JP2773941B2 - Palladium dissolution method - Google Patents
Palladium dissolution methodInfo
- Publication number
- JP2773941B2 JP2773941B2 JP1338919A JP33891989A JP2773941B2 JP 2773941 B2 JP2773941 B2 JP 2773941B2 JP 1338919 A JP1338919 A JP 1338919A JP 33891989 A JP33891989 A JP 33891989A JP 2773941 B2 JP2773941 B2 JP 2773941B2
- Authority
- JP
- Japan
- Prior art keywords
- palladium
- nitric acid
- lump
- dissolving
- dissolved
- 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
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直接硝酸に溶解
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塩素イオンが数百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, and it is possible to dissolve a palladium lump into a small lump directly in nitric acid, and to dissolve it in an extremely short time. Chloride ion in nitric acid solution with palladium dissolved is several hundred mg /
An object of the present invention is to provide a dissolving method that can:
（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加熱した硝酸中に加
え、さらに硝酸中に100〜200mg/の塩素イオンを加え
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
あり、前記硝酸中に加える塩素イオンが塩酸または塩化
ナトリウム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, a small mass of the palladium is added to heated nitric acid, and further, 100 to 200 mg / chlorine ion is added to the nitric acid to cause a reaction, and the chlorine is added to the nitric acid. This is a method for dissolving palladium in which the ion is hydrochloric acid or sodium chloride.
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、
硝酸を加熱しておき、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,
Heating the nitric acid and adding the palladium lumps
Because it is preferable that the dissolution reaction be 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 the dissolution reaction difficult. is there.
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.
次いで、硝酸中に塩酸または塩化ナトリウムを該硝酸
中に100〜200mg/の塩素イオン量となる分を加えるこ
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。Then, by adding hydrochloric acid or sodium chloride in nitric acid in an amount of 100 to 200 mg / chloride ion in nitric acid, the palladium small lump acts as an auxiliary agent for proceeding to the reaction of dissolving in nitric acid. Can be dissolved.
該塩素イオン量が硝酸溶液中で100〜200mg/とする
のは、100mg/以下では溶解時間が長くなり、200mg/
以上では塩化パラジウムが生成するのと、塩素イオンが
多くなり除去操作を必要としてしまうからである。The reason why the amount of chloride ions is set to 100 to 200 mg / in a nitric acid solution is that the dissolution time becomes longer at 100 mg / or less, and 200 mg /
This is because palladium chloride is generated and chlorine ions increase to require a removal operation.
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 5 kg 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 small palladium lumps.
硝酸（濃度13.5規定）10を62℃に加熱したところ
え、上記のパラジウムの小塊（平均粒径8.5mm）を加
え、直ちに濃塩酸5ml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80.8％分を溶解させることがで
きた。When nitric acid (concentration: 13.5N) 10 was heated to 62 ° C, the above-mentioned small palladium lump (average particle size: 8.5 mm) was added, and immediately 5 ml of concentrated hydrochloric acid was added to dissolve it. Was able to dissolve 80.8%.
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150mg/であった。The concentration of chloride ions in the nitric acid solution in which palladium was dissolved was 150 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、6
0℃に加熱した硝酸（濃度13.5規定）60mlに加え、直ち
に塩化ナトリウム1.5g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76.4％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塩素イオ
ンの濃度は150mg/であった。(Example 2) 30 g of palladium lump processed in the same manner as in Example 1 was
To 60 ml of nitric acid (concentration: 13.5N) heated to 0 ° C, immediately add 1.5 g of sodium chloride and dissolve. After 30 minutes, a small palladium lump can dissolve 76.4% of the palladium and dissolve palladium. The concentration of chloride ion in the obtained nitric acid solution was 150 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、加熱して塩素イオン90
mg/分を加えて溶解させたが、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 a small lump of palladium processed in the same manner as in Example 1 was added to 10 nitric acid (concentration of 13.5 N), and heated to 90% chlorine ion.
mg / min was added to dissolve, but after 30 minutes only 29.7% of the palladium lumps had dissolved.
（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塩素イオン濃度
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 chloride ion concentration 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加熱した硝酸中に加
え、さらに硝酸中に100〜200mg/の塩素イオンを加え
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, characterized by adding 100 to 200 mg / chloride ion to nitric acid in addition to heated nitric acid to cause a reaction.
は塩化ナトリウムである請求項１に記載のパラジウムの
溶解方法。2. The method for dissolving palladium according to claim 1, wherein the chloride ion added to the nitric acid is hydrochloric acid or sodium chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1338919A JP2773941B2 (en) | 1989-12-27 | 1989-12-27 | Palladium dissolution method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1338919A JP2773941B2 (en) | 1989-12-27 | 1989-12-27 | Palladium dissolution method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03199127A JPH03199127A (en) | 1991-08-30 |
| JP2773941B2 true JP2773941B2 (en) | 1998-07-09 |
Family
ID=18322566
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1338919A Expired - Lifetime JP2773941B2 (en) | 1989-12-27 | 1989-12-27 | Palladium dissolution method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2773941B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912141B (en) * | 2021-12-09 | 2023-05-05 | 沈阳有色金属研究院有限公司 | Method for preparing palladium chloride by using deactivated palladium nitrate |
-
1989
- 1989-12-27 JP JP1338919A patent/JP2773941B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03199127A (en) | 1991-08-30 |
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