JP2773942B2 - Palladium dissolution method - Google Patents
Palladium dissolution methodInfo
- Publication number
- JP2773942B2 JP2773942B2 JP1338920A JP33892089A JP2773942B2 JP 2773942 B2 JP2773942 B2 JP 2773942B2 JP 1338920 A JP1338920 A JP 1338920A JP 33892089 A JP33892089 A JP 33892089A JP 2773942 B2 JP2773942 B2 JP 2773942B2
- Authority
- JP
- Japan
- Prior art keywords
- palladium
- lump
- nitric acid
- dissolved
- dissolving
- 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 - Fee Related
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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は、パラジウム硝酸溶液を調製するためのパラ
ジウムの溶解方法に関するものである。Description: TECHNICAL FIELD The present invention relates to a method for dissolving palladium for preparing a palladium nitrate solution.
（従来技術とその問題点） 従来、パラジウム塊を溶解する方法として、パラジウ
ムを加熱溶解してショットし粒状または偏平小塊にする
か、圧延して薄板状にして王水に溶解し、水酸化アルカ
リを加えて中和してパラジウムの水酸化物を生成し、濾
過洗浄してパラジウムの水酸化物を硝酸に溶解してパラ
ジウムの硝酸溶液を調製する方法で製造工程が長く、し
かも水酸化パラジウム中に塩素イオンが吸着し洗浄を十
分に行っても塩素イオンを除くことが困難で、塩素イオ
ンを除くために硝酸銀または酸化銀を塩素イオンの当量
を加えて塩化銀の沈澱を生成して濾過分離するというこ
とが必要であった。(Prior art and its problems) Conventionally, as a method for dissolving palladium lump, palladium is heated and melted and shot into granules or flat small lump, or rolled into a thin plate and dissolved in aqua regia, and hydroxylated. A method of preparing a palladium hydroxide by neutralizing by adding an alkali to produce a palladium hydroxide, washing by filtration, dissolving the palladium hydroxide in nitric acid to prepare a palladium nitric acid solution, and a long production process, and furthermore, palladium hydroxide Chlorine ions are adsorbed inside and it is difficult to remove chloride ions even if washing is performed sufficiently. To remove chloride ions, silver chloride is added to silver nitrate or silver oxide by adding an equivalent of chloride ions to form a precipitate of silver chloride, which is then filtered. It was necessary to separate.
また、前記パラジウムの薄板状、粒状あるいは偏平小
塊にしたものを直接硝酸に溶解しようとしても極めて長
時間を要し生産効率の低いという欠点があった。Further, there is a drawback in that even if the palladium formed into a thin plate, granular or flat small mass is directly dissolved in nitric acid, it takes an extremely long time and the production efficiency is low.
他に、微粉末を生成して硝酸に溶解する方法もある
が、やはりパラジウム塊を微粉末にする工程が必要で工
程が長くなり生産効率が低いものであった。In addition, there is a method of producing fine powder and dissolving it in nitric acid. However, a step of pulverizing the palladium lump into fine powder is required, which requires a long process and low production efficiency.
（発明の目的） 本発明は、上記従来法の欠点を解決するために成され
たもので、パラジウム塊を小塊にしてハロゲン化合物の
水溶液に浸漬したのち、硝酸に溶解し、しかも、極めて
短時間で溶解することができ、パラジウムを溶解した硝
酸溶液中のハロゲンイオンを数百mg/以下にすること
ができるという、溶解方法を提供することを目的とする
ものである。(Object of the Invention) The present invention has been made in order to solve the above-mentioned drawbacks of the conventional method. A palladium lump is made into a small lump, immersed in an aqueous solution of a halogen compound, and then dissolved in nitric acid. An object of the present invention is to provide a dissolving method capable of dissolving in a short time and reducing the amount of halogen ions in a nitric acid solution in which palladium is dissolved to several hundred mg / or less.
（問題点を解決するための手段） 本発明は、パラジウム塊を溶解する方法において、該
パラジウム塊を窒素雰囲気中で加熱溶解し、溶解したパ
ラジウムの溶湯を水中に落下させてパラジウムの小塊と
し、次いで、該パラジウムの小塊をハロゲン化合物の水
溶液に浸漬させたのち、該パラジウムの小塊を洗浄し
て、加熱した硝酸中に加えて反応させることを特徴とす
るパラジウムの溶解方法で、前記ハロゲン化合物が弗化
水素、塩化水素、臭化水素、沃化水素より選ばれた１種
であるパラジウムの溶解方法である。(Means for Solving the Problems) The present invention relates to a method for dissolving a palladium lump, which comprises heating and dissolving the palladium lump in a nitrogen atmosphere, and dropping a melt of the dissolved palladium into water to form a small palladium lump. Then, after immersing the palladium lumps in an aqueous solution of a halogen compound, the palladium lumps are washed and added to heated nitric acid to cause a reaction. This is a method for dissolving palladium in which the halogen compound is one selected from hydrogen fluoride, hydrogen chloride, hydrogen bromide and hydrogen iodide.
パラジウム塊をまず窒素雰囲気中で加熱溶解してパラ
ジウムの溶湯とし、該溶湯を水中に落下させてパラジウ
ムの小塊とするのは表面積を大きくして硝酸に溶解させ
やすくするためである。First, the mass of palladium is heated and dissolved in a nitrogen atmosphere to form a molten palladium, and the molten metal is dropped into water to form a small mass of palladium in order to increase the surface area and facilitate dissolution in nitric acid.
窒素雰囲気中で加熱溶解するのは、大気中ではパラジ
ウムが酸化して硝酸に溶解しなくなるからである。The reason for heating and dissolving in a nitrogen atmosphere is that palladium is oxidized in the air and no longer dissolves in nitric acid.
パラジウムの小塊を硝酸に溶解するにあたり、まず、
ハロゲン化合物の水溶液に浸漬させ、次いで水洗しての
ち、加熱した硝酸にハロゲン化合物の水溶液に浸漬し水
洗した該パラジウムの小塊を加えるのは、溶解反応を短
時間で行わせることが好ましいからで、硝酸を加熱して
おかないでパラジウム小塊を加えるとパラジウム小塊の
表面に不動態膜が形成しやすく、溶解反応をさせにくく
するからである。In dissolving small palladium lumps in nitric acid,
The reason why the small palladium immersed in the aqueous solution of the halogen compound and then washed with water is added to the heated nitric acid after immersion in the aqueous solution of the halogen compound and then washed with water is because the dissolution reaction is preferably performed in a short time. If a small palladium lump is added without heating the nitric acid, a passivation film is easily formed on the surface of the small palladium lump, which makes it difficult to cause a dissolution reaction.
硝酸の温度は50〜70℃とするのが好ましく、50℃以下
では反応が不十分であり、70℃以上では硝酸が揮発しや
すくムダを生ずるだけでなく、パラジウムの小塊が蓄熱
して酸化してしまうことが生じやすいからである。The temperature of nitric acid is preferably 50 to 70 ° C. If the temperature is lower than 50 ° C, the reaction is insufficient.If it is higher than 70 ° C, not only nitric acid is easily volatilized, but also waste is generated. This is because it is easy to occur.
ハロゲン化合物の水溶液に浸漬させるのは、パラジウ
ムの小塊にハロゲンイオンを数百PPM含浸させことで、
パラジウム小塊が硝酸に溶解する反応へ進ませる補助剤
として働くので、短時間で溶解させることができる。Dipping in an aqueous solution of a halogen compound is achieved by impregnating small palladium lumps with halogen ions at several hundred ppm.
Since the palladium lumps serve as an auxiliary for promoting the reaction of dissolving in nitric acid, they can be dissolved in a short time.
該ハロゲン化合物の水溶液の濃度は3.8〜5.5モル／
とするのが良く、浸漬時間は20分間以上で良い。The concentration of the aqueous solution of the halogen compound is 3.8 to 5.5 mol /
The immersion time may be 20 minutes or more.
また、ハロゲン化合物の水溶液に浸漬させたパラジウ
ムの小塊を水洗するのはハロゲン化合物が多すぎるとハ
ロゲン化パラジウムが生成するのと、ハロゲンイオンが
多くなり除去操作を必要としてしまうからで、水洗の程
度は洗浄した水が中性になったところで止めるのが良
い。In addition, washing a small lump of palladium immersed in an aqueous solution of a halogen compound with water is not sufficient because palladium halide is generated when the amount of the halogen compound is too large, and the amount of halogen ions increases and a removal operation is required. It is better to stop when the washed water becomes neutral.
