JP2773920B2 - Method for producing tetraammine palladium (II) chloride - Google Patents
Method for producing tetraammine palladium (II) chlorideInfo
- Publication number
- JP2773920B2 JP2773920B2 JP1254358A JP25435889A JP2773920B2 JP 2773920 B2 JP2773920 B2 JP 2773920B2 JP 1254358 A JP1254358 A JP 1254358A JP 25435889 A JP25435889 A JP 25435889A JP 2773920 B2 JP2773920 B2 JP 2773920B2
- Authority
- JP
- Japan
- Prior art keywords
- chloride
- palladium
- producing
- ethanol
- crystals
- 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
- C01G55/002—Compounds containing, besides ruthenium, rhodium, palladium, osmium, iridium, or platinum, two or more other elements, with the exception of oxygen or hydrogen
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、テトラアンミンパラジウム（II）クロライ
ドの製造方法に関するものである。Description: TECHNICAL FIELD The present invention relates to a method for producing tetraamminepalladium (II) chloride.
（従来技術とその問題点） 従来、テトラアンミンパラジウム（II）クロライド
（以下「〔Pd（NH3）４〕Cl2」と記載する。）の結晶の
製造方法は、一般的には塩化パラジウムをアンモニアア
ルカリとし溶液にしたものを濃縮またはエタノールで結
晶化させて合成するが、製造歩留りが低いという欠点が
ある。(Prior art and its problems) Conventionally, a method for producing crystals of tetraamminepalladium (II) chloride (hereinafter referred to as “[Pd (NH 3 ) 4 ] Cl 2 )” generally uses palladium chloride with ammonia. The solution is converted into an alkali, and the solution is concentrated or crystallized with ethanol for synthesis. However, there is a disadvantage that the production yield is low.
（発明の目的） 本発明は、従来の製造方法の欠点を解決するために成
されたもので、製造歩留りを向上させた〔Pd（N
H3）４〕Cl2の製造方法を提供することを目的とする。(Object of the Invention) The present invention has been made to solve the drawbacks of the conventional manufacturing method, and has improved manufacturing yield [Pd (N
An object of the present invention is to provide a method for producing H 3 ) 4 ] Cl 2 .
（問題点を解決するための手段） 本発明は、テトラアンミンパラジウム（II）クロライ
ドの製造方法において、乾燥した粉末状のジクロロジア
ンミンパラジウム（II）を反応理論量の1.4〜1.6倍の濃
アンモニア水中で室温、撹拌下で反応させ、濾過し、エ
タノールで洗浄して空気乾燥させることを特徴とするテ
トラアンミンパラジウム（II）クロライドの製造方法で
ある。(Means for Solving the Problems) The present invention relates to a process for producing tetraamminepalladium (II) chloride, wherein dried powdery dichlorodiamminepalladium (II) is dissolved in concentrated ammonia water of 1.4 to 1.6 times the theoretical amount of reaction. A process for producing tetraamminepalladium (II) chloride, which comprises reacting at room temperature under stirring, filtering, washing with ethanol, and air-drying.
上記の乾燥した粉末状のジクロロジアンミンパラジウ
ム（II）は、塩化パラジウムに塩化アンモン、塩化カリ
ウムまたは塩化ナトリウムを加えて得られるテトラクロ
ロパラジウム（II）塩に酢酸アンモニウム等を反応させ
て得られる黄色結晶であり、乾燥して粉末状とするの
は、アンモニア水との反応を速やかにさせることと、ア
ンモニア水の反応理論量を算出することが必要であり、
テトラアンミンパラジウム（II）クロライドの製造歩留
りを安定したものとするためである。The dried powdered dichlorodiammine palladium (II) is a yellow crystal obtained by reacting ammonium acetate or the like with a tetrachloropalladium (II) salt obtained by adding ammonium chloride, potassium chloride or sodium chloride to palladium chloride. In order to dry the powder, it is necessary to promptly react with the ammonia water and to calculate the reaction theoretical amount of the ammonia water,
This is because the production yield of tetraammine palladium (II) chloride is stabilized.
また、濃アンモニア水をジクロロジアンミンパラジウ
ム（II）の反応理論量の1.4〜1.6倍としたのは、1.7倍
以上では一部分溶解して歩留りの低下を生じ、1.3倍以
下では反応が不完全になりやすいからである。Also, the concentration of concentrated aqueous ammonia was set to 1.4 to 1.6 times the theoretical theoretical amount of dichlorodiammine palladium (II). If it was 1.7 times or more, it partially dissolved and the yield decreased, and if it was 1.3 times or less, the reaction was incomplete. Because it is easy.
前記反応理論量の算出に係わる反応式は次式による。 The reaction formula relating to the calculation of the reaction theoretical amount is as follows.
