溶液は、市販されているものを使用することができる。通常市販されている塩化イリジウム溶液は、３価の塩化イリジウムと４価の塩化イリジウムが混在した溶液となっている。本発明の硝酸イリジウムの製造方法では、３価と４価の塩化イリジウムが混在している物を出発物質とできる。
このような塩化イリジウムを酸化し、４価の状態に保つには、塩化イリジウム溶液に酸化剤を加える必要がある。
【０００７】
本発明において、上記の目的に使用される酸化剤としては、塩素ガス又は過酸化水素水が好ましく用いられる。例えば、塩素ガスを酸化剤として使用する場合、塩化イリジウム溶液中に塩素ガスを供給しながら８０〜 １００℃で５時間程度加熱すれば、ほぼ全体が４価の塩化イリジウム溶液となる。
このようにして得られる塩化イリジウム（ＩＶ）溶液に水酸化ナトリウム等のアルカリ性溶液を加え、ｐＨを１１程度に調整して８０℃で加熱すると、水酸化イリジウムの沈殿が得られる。
【０００８】
この沈殿を濾別し、水洗と濾過をくりかえすことにより未反応物や副生成物等の不純物が十分に除去された水酸化イリジウムが得られる。
【０００９】
こうして得られる水酸化イリジウムに硝酸を加え、約９０℃に加熱すると沈殿が溶解し、硝酸イリジウム溶液が得られる。
【００１０】
以上の方法により、不純物の混入が極めて少ない硝酸イリジウム溶液を高い収率で製造することができるものである。
【００１１】
【実施例】
以下、本発明に係わる実施例を記載するが、該実施例は本発明を限定するものではない。
【００１２】
【実施例１】
塩化イリジウム溶液（Ｉｒとして５．２ｇ含有する）に塩素ガスを供給しながら８０〜 １００℃で５時間程度加熱した。次に、この溶液に水酸化ナトリウムを加え、ｐＨを１１に調整し、８０℃で５時間加熱した。得られた沈殿を濾別し、水洗と濾過を５回繰り返して水酸化イリジウム結晶を得た。この洗浄濾過過程で排出された濾液中の塩素濃度は７ｍｇ／ｌ以下であった。この結晶に濃硝酸１１３ｇを加え、９０℃で４時間加熱した。沈殿物を濾過除去して硝酸イリジウム溶液（ Ｉｒとして３．７ｇ含有）を得た。溶液中の塩素濃度は１ｐｐｍ以下であった。
【００１３】
【実施例２】
塩化イリジウム溶液（Ｉｒとして５．１ｇ含有する）に過酸化水素水５０ｍｌを加えてから、８０〜 １００℃で５時間程度加熱した。次に、この溶液に水酸化ナトリウムを加え、ｐＨを１１に調整し、８０℃で５時間加熱した。得られた沈殿を濾別し、水洗と濾過を５回繰り返して水酸化イリジウム結晶を得た。この洗浄濾過過程で排出された濾液中の塩素濃度は２ｍｇ／ｌ以下であった。この結晶に濃硝酸１１０ｇを加え、９０℃で４時間加熱した。沈殿物を濾過除去して硝酸イリジウム溶液（ Ｉｒとして２．７ｇ含有）を得た。溶液中の塩素濃度は１ｐｐｍ以下であった。
【００１４】
実施例１、２のいずれの溶液とも、室温で７週間放置した後も沈殿が発生せず極めて安定性が高かった。
【００１５】
【発明の効果】
以上の説明で明らかなように、本発明の方法によれば、塩素ガス等の酸化剤を用いて塩化イリジウムを酸化し、４価の状態に保つことにより、水酸化物への転換率を上げると共に、濾過洗浄を繰り返すことにより不純物成分を充分除去するため、溶液中の塩素イオン等不純物の少ない安定した硝酸イリジウム溶液が高い収率で製造できる所となる。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for producing an iridium nitrate solution as a starting material for a catalyst or a starting material for the synthesis of an iridium compound.
[0002]
[Prior art]
Conventionally, there is no known literature as a method for industrially producing an iridium nitrate solution. As a related technique, a method for producing a rhodium nitrate solution as described below is known. That is, this is a method in which an alkaline solution is added to a rhodium chloride solution to form a rhodium hydroxide precipitate, and the precipitate is dissolved in nitric acid to obtain a rhodium nitrate solution. However, this method has a problem in that the conversion of rhodium chloride to rhodium hydroxide is inadequate, so that a large amount of impurities are mixed in the final product rhodium nitrate solution. This problem is considered to be a problem that occurs even when this method is diverted as a method for producing an iridium nitrate solution. In addition, the conversion of iridium chloride to iridium hydroxide was found to be significantly lower than the conversion of rhodium chloride to rhodium hydroxide.
[0003]
[Problems to be solved by the invention]
The present invention has been made in view of the above circumstances, and has as its object to provide a novel method for producing an iridium nitrate solution with extremely few impurities in a high yield.
[0004]
[Means for Solving the Problems]
The present inventor has conducted intensive studies in view of the current state of the art. As a result, trivalent iridium chloride ion [IrCl 6 ] 3- is substituted and inactive, and conversion to iridium hydroxide Ir (OH) 3 is remarkable. While it is difficult, tetravalent [IrCl 6 ] 2- is relatively active, and can be converted to a hydroxide. By focusing on the fact that iridium chloride is converted into [IrCl 6 ] 2- It has been found that by maintaining iridium hydroxide, iridium nitrate can be synthesized via iridium hydroxide, and the present invention has been completed.
[0005]
That is, the present invention provides the following method for producing iridium nitrate.
The present invention provides a step of adding an oxidizing agent to an iridium chloride solution, a step of adding an alkaline solution to the solution to form iridium hydroxide, a step of filtering the precipitate, repeating washing and filtration, and adding nitric acid and heating. And reacting the iridium nitrate solution.
[0006]
BEST MODE FOR CARRYING OUT THE INVENTION
A commercially available iridium chloride solution can be used. A commercially available iridium chloride solution is a mixed solution of trivalent iridium chloride and tetravalent iridium chloride. In the method for producing iridium nitrate of the present invention, a mixture of trivalent and tetravalent iridium chloride can be used as a starting material.
In order to oxidize such iridium chloride and keep it in a tetravalent state, it is necessary to add an oxidizing agent to the iridium chloride solution.
[0007]
In the present invention, as the oxidizing agent used for the above purpose, chlorine gas or aqueous hydrogen peroxide is preferably used. For example, when chlorine gas is used as the oxidizing agent, if the iridium chloride solution is heated at 80 to 100 ° C. for about 5 hours while supplying the chlorine gas, almost the whole becomes a tetravalent iridium chloride solution.
An alkaline solution such as sodium hydroxide is added to the iridium (IV) chloride solution thus obtained, the pH is adjusted to about 11, and the mixture is heated at 80 ° C., whereby a precipitate of iridium hydroxide is obtained.
[0008]
The precipitate is separated by filtration, and iridium hydroxide from which impurities such as unreacted substances and by-products are sufficiently removed can be obtained by repeating washing with water and filtration.
[0009]
When nitric acid is added to the iridium hydroxide thus obtained and heated to about 90 ° C., the precipitate is dissolved, and an iridium nitrate solution is obtained.
[0010]
According to the above-mentioned method, an iridium nitrate solution containing extremely few impurities can be produced at a high yield.
[0011]
【Example】
Hereinafter, examples according to the present invention will be described, but the examples do not limit the present invention.
[0012]
Embodiment 1
The iridium chloride solution (containing 5.2 g as Ir) was heated at 80 to 100 ° C. for about 5 hours while supplying chlorine gas. Next, sodium hydroxide was added to the solution to adjust the pH to 11, and the solution was heated at 80 ° C for 5 hours. The obtained precipitate was separated by filtration, and washing with water and filtration were repeated 5 times to obtain iridium hydroxide crystals. The concentration of chlorine in the filtrate discharged in the washing and filtering process was 7 mg / l or less. 113 g of concentrated nitric acid was added to the crystals and heated at 90 ° C. for 4 hours. The precipitate was removed by filtration to obtain an iridium nitrate solution (containing 3.7 g as Ir). The chlorine concentration in the solution was 1 ppm or less.
[0013]
Embodiment 2
After adding 50 ml of hydrogen peroxide solution to the iridium chloride solution (containing 5.1 g as Ir), the mixture was heated at 80 to 100 ° C for about 5 hours. Next, sodium hydroxide was added to the solution to adjust the pH to 11, and the solution was heated at 80 ° C for 5 hours. The obtained precipitate was separated by filtration, and washing with water and filtration were repeated 5 times to obtain iridium hydroxide crystals. The concentration of chlorine in the filtrate discharged in the washing and filtering process was 2 mg / l or less. 110 g of concentrated nitric acid was added to the crystals and heated at 90 ° C. for 4 hours. The precipitate was removed by filtration to obtain an iridium nitrate solution (containing 2.7 g as Ir). The chlorine concentration in the solution was 1 ppm or less.
[0014]
Both the solutions of Examples 1 and 2 did not precipitate even after standing at room temperature for 7 weeks, and had extremely high stability.
[0015]
【The invention's effect】
As is apparent from the above description, according to the method of the present invention, iridium chloride is oxidized using an oxidizing agent such as chlorine gas, and is maintained in a tetravalent state, thereby increasing the conversion rate to hydroxide. At the same time, since the impurity component is sufficiently removed by repeating the filtration and washing, a stable iridium nitrate solution with a small amount of impurities such as chloride ions in the solution can be produced at a high yield.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28901999A JP3545658B2 (en) | 1999-10-12 | 1999-10-12 | Method for producing iridium nitrate solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28901999A JP3545658B2 (en) | 1999-10-12 | 1999-10-12 | Method for producing iridium nitrate solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2001106536A JP2001106536A (en) | 2001-04-17 |
| JP3545658B2 true JP3545658B2 (en) | 2004-07-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28901999A Expired - Fee Related JP3545658B2 (en) | 1999-10-12 | 1999-10-12 | Method for producing iridium nitrate solution |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2419517C2 (en) * | 2009-07-20 | 2011-05-27 | Открытое акционерное общество "Производственное объединение Электрохимический завод" (ОАО "ПО ЭХЗ") | Method of producing of metal iridium powder from (trifluorophosphine) iridium hydride tetrakis |
| JP6651168B2 (en) | 2016-01-14 | 2020-02-19 | 国立研究開発法人産業技術総合研究所 | Method for producing cyclometallated iridium complex |
| CN114506881B (en) * | 2022-03-18 | 2023-03-31 | 昆明理工大学 | Preparation method of iridium tetraiodide |
| CN114920641A (en) * | 2022-06-28 | 2022-08-19 | 浙江微通催化新材料有限公司 | Iridium precipitate, preparation method thereof and preparation method of iridium acetate |
| CN116177626A (en) * | 2023-02-17 | 2023-05-30 | 派瑞科技有限公司 | Method for preparing iridium nitrate solution |
| GB202318315D0 (en) * | 2023-11-30 | 2024-01-17 | Johnson Matthey Plc | Method of treating an iridium containing effluent stream |
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1999
- 1999-10-12 JP JP28901999A patent/JP3545658B2/en not_active Expired - Fee Related
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| JP2001106536A (en) | 2001-04-17 |
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