なお、ハロゲン化合物として前記のハロゲン化合物に
限定するのは、パラジウムを溶解した硝酸溶液中に陽イ
オンとしてアルカリ金属イオン等の不純物を混入させな
いためである。The reason why the halogen compound is limited to the above-mentioned halogen compound is to prevent impurities such as alkali metal ions and the like as cations from being mixed in a nitric acid solution in which palladium is dissolved.
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。Hereinafter, examples according to the present invention will be described, but the examples do not limit the present invention.
（実施例１） パラジウムの5kg塊をジルコニア製ルツボ内に入れ高
周波炉で1600℃で窒素雰囲気中で溶解し、溶湯を水中に
落下させてパラジウムの小塊に加工した。(Example 1) A 5 kg lump of palladium was placed in a zirconia crucible, melted in a high-frequency furnace at 1600 ° C in a nitrogen atmosphere, and the molten metal was dropped into water to be processed into a small palladium lump.
該パラジウムの小塊を塩化水素水溶液（12％）に20分
間浸漬し、次いで、該パラジウムの小塊を純粋で洗浄し
た水が中性になるまで行ったのち、硝酸（濃度13.5規
定）10を62℃に加熱したところへ、上記のパラジウム
の小塊（平均粒径8.5mm）を加えて溶解したところ、30
分間後にパラジウムの小塊が86.7％分を溶解させること
ができた。The lumps of palladium are immersed in an aqueous hydrogen chloride solution (12%) for 20 minutes, and the lumps of palladium are washed until the pure and washed water becomes neutral. When heated to 62 ° C., the above small palladium lump (average particle size 8.5 mm) was added and dissolved.
After a minute, the palladium nodules were able to dissolve 86.7%.
また、パラジウムを溶解した硝酸溶液中の塩素イオン
の濃度は154mg/であった。Further, the concentration of chloride ion in the nitric acid solution in which palladium was dissolved was 154 mg /.
（実施例２） 実施例１と同様に加工したパラジウムの小塊30gを、
弗化水素水溶液（12％）に20分間浸漬したのち、純粋で
洗浄して洗浄水が中性となったのち、60℃に加熱した硝
酸（濃度13.5規定）60mlに加え、溶解したところ、30分
間後にパラジウムの小塊が88.5％分を溶解させることが
でき、また、パラジウムを溶解した硝酸溶液中の弗素イ
オンの濃度は150mg/であった。(Example 2) A small lump of palladium 30 g processed in the same manner as in Example 1 was
After immersion in hydrogen fluoride aqueous solution (12%) for 20 minutes, washing with pure water and neutralization of the washing water, the solution was added to 60 ml of nitric acid (concentration: 13.5N) heated to 60 ° C and dissolved. After minutes, the palladium lumps were able to dissolve 88.5%, and the concentration of fluoride ions in the palladium dissolved nitric acid solution was 150 mg /.
（実施例３） 実施例１と同様に加工したパラジウムの小塊30gを、
臭化水素水溶液（12％）に30分間浸漬したのち、純粋で
洗浄して洗浄水が中性となったのち、60℃に加熱した硝
酸（濃度13.5規定）60mlに加え、溶解したところ、30分
間後にパラジウムの小塊が85.5％分を溶解させることが
でき、また、パラジウムを溶解した硝酸溶液中の臭素イ
オンの濃度は140mg/であった。(Example 3) 30 g of palladium lump processed in the same manner as in Example 1 was
After being immersed in a hydrogen bromide aqueous solution (12%) for 30 minutes, washed with pure water and the washing water became neutral, the solution was added to 60 ml of nitric acid (concentration: 13.5N) heated to 60 ° C and dissolved. After a minute, the palladium lumps were able to dissolve 85.5%, and the concentration of bromine ions in the nitric acid solution in which palladium was dissolved was 140 mg /.
（実施例４） 実施例１と同様に加工したパラジウムの小塊30gを、
沃化水素水溶液（12％）に30分間浸漬したのち、純粋で
洗浄して洗浄水が中性となったのち、60℃に加熱した硝
酸（濃度13.5規定）60mlに加え、溶解したところ、30分
間後にパラジウムの小塊が89.5％分を溶解させることが
でき、また、パラジウムを溶解した硝酸溶液中の沃素イ
オンの濃度は130mg/であった。(Example 4) 30 g of a small lump of palladium processed in the same manner as in Example 1 was used.