〔PdCl2（NH3）２〕＋2NH3→〔Pd（NH3）４〕Cl2 なお、反応は室温、撹拌下で行うのはアンモニアの蒸
発を抑制しながら短時間で反応させるためであり、反応
完結のポイントはジクロロジアンミンパラジウム（II）
の黄色結晶粉末が白色に完全に変化した点で、おおむね
２〜３時間で反応は完結する。[PdCl 2 (NH 3 ) 2 ] + 2NH 3 → [Pd (NH 3 ) 4 ] Cl 2 The reaction is carried out at room temperature and under stirring in order to carry out the reaction in a short time while suppressing the evaporation of ammonia. The point of completion of the reaction is dichlorodiammine palladium (II)
When the yellow crystalline powder has completely changed to white, the reaction is completed in about 2 to 3 hours.
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） 塩化パラジウム水溶液に塩化カリウム水溶液を加えて
加熱反応させ、さらに加熱して濃縮しテトラクロロパラ
ジウム（II）酸カリウムの結晶を得る。(Example 1) An aqueous potassium chloride solution was added to an aqueous palladium chloride solution, and the mixture was heated and reacted, and further heated and concentrated to obtain crystals of potassium tetrachloropalladium (II).
次いで、該結晶を少量の水に溶解し、酢酸アンモニウ
ム水溶液を５℃に冷却して混合し、５℃に保ち24時間後
濾過し、冷水にて洗浄し空気中で乾燥してジクロロジア
ンミンパラジウム（II）の黄色結晶を得る。Next, the crystals were dissolved in a small amount of water, and an aqueous ammonium acetate solution was cooled to 5 ° C. and mixed, kept at 5 ° C., filtered after 24 hours, washed with cold water, dried in air, and dried in dichlorodiammine palladium ( The yellow crystals of II) are obtained.
次いで、該ジクロロジアンミンパラジウム（II）の黄
色結晶（Pdとして10g）を粉末にしたものを、反応理論
量の1.5倍のアンモニア水（28％アンモニア水）40mlを
撹拌しながら、該粉末を少量ずつ加えたのち室温で約２
時間撹拌を続けて黄色粉末が完全に白色に変化したとこ
ろで撹拌を止め、ガラスフィルタで濾過し、エタノール
で洗浄して一夜間室温で乾燥して白色の結晶を得た。Next, yellow powder of dichlorodiammine palladium (II) (10 g as Pd) was powdered, and the powder was added little by little while stirring 40 ml of aqueous ammonia (28% ammonia water) 1.5 times the theoretical amount of reaction. After adding, about 2 at room temperature
Stirring was continued for a time, and when the yellow powder turned completely white, the stirring was stopped, and the mixture was filtered through a glass filter, washed with ethanol, and dried overnight at room temperature to obtain white crystals.
上記で得た白色結晶は18.8gでパラジウムの含有率を
化学分析したところ50.52wt％でＸ線回折により確認し
たところテトラアンミンパラジウム（II）クロライドで
あった。18.8 g of the white crystals obtained above were subjected to a chemical analysis of the palladium content at 50.52% by weight and confirmed by X-ray diffraction to be tetraamminepalladium (II) chloride.
得られた白色結晶からパラジウムの製造歩留りはジク
ロロジアンミンパラジウム（II）から95％であった。The production yield of palladium from the obtained white crystals was 95% from dichlorodiammine palladium (II).
（従来例） 塩化パラジウム（II）二水和物（Pdとして10g）を水
に溶解して過剰のアンモニア水を加え、湯浴上で加熱し
て無色の溶液とし、次いでこの溶液をホットプレート上
で加熱濃縮し、エタノール500ml加えて結晶を生成さ
せ、ガラスフィルタで濾過しエタノールで洗浄して一夜
間室温で乾燥して白色の結晶を得た。(Conventional example) Palladium (II) chloride dihydrate (10 g as Pd) is dissolved in water, excess ammonia water is added, and the mixture is heated on a hot water bath to form a colorless solution, and then this solution is placed on a hot plate. The solution was concentrated by heating with, and 500 ml of ethanol was added to generate crystals, which were filtered through a glass filter, washed with ethanol, and dried overnight at room temperature to obtain white crystals.
上記で得た白色結晶は9.50gでパラジウムの含有率を
化学分析したところ50.53wt％でＸ線回折により確認し
たところテトラアンミンパラジウム（II）クロライドで
あった。9.50 g of the white crystals obtained above were chemically analyzed for palladium content at 50.53 wt%, and were confirmed by X-ray diffraction to be tetraamminepalladium (II) chloride.
得られた白色結晶からパラジウムの製造歩留りは、塩
化パラジウムから48％であった。The production yield of palladium from the obtained white crystals was 48% from palladium chloride.
（実施例２） 塩化パラジウム水溶液に塩化アンモニウム粉末を加え
て撹拌し反応させ、濾過してテトラクロロパラジウム
（II）酸アンモニウムの結晶を得る。(Example 2) Ammonium chloride powder was added to an aqueous solution of palladium chloride, stirred, reacted, and filtered to obtain ammonium tetrachloropalladium (II) crystal.
次いで、該結晶を無水エタノールを加えて加熱溶解
し、エタノールにより還元されて生じた金属パラジウム
を濾過し、濾過液を−15℃に冷却し４倍モルの酢酸アン
モニウムのエタノール溶液を−15℃に冷却して混合し、
15分間後濾過し、冷エタノールにて洗浄し空気中で乾燥
してジクロロジアンミンパラジウム（II）の黄色結晶を
得る。Next, the crystals were dissolved by heating by adding anhydrous ethanol, and the metal palladium produced by the reduction with ethanol was filtered. The filtrate was cooled to -15 ° C, and a 4-fold molar solution of ammonium acetate in ethanol was cooled to -15 ° C. Cool and mix,
After fifteen minutes, the mixture is filtered, washed with cold ethanol and dried in air to obtain yellow crystals of dichlorodiamminepalladium (II).
次いで、該ジクロロジアンミンパラジウム（II）の黄
色結晶（Pdとして106.4g）を粉末にしたものを、反応理
論量の1.5倍のアンモニア水（28％アンモニア水）430ml
を撹拌しながら、該粉末を少量ずつ加えたのち室温で約
３時間撹拌を続けて黄色粉末が完全に白色に変化したと
ころで撹拌を止め、ガラスフィルタで濾過し、エタノー
ルで洗浄して一夜間室温で乾燥して白色の結晶を得た。
上記で得た白色結晶は200.1gでパラジウムの含有率を化
学分析したところ50.51wt％でＸ線回折により確認した
ところテトラアンミンパラジウム（II）クロライドであ
った。Next, powdery yellow crystals of dichlorodiammine palladium (II) (106.4 g as Pd) were added to 430 ml of aqueous ammonia (28% aqueous ammonia) 1.5 times the theoretical amount of reaction.
While stirring, the powder was added little by little, and stirring was continued at room temperature for about 3 hours. When the yellow powder turned completely white, the stirring was stopped, and the mixture was filtered through a glass filter, washed with ethanol, and washed overnight at room temperature. To give white crystals.
When the content of palladium in the white crystals obtained above was 200.1 g, the content of palladium was chemically analyzed. The content of the crystals was 50.51 wt%, and the content was confirmed to be tetraamminepalladium (II) chloride by X-ray diffraction.
得られた白色結晶からパラジウムの製造歩留りはジク
ロロジアンミンパラジウム（II）から95％であった。The production yield of palladium from the obtained white crystals was 95% from dichlorodiammine palladium (II).
（発明の効果） 以上説明したように、本発明の製造方法によればテト
ラアンミンパラジウム（II）クロライドを製造歩留りが
従来法に比べ極めて高いものとなり経済的効果のある画
期的なものと言える。(Effect of the Invention) As described above, according to the production method of the present invention, the production yield of tetraamminepalladium (II) chloride is extremely higher than that of the conventional method, and it can be said that this is an epoch-making one having an economic effect.
Claims (1)
ドの製造方法において、乾燥した粉末状のジクロロジア
ンミンパラジウム（II）を反応理論量の1.4〜1.6倍の濃
アンモニア水中で室温、撹拌下で反応させ、濾過し、エ
タノールで洗浄して空気乾燥させることを特徴とするテ
トラアンミンパラジウム（II）クロライドの製造方法。In a method for producing tetraamminepalladium (II) chloride, dried powdery dichlorodiamminepalladium (II) is reacted in 1.4 to 1.6 times the theoretical reaction amount of concentrated aqueous ammonia under stirring at room temperature and filtered. Washing the mixture with ethanol and drying the mixture with air, and then drying the mixture with air.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1254358A JP2773920B2 (en) | 1989-09-29 | 1989-09-29 | Method for producing tetraammine palladium (II) chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1254358A JP2773920B2 (en) | 1989-09-29 | 1989-09-29 | Method for producing tetraammine palladium (II) chloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03115127A JPH03115127A (en) | 1991-05-16 |
| JP2773920B2 true JP2773920B2 (en) | 1998-07-09 |
Family
ID=17263883
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1254358A Expired - Fee Related JP2773920B2 (en) | 1989-09-29 | 1989-09-29 | Method for producing tetraammine palladium (II) chloride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2773920B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102408091B1 (en) | 2021-11-30 | 2022-06-16 | 성일하이메탈(주) | method for tetramine dichloropalladium(Ⅱ) and tetramine dichloropalladium(Ⅱ) manufactured with this |
| KR102536993B1 (en) | 2022-10-27 | 2023-05-30 | 성일하이메탈(주) | method for tetramine palladium hydrogen carbonate and tetramine palladium hydrogen carbonate manufactured with this |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108864200B (en) * | 2018-08-06 | 2020-12-11 | 金川集团股份有限公司 | One-step preparation method of ethylenediamine palladium sulfate for electroplating |
-
1989
- 1989-09-29 JP JP1254358A patent/JP2773920B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102408091B1 (en) | 2021-11-30 | 2022-06-16 | 성일하이메탈(주) | method for tetramine dichloropalladium(Ⅱ) and tetramine dichloropalladium(Ⅱ) manufactured with this |
| KR102536993B1 (en) | 2022-10-27 | 2023-05-30 | 성일하이메탈(주) | method for tetramine palladium hydrogen carbonate and tetramine palladium hydrogen carbonate manufactured with this |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03115127A (en) | 1991-05-16 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |