JPH02116634A - Preparation of chloroiridic acid - Google Patents
Preparation of chloroiridic acidInfo
- Publication number
- JPH02116634A JPH02116634A JP27056788A JP27056788A JPH02116634A JP H02116634 A JPH02116634 A JP H02116634A JP 27056788 A JP27056788 A JP 27056788A JP 27056788 A JP27056788 A JP 27056788A JP H02116634 A JPH02116634 A JP H02116634A
- Authority
- JP
- Japan
- Prior art keywords
- hydrochloric acid
- acid
- chloroiridic
- iridium
- heating
- 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
- 239000002253 acid Substances 0.000 title claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 64
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000007664 blowing Methods 0.000 claims abstract description 6
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 24
- 229910052741 iridium Inorganic materials 0.000 claims description 17
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 abstract description 6
- 229910052801 chlorine Inorganic materials 0.000 abstract description 6
- -1 Na3IrCl6 Chemical class 0.000 abstract description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 4
- 239000000725 suspension Substances 0.000 abstract description 4
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 abstract description 2
- 229910001626 barium chloride Inorganic materials 0.000 abstract description 2
- 238000005342 ion exchange Methods 0.000 abstract description 2
- 239000011780 sodium chloride Substances 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000007800 oxidant agent Substances 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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
- C01G55/005—Halides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、イリジウムを塩酸に溶解して塩化イリジウム
酸を製造する方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing chloroiridic acid by dissolving iridium in hydrochloric acid.
（従来技術とその問題点）
従来から塩化イリジウム酸（Ｌ［ｒＣｌｓ）はイリジウ
ム粉末と塩化ナトリウム又は塩化バリウムとを混合し塩
素雰囲気中で加熱してＮａ３１ｒＣ１６等の可溶性塩に
転換し、これを水で抽出して塩化イリジウム酸塩の溶液
を得るようにしている。しかし該溶液中にはナトリウム
やバリウムが含まれているため、純粋な塩化イリジウム
酸を得るためには、イオン交換等を用いてＮａ”やＨａ
２ ＋を除去する必要があり、又可溶性の塩となる率
が小さく、歩留りが悪いという欠点がある。(Prior art and its problems) Chloroiridic acid (L[rCls) has traditionally been produced by mixing iridium powder with sodium chloride or barium chloride and heating it in a chlorine atmosphere to convert it into a soluble salt such as Na31rC16. to obtain a solution of iridium chloride. However, since this solution contains sodium and barium, in order to obtain pure chloroiridic acid, it is necessary to use ion exchange etc.
2 + must be removed, and the rate of conversion to soluble salts is low, resulting in poor yield.
又この他にもイリジウム粉末と塩素を反応させ塩化イリ
ジウムを生成させる研究が広く行われているが、いずれ
も２５０℃以上の高温を必要とするため、塩化イリジウ
ム酸製造の一工程として採用するには装置の耐熱性等に
関するコストが嵩み、経済的ではなくなるという欠点が
ある。In addition to this, research has been widely conducted to generate iridium chloride by reacting iridium powder with chlorine, but since both require high temperatures of 250°C or higher, it is difficult to adopt this method as a step in the production of chloroiridic acid. However, the disadvantage is that the cost associated with the heat resistance of the device increases, making it uneconomical.
更に、微細なイリジウムブラックは濃塩酸と煮沸するこ
とにより極く僅か溶解して塩化イリジウム酸を与えるが
、溶解量が不十分で経済的な操業を行うにはほど遠い。Furthermore, when fine iridium black is boiled with concentrated hydrochloric acid, it dissolves in a very small amount to give chloroiridic acid, but the dissolved amount is insufficient and is far from economical to operate.
この他に、活性アルミナ等の無機多孔質担体に担持され
た白金族金属を塩酸及び酸化剤を使用して抽出する方法
が知られている（特公昭６１−１、６３２６号）が、担
持された金属であるため単一操作では回収率が上昇せず
、塩酸及び酸化剤による抽出の後に更に塩酸による洗浄
工程を設けて回収率を上げるようにしている。この方法
により満足できる回収率を達成することができるが、作
業性向上のためには工程数を減らすことが望ましく、又
この方法をそのまま塩化イリジウム酸の製造に適用する
ことはできない。In addition, a method is known in which platinum group metals supported on an inorganic porous carrier such as activated alumina are extracted using hydrochloric acid and an oxidizing agent (Japanese Patent Publication No. 6326, 1983). Since the metal is a metal, the recovery rate cannot be increased by a single operation, and after extraction with hydrochloric acid and an oxidizing agent, a washing step with hydrochloric acid is further provided to increase the recovery rate. Although a satisfactory recovery rate can be achieved by this method, it is desirable to reduce the number of steps in order to improve workability, and this method cannot be directly applied to the production of chloroiridic acid.
（発明の目的）
本発明の目的は、比較的簡単な模作でほぼ定量的にイリ
ジウムを塩酸に溶解して塩化イリジウム酸を製造するこ
とのできる方法を提供することである。(Objective of the Invention) An object of the present invention is to provide a method capable of producing chloroiridic acid by dissolving iridium in hydrochloric acid almost quantitatively with a relatively simple imitation.
（問題点を解決するための手段）
本発明は、イリジウム、又はイリジウムを含む混合物を
濃塩酸中で加熱して懸濁させながら塩素ガスを吹き込ん
で溶解し、塩化イリジウム酸を製造することから成る塩
化イリジウム酸の製造方法である。(Means for Solving the Problems) The present invention comprises heating and suspending iridium or a mixture containing iridium in concentrated hydrochloric acid and dissolving it by blowing in chlorine gas to produce chloroiridic acid. This is a method for producing chloroiridic acid.
以下本発明の詳細な説明する。The present invention will be explained in detail below.
本発明におけるイリジウムとは、イリジウム粉末、イリ
ジウムブラック等の純粋な単体の他、例えば少量の他の
白金族金属と合金を形成しているイリジウム等も含まれ
る。又イリジウムを含む混合物とは、特にイリジウム回
収物等性の用途で使用されたイリジウムを含む混合物を
いう。Iridium in the present invention includes not only pure elements such as iridium powder and iridium black, but also iridium formed in an alloy with a small amount of other platinum group metals. Further, the mixture containing iridium refers to a mixture containing iridium used particularly for purposes such as recovered iridium.
又使用する塩酸の濃度は１２規定以上とすることが好ま
しく、１２規定未満とすると溶解に時間が掛かり過ぎる
からである。Further, the concentration of the hydrochloric acid used is preferably 12N or more, because if it is less than 12N, it will take too much time for dissolution.
本発明では、この塩酸溶液中で前記イリジウム又はその
混合物を撹拌して懸濁状態とする。この懸濁によりイリ
ジウムが塩酸溶液中に十分分散して塩酸及び後述する塩
素ガスと十分接触して反応性が向上することになる。In the present invention, the iridium or the mixture thereof is stirred in this hydrochloric acid solution to form a suspension. Through this suspension, iridium is sufficiently dispersed in the hydrochloric acid solution and brought into sufficient contact with hydrochloric acid and chlorine gas, which will be described later, to improve reactivity.
次いで撹拌し懸濁状態を維持しながら該塩酸溶液を加熱
して更に反応性を向上させる。加熱温度：よ一定以上の
溶解速度を得るために少なくとも６０℃とすることが好
ましく、溶液中の溶存酸素を除去するためである。加熱
温度の上限は塩酸の沸点（２０，２４％の塩酸の１気圧
下の沸点は１０８．６℃）とする。該加熱温度は必要な
溶解速度に応じて適宜選択することができる。Next, the hydrochloric acid solution is heated while stirring and maintaining a suspended state to further improve reactivity. Heating temperature: preferably at least 60° C. in order to obtain a dissolution rate above a certain level, and to remove dissolved oxygen in the solution. The upper limit of the heating temperature is the boiling point of hydrochloric acid (the boiling point of 20.24% hydrochloric acid under 1 atmosphere is 108.6°C). The heating temperature can be appropriately selected depending on the required dissolution rate.
撹拌及び加熱を続けながら、溶存酸素を除去し次いで前
記塩酸溶液中に塩素ガスを吹き込む。塩素ガスの吹き込
み量は加熱温度と溶液の量によって異なるが、１００℃
程度の加熱温度で１β程度の溶液の場合には１１／分程
度とし、吹き込み時に塩素ガスを加熱して吹き込むとよ
り好ましく、その温度は６０〜９０℃が良い。While stirring and heating are continued, dissolved oxygen is removed and chlorine gas is bubbled into the hydrochloric acid solution. The amount of chlorine gas blown varies depending on the heating temperature and the amount of solution, but it is
In the case of a solution with a heating temperature of about 1β, the heating rate is about 11/min, and it is more preferable to heat the chlorine gas at the time of blowing, and the temperature is preferably 60 to 90°C.
詳細な反応機構は明らかではないが、塩素ガスは酸化剤
として機能しイリジウムの酸化に寄与する。この場合従
来における塩素ガスの使用の場合と異なり反応が液相で
行われるため、より穏やかな条件つまり反応温度が塩酸
の沸点以下でも反応が十分に進行する。Although the detailed reaction mechanism is not clear, chlorine gas functions as an oxidizing agent and contributes to the oxidation of iridium. In this case, unlike the conventional case of using chlorine gas, the reaction is carried out in a liquid phase, so the reaction proceeds satisfactorily even under milder conditions, that is, the reaction temperature is below the boiling point of hydrochloric acid.
又酸化剤である塩素ガスは比較的容易に塩酸溶液から除
去することができ、塩素イオンとして溶液中に混入して
も加熱濃縮することで、純度の高い塩化イリジウム酸を
製造することができる。In addition, chlorine gas, which is an oxidizing agent, can be removed relatively easily from the hydrochloric acid solution, and even if it is mixed into the solution as chlorine ions, highly pure chloroiridic acid can be produced by heating and concentrating it.
（実施例）
次に本発明による塩化イリジウム酸の製造に関わる一実
施例を記載するが、本発明は該実施例により限定される
ものではない。(Example) Next, an example related to the production of chloroiridic acid according to the present invention will be described, but the present invention is not limited to this example.
イリジウム粉末２ｇを、９５℃で１２規定の塩酸溶液１
１に十分に撹拌しながら懸濁させた。該塩酸溶液を９５
℃に加熱し撹拌しながら、塩素ガスを約１！／分となる
ように３６時間連続して吹き込んだ。その後塩素ガス吹
き込みを停止し、塩酸溶液を濾過して未溶解のイリジウ
ム粉末を濾別し、乾燥後秤量したところその重量は０．
７５ ｇであった（溶解率６２．５％）。2 g of iridium powder was dissolved in 12 N hydrochloric acid solution at 95°C.
1 with thorough stirring. 95% of the hydrochloric acid solution
While heating to ℃ and stirring, add chlorine gas to about 1! The air was blown continuously for 36 hours at a rate of 1/min. After that, the chlorine gas blowing was stopped, the hydrochloric acid solution was filtered to remove undissolved iridium powder, and when it was dried and weighed, the weight was 0.
It was 75 g (dissolution rate 62.5%).
（発明の効果）
本発明は、イリジウム、又はイリジウムを含む混合物を
塩酸に溶解して塩化イリジウム酸を製造するにあたり、
該塩酸溶液を加熱するとともに、塩素ガスを吹き込んで
イリジウムを溶解するようにしである。この場合塩素ガ
スは酸化剤として機能し反応が液相で起こるため、反応
温度が塩酸の沸点以下の比較的穏やかな条件下でしかも
従来技術と比較して簡略化されたプロセスで、高い溶解
率で反応が十分に進行し、高い収率で塩化イリジウム酸
を得ることができる。又酸化剤である塩素ガスは比較的
容易に塩酸溶液から除去することができ、塩素イオンと
して溶液中に混入しても塩酸溶液中に既に存在している
ため不純物とはなることがなく、純度の高い塩化イリジ
ウム酸を製造することができる。(Effects of the Invention) The present invention provides the following steps when producing chloroiridic acid by dissolving iridium or a mixture containing iridium in hydrochloric acid.
While heating the hydrochloric acid solution, chlorine gas was blown into the solution to dissolve iridium. In this case, chlorine gas functions as an oxidizing agent and the reaction occurs in the liquid phase, so it is possible to achieve a high dissolution rate under relatively mild conditions where the reaction temperature is below the boiling point of hydrochloric acid, and in a process that is simplified compared to conventional technology. The reaction proceeds satisfactorily and chloroiridic acid can be obtained in high yield. In addition, chlorine gas, which is an oxidizing agent, can be removed relatively easily from the hydrochloric acid solution, and even if it is mixed into the solution as chlorine ions, it will not become an impurity because it already exists in the hydrochloric acid solution, and the purity will be reduced. It is possible to produce high chlorinated iridic acid.
Claims (1)
中で加熱して懸濁させながら塩素ガスを吹き込んで溶解
し、塩化イリジウム酸を製造することから成る塩化イリ
ジウム酸の製造方法。 ２、塩酸の濃度が６〜１２規定である特許請求の範囲第
１項に記載の方法。 ３、加熱温度が６０℃から塩酸の沸点までの間である特
許請求の範囲第１項又は第２項に記載の方法。 ４、塩素ガスの吹き込みを２０〜１００ｍｌ／分で行う
ようにした特許請求の範囲第１項から第３項までのいず
れかに記載の方法。[Claims] 1. A method for producing chloroiridic acid, which comprises heating and suspending iridium or a mixture containing iridium in concentrated hydrochloric acid and dissolving it by blowing chlorine gas into it to produce chloroiridic acid. . 2. The method according to claim 1, wherein the concentration of hydrochloric acid is 6 to 12 normal. 3. The method according to claim 1 or 2, wherein the heating temperature is between 60° C. and the boiling point of hydrochloric acid. 4. The method according to any one of claims 1 to 3, wherein the chlorine gas is blown at a rate of 20 to 100 ml/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27056788A JPH02116634A (en) | 1988-10-26 | 1988-10-26 | Preparation of chloroiridic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27056788A JPH02116634A (en) | 1988-10-26 | 1988-10-26 | Preparation of chloroiridic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02116634A true JPH02116634A (en) | 1990-05-01 |
Family
ID=17487956
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27056788A Pending JPH02116634A (en) | 1988-10-26 | 1988-10-26 | Preparation of chloroiridic acid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02116634A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015010667A1 (en) * | 2013-07-26 | 2015-01-29 | Safina, A.S. | Method of bulk iridium dissolution in hydrochloric acid media |
-
1988
- 1988-10-26 JP JP27056788A patent/JPH02116634A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015010667A1 (en) * | 2013-07-26 | 2015-01-29 | Safina, A.S. | Method of bulk iridium dissolution in hydrochloric acid media |
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