After being immersed in an aqueous solution of hydrogen iodide (12%) for 30 minutes, washed with pure water to make the washing water neutral, the solution was added to 60 ml of nitric acid (concentration: 13.5 N) heated to 60 ° C. and dissolved. After minutes, the palladium lumps were able to dissolve 89.5% of the mass, and the concentration of iodine ions in the nitric acid solution in which palladium was dissolved was 130 mg /.
（比較例） 実施例１と同様に加工したパラジウムの小塊5kgを硝
酸（濃度13.5規定）10に加え、加熱して溶解させた
が、30分間後で29.7％分のパラジウムの小塊が溶解した
だけであった。(Comparative Example) 5 kg of palladium lumps processed in the same manner as in Example 1 were added to 10 nitric acid (concentration: 13.5) and dissolved by heating. After 30 minutes, 29.7% of palladium lumps were dissolved. I just did.
（発明の効果） 以上のように、本発明の方法によれば、パラジウムの
塊を極めて短時間で硝酸に溶解させることができ、しか
も、パラジウムを溶解した硝酸溶液中のハロゲンイオン
濃度も200mg/以下と極めて少ないものであり、硝酸パ
ラジウム溶液として各種のパラジウム化合物等を合成さ
せるための出発原料として用いることができという、画
期的な方法である。(Effect of the Invention) As described above, according to the method of the present invention, a lump of palladium can be dissolved in nitric acid in a very short time, and the concentration of halogen ions in the nitric acid solution in which palladium is dissolved is also 200 mg / p. This is an epoch-making method that can be used as a starting material for synthesizing various palladium compounds and the like as a palladium nitrate solution.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.6，ＤＢ名) B01F 1/00 B22F 9/00 - 9/30 C01G 25/00 - 47/00 C01G 49/10 - 57/00 ＣＡＳ ｏｎ−ｌｉｎｅ──────────────────────────────────────────────────続 き Continuation of front page (58) Field surveyed (Int.Cl. 6 , DB name) B01F 1/00 B22F 9/00-9/30 C01G 25/00-47/00 C01G 49/10-57 / 00 CAS on-line
Claims (2)
パラジウム塊を窒素雰囲気中で加熱溶解し、溶解したパ
ラジウムの溶湯を水中に落下させてパラジウムの小塊と
し、次いで、該パラジウムの小塊をハロゲン化合物の水
溶液に浸漬させたのち、該パラジウムの小塊を洗浄し
て、加熱した硝酸中に加えて反応させることを特徴とす
るパラジウムの溶解方法。In the method for dissolving a palladium lump, the palladium lump is heated and dissolved in a nitrogen atmosphere, and a melt of the dissolved palladium is dropped into water to form a palladium lump, and then the palladium lump is removed. A method for dissolving palladium, comprising immersing the palladium in an aqueous solution of a halogen compound, washing the palladium lumps, and adding the reaction to heated nitric acid for reaction.
素、臭化水素、沃化水素より選ばれた１種である請求項
１に記載のパラジウムの溶解方法。2. The method according to claim 1, wherein the halogen compound is one selected from hydrogen fluoride, hydrogen chloride, hydrogen bromide, and hydrogen iodide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1338920A JP2773942B2 (en) | 1989-12-27 | 1989-12-27 | Palladium dissolution method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1338920A JP2773942B2 (en) | 1989-12-27 | 1989-12-27 | Palladium dissolution method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03199128A JPH03199128A (en) | 1991-08-30 |
| JP2773942B2 true JP2773942B2 (en) | 1998-07-09 |
Family
ID=18322575
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1338920A Expired - Fee Related JP2773942B2 (en) | 1989-12-27 | 1989-12-27 | Palladium dissolution method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2773942B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4599558B2 (en) | 2005-04-22 | 2010-12-15 | 国立大学法人九州工業大学 | Pitch period equalizing apparatus, pitch period equalizing method, speech encoding apparatus, speech decoding apparatus, and speech encoding method |
| PL2987571T3 (en) * | 2014-08-19 | 2019-02-28 | Heraeus Deutschland GmbH & Co. KG | Method for the production of active palladium (0) powder, active palladium (0) powder and its use in making a palladium salt |
-
1989
- 1989-12-27 JP JP1338920A patent/JP2773942B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03199128A (en) | 1991-08-30 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |