JP2879582B2 - Purification method of cyanuric diaurate - Google Patents
Purification method of cyanuric diaurateInfo
- Publication number
- JP2879582B2 JP2879582B2 JP30233189A JP30233189A JP2879582B2 JP 2879582 B2 JP2879582 B2 JP 2879582B2 JP 30233189 A JP30233189 A JP 30233189A JP 30233189 A JP30233189 A JP 30233189A JP 2879582 B2 JP2879582 B2 JP 2879582B2
- Authority
- JP
- Japan
- Prior art keywords
- diaurate
- cyanide
- potassium
- cyanuric
- acetone
- 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
Landscapes
- Chemically Coating (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は、金メッキ工程で採用される金メッキ浴の金
源として使用されているシアン化第２金酸カリウムやシ
アン化第２金酸ナトリウム等のシアン化第２金酸塩、す
なわちテトラシアノ金（III）酸塩MI［Au（CN）４］（M
Iは１価陽イオン）の粗製品の精製方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to potassium cyanide diaurate, sodium cyanide diaurate and the like used as a gold source in a gold plating bath employed in a gold plating step. Cyanodiaurate, ie, tetracyanoaurate (III), M I [Au (CN) 4 ] (M
I is a monovalent cation).
［従来の技術］ シアン化第２金酸カリウムは塩化第２金酸カリウムを
シアン化カリウムで置換して得られている。また、シア
ン化第２金酸ナトリウムは、塩化第２金酸ナトリウムを
シアン化ナトリウムで置換して得られている。これらの
反応は次の式で表わすことができる。[Prior Art] Potassium cyanide diaurate is obtained by replacing potassium dichloroaurate with potassium cyanide. Also, sodium cyanide diaurate is obtained by replacing sodium diaurate chloride with sodium cyanide. These reactions can be represented by the following equations.
Ｍ［AuCl4］＋4MCN→ MAu（CN）４＋4MCl （式中のＭはＫまたはNaを表わす。） ‥‥（１） （１）式からわかるように、この反応の副生成物とし
て、塩化カリウムまたは塩化ナトリウムが生成する。こ
れらの副生成物を除去するために、水溶液中でシアン化
第２金酸カリウムKAu（CN）４またはシアン化第２金酸
ナトリウムNaAu（CN）４を晶析させて固液分離する方法
やエタノールでシアン化第２金酸カリウムまたはシアン
化第２金酸ナトリウムを溶媒抽出する方法などが行われ
ている。M [AuCl 4 ] + 4MCN → MAu (CN) 4 + 4MCl (M in the formula represents K or Na) (1) As can be seen from the formula (1), potassium chloride is used as a by-product of this reaction. Or sodium chloride forms. In order to remove these by-products, a method of crystallizing potassium diaurate potassium KAu (CN) 4 or sodium cyanide diaurate NaAu (CN) 4 in an aqueous solution and performing solid-liquid separation, A method of extracting potassium cyanide diaurate or sodium cyanide diaurate with ethanol has been used.
［発明が解決しようとする課題］ 前記（１）式に従って行う従来技術の、水溶液中でシ
アン化第２金酸カリウムまたはシアン化第２金酸ナトリ
ウムを晶析させる方法においては、これらの第２金酸塩
が水に易溶であるため、晶析しないで水溶液中に残存す
る金が相当量ある。そこで、晶析後固液分離して得た液
を前記（１）式に従う置換反応系に戻して再使用するこ
とが行われるが、これを何回も繰り返すと溶液中に塩化
カリウムまたは塩化ナトリウムが蓄積される結果、晶析
した製品中に混入する塩化カリウムまたは塩化ナトリウ
ムの量が増加してくるため、製品が本来の目的にそぐわ
ない純度の低いものとなってしまう。このため、上記従
来の方法においては、晶析工程終了後の溶液を常に前記
置換反応工程に戻して再使用するわけにはいかず、少な
くともこの溶液の一部を別途処理して液中の金を回収す
る工程を設けることがどうしても必要となる。このよう
に副次的回収工程の増加と、該回収工程における金の収
率の低さと、これによる金の直接歩留りの低下等が製品
コストを高める重要な原因の一つとなっている。[Problems to be Solved by the Invention] In the prior art method of crystallizing potassium cyanide diaurate or sodium cyanide diaurate in an aqueous solution carried out according to the above formula (1), these second methods are used. Since gold salts are easily soluble in water, a considerable amount of gold remains in the aqueous solution without crystallization. Therefore, the liquid obtained by solid-liquid separation after crystallization is returned to the substitution reaction system according to the above formula (1) and reused. If this is repeated many times, potassium chloride or sodium chloride is contained in the solution. As a result, the amount of potassium chloride or sodium chloride mixed into the crystallized product increases, resulting in the product having a low purity that does not meet its intended purpose. For this reason, in the above-mentioned conventional method, the solution after the crystallization step cannot always be returned to the substitution reaction step and reused, and at least a part of the solution is separately treated to remove gold in the solution. It is absolutely necessary to provide a recovery step. As described above, the increase in the number of the secondary recovery steps, the low yield of gold in the recovery step, and the reduction in the direct yield of gold due to this increase are one of the important factors that increase the product cost.
一方、従来技術のエタノールで溶媒抽出する方法は、
エタノールへの塩化カリウムの溶解度が0.08KCl/C2H5OH
100mlという比較的高い値であるため（Atherton Seidel
l,“Solubilities",1953,D・Van Nosthrand Company p.
776,p.780）、塩化カリウムの除去を完全に行うことは
困難である。On the other hand, the solvent extraction method using ethanol of the prior art
The solubility of potassium chloride in ethanol is 0.08KCl / C 2 H 5 OH
Because of the relatively high value of 100ml (Atherton Seidel
l, “Solubilities”, 1953, D. Van Nosthrand Company p.
776, p.780), and it is difficult to completely remove potassium chloride.
［課題を解決するための手段］ 上記課題を解決するため鋭意研究した成果として、本
発明者は、アセトンをシアン化第２金酸カリウムまたは
シアン化第２金酸ナトリウムの溶媒として使用すること
により、それらシアン化第２金酸塩の精製を有利に実施
できることを見出し、本発明に到達した。[Means for Solving the Problems] As a result of earnest studies to solve the above problems, the present inventor has found that acetone is used as a solvent for potassium cyanide diaurate or sodium cyanide diaurate. The inventors have found that the purification of these cyanuric diaurates can be advantageously performed, and have reached the present invention.
［作用］ 本発明者の研究により、次のことが見い出された。[Action] The following has been found by the study of the present inventors.
シアン化第２金酸カリウム［KAu（CN）４］およびシ
アン化第２金酸ナトリウム［NaAu（CN）４］は、いずれ
もアセトンへの溶解が容易であり、その溶解度も大き
い。一方塩化カリウム（KCl）および塩化ナトリウム（N
aCl）のアセトンへの溶解度はいずれも極めて小さく、
ほとんど０に近い。したがって、アセトンの持つこの特
性を利用すれば、KClを不純物として含む粗製KAu（CN）
４、またはNaClを不純物として含む粗製NaAu（CN）４を
アセトンに溶解して固液分離し、得られた液分からアセ
トンを減圧等の手段で蒸発除去することにより、容易に
純度の高いKAu（CN）４またはNaAu（CN）４を得ること
ができる。Potassium cyanide diaurate [KAu (CN) 4 ] and sodium cyanide diaurate [NaAu (CN) 4 ] are both easily dissolved in acetone and have high solubility. On the other hand, potassium chloride (KCl) and sodium chloride (N
aCl) has very low solubility in acetone,
Nearly 0. Therefore, by utilizing this property of acetone, crude KAu (CN) containing KCl as an impurity
4 or crude NaAu (CN) 4 containing NaCl as an impurity is dissolved in acetone to perform solid-liquid separation, and acetone is evaporated and removed from the obtained liquid by means of reduced pressure or the like, so that highly pure KAu ( CN) 4 or NaAu (CN) 4 can be obtained.
上記のアセトンを有機相として用いる溶媒抽出法を利
用すれば、前記（１）式の置換反応系に戻すことのでき
ないシアン化第２金酸塩を含む置換終了後の液から、シ
アン化第２金酸塩を容易に回収することができる。If the solvent extraction method using acetone as the organic phase is used, the liquid after the completion of the substitution containing the cyanuric diaurate, which cannot be returned to the substitution reaction system of the above formula (1), is used. Goldate can be easily recovered.
［実施例１］ 試薬のシアン化第２金酸カリウム、KAu（CN）４・0.5
H2O（金量で300.0g）と試薬の塩化カリウム、KCl（300
g）とを混合した試料を用いて、下記の手順により該混
合試料の精製試験を行った。[Example 1] Potassium cyanide second aurate reagents, KAu (CN) 4 · 0.5
H 2 O (300.0 g in gold) and reagents potassium chloride and KCl (300
g) was used to perform a purification test on the mixed sample according to the following procedure.
混合試料を試薬特級のアセトン２に溶解させ、不溶
分であるKClを濾過により除去した。さらにこの不溶分
をアセトンで充分に洗浄し、洗浄液は先の瀘液に合体さ
せた。この濾液をエバポレータに移し減圧してアセトン
を蒸発除去した。残留した固形分を80℃で数分間かけて
重量が一定になるまで乾燥したものを精製シアン化第２
金酸カリウムとし、分析した下記第１表に示す結果を得
た。The mixed sample was dissolved in reagent grade acetone 2 and insoluble KCl was removed by filtration. Further, this insoluble content was sufficiently washed with acetone, and the washing solution was combined with the filtrate. The filtrate was transferred to an evaporator, and the pressure was reduced to remove acetone by evaporation. The remaining solid was dried at 80 ° C. for several minutes until the weight became constant, and purified cyanide
The results are shown in Table 1 below, which were analyzed by using potassium aurate.
［発明の効果］ 実施例１の経過から明らかであるように、粗製シアン
化第２金酸塩の精製においては金の直接歩留りがほぼ10
0％に近く、不純物の塩素分はほぼ０である。アセトン
がシアン化第２金酸カリウムまたはシアン化第２金酸ナ
トリウムの精製用溶媒として極めて優れていることは明
白である。 [Effect of the Invention] As is clear from the course of Example 1, in the purification of the crude cyanide diaurate, the direct yield of gold was almost 10%.
It is close to 0%, and the chlorine content of the impurity is almost 0. It is evident that acetone is a very good solvent for the purification of potassium diaurate cyanide or sodium diaurate cyanide.
Claims (3)
ンで溶解した後、固液分離して不純物を固形物として除
き、得られた液分からアセトンを蒸発除去することを特
徴とするシアン化第２金酸塩の精製方法。1. A cyanide comprising dissolving a cyanuric diaurate containing impurities in acetone, separating the solids and liquids to remove impurities as solids, and evaporating and removing acetone from the obtained liquid fraction. A method for purifying an activated secondary gold salt.
酸カリウム、KAu（CN）４であり、主たる不純物がKClで
ある請求項１記載の方法。2. The method according to claim 1, wherein said dicyanoaurate is potassium diaurate, KAu (CN) 4 and the main impurity is KCl.
酸ナトリウム、NaAu（CN）４であり、主たる不純物がNA
Clである請求項１記載の方法。3. The cyanuric diaurate is sodium cyanide diaurate, NaAu (CN) 4 , and the main impurity is NA.
2. The method according to claim 1, wherein Cl is Cl.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30233189A JP2879582B2 (en) | 1989-11-21 | 1989-11-21 | Purification method of cyanuric diaurate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30233189A JP2879582B2 (en) | 1989-11-21 | 1989-11-21 | Purification method of cyanuric diaurate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03164428A JPH03164428A (en) | 1991-07-16 |
| JP2879582B2 true JP2879582B2 (en) | 1999-04-05 |
Family
ID=17907652
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30233189A Expired - Fee Related JP2879582B2 (en) | 1989-11-21 | 1989-11-21 | Purification method of cyanuric diaurate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2879582B2 (en) |
-
1989
- 1989-11-21 JP JP30233189A patent/JP2879582B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03164428A (en) | 1991-07-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| SU867319A3 (en) | Method of processing materials containing arsenic and metal | |
| JP2879582B2 (en) | Purification method of cyanuric diaurate | |
| EP0863135B1 (en) | Method for separating ammonium sulfate and ammonium bisulfate from each other and process for producing 2-hydroxy-4-methylthiobutanoic acid utilizing the method | |
| EP0174142B1 (en) | Recovery of squaric acid | |
| US2984661A (en) | Method of preparing pure vitamin b12 and intermediary obtained thereby | |
| JP4483441B2 (en) | Method for purifying rhodium from liquid containing high iridium and ruthenium | |
| JP3753554B2 (en) | Silver recovery method | |
| US2005700A (en) | Process of extracting sex hormones and a compound of a sex hormone with an alkaloid | |
| JPH0135765B2 (en) | ||
| SU1303631A1 (en) | Method for extracting copper from used copper-ammoniate pickling solutions | |
| JP3407336B2 (en) | Method for purifying aminoethanesulfonic acids | |
| EP0564775A2 (en) | Process for pharmaceutical grade high purity iodeoxycholic acid preparation | |
| US4418016A (en) | Method for recovering omega-amino-dodecanoic acid from crystallization mother liquors | |
| JP4683172B2 (en) | Purification method of water-soluble dioxetane derivatives | |
| JP2838897B2 (en) | Recovery of rodan salt | |
| JPS5829294B2 (en) | Method for purifying isoleucine from a mixture of leucine and isoleucine | |
| BE707232A (en) | ||
| RU2184788C1 (en) | Method of rhenium desorption | |
| US2162655A (en) | Production of solid ammonium perphosphate | |
| JPH0375223A (en) | Recovery of indium | |
| SU1278299A1 (en) | Method of separating strontium and barium chlorides | |
| JP3835487B2 (en) | Rhodium purification method | |
| KR830001475B1 (en) | Tungsten Extraction Method from Alkali Metal Tungstate Solution | |
| US4343781A (en) | Decomposition of 2KCl.CuCl to produce cuprous chloride and potassium chloride | |
| JPH0233753B2 (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| LAPS | Cancellation because of no payment of annual fees |