KR100939577B1 - Chemistry processing of high purity gold from low grade gold scraps - Google Patents
Chemistry processing of high purity gold from low grade gold scraps Download PDFInfo
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Abstract
본 발명은 저순도 금을 이용한 초고순도 금의 제조방법에 관한 것으로, 금의 함량이 60%∼75%인 저순도 금을 99.999%(이하, 5N) 이상의 초고순도 금으로 제조하고 이를 기존 고순도방법보다 간단하고 용이하며 경제적으로 대량 정제함을 목적으로 한다.The present invention relates to a method for producing ultra-high purity gold using low purity gold, and to produce a low-purity gold with a gold content of 60% to 75% of ultra high purity gold of 99.999% (hereinafter, 5N) or more and the existing high purity method It is aimed at simpler, easier and economical mass purification.
본 발명에 의한 저순도 금을 이용한 초고순도 금의 제조방법은, 저순도 금을 왕수(Aqua Regia)용액에 용해하여 냉각여과한 금 함유용액에 수산화나트륨(NaOH)를 이용하여 불순물로 존재하는 철을 제거하는 단계와; 상기 불순물이 제거된 금함유 왕수(Aqua Regia)용액에 용매추출제인 디에틸렌 글리콜 디엔부틸 에테르(Diethylene Glycol Di-n-butyl Ether=(CH3(CH2)3OCH- 2)2)O=218.33)와 반응시켜 금이온을 추출한 후 염산(HCl)으로 세정한 금 함유 유기상에 암모니아수(NH4OH)와 반응시켜 풀미네이팅 골드(Fulminating Gold)(Au2O33NH3)를 제조하는 단계와; 그리고, 상기 제조된 풀미네이팅 골드(Fulminating Gold)에 암모니아수(NH4OH)와 환원제인 하이드라진(N2H4) 또는 과산화수소수와 동시 반응시켜 초고순도 금 파우더(Au Powder)를 제조하는 단계를 포함하여 이루어진다.According to the present invention, a method for producing ultra high purity gold using low purity gold is obtained by dissolving low purity gold in an aqua regia solution and using iron hydroxide (NaOH) as an impurity in a gold-containing solution that has been cooled and filtered. Removing the; Diethylene Glycol Di-n-butyl Ether = (CH 3 (CH 2 ) 3 OCH - 2 ) 2 ) O = 218.33 as a solvent extractant in the gold-containing Aqua Regia solution from which the impurities were removed. ) To extract gold ions, and then to react with ammonia water (NH 4 OH) in a gold-containing organic phase washed with hydrochloric acid (HCl) to prepare the pulminating gold (Au 2 O 3 3 NH 3 ) and ; The ultrapure gold powder (Au Powder) is prepared by simultaneously reacting ammonia water (NH 4 OH) and reducing agent hydrazine (N 2 H 4 ) or hydrogen peroxide solution to the prepared pulminating gold. It is made to include.
초고순도금, 99.999% 금, 5Nine GOLD, 반도체용 금, 고순도금제조방법 Ultra High Purity, 99.999% Gold, 5Nine Gold, Semiconductor Gold, High Purity Plating
Description
본 발명은 초고순도 금의 제조방법에 관한 것으로서, 더욱 상세하게는 금의 함량이 60%∼75%의 저순도 금을 왕수(Aqua Regia)에 용해한 후 초고순도의 가장 큰 불순물로 존재하는 철을 수산화나트륨(NaOH)를 이용하여 제거하고 금 함유 유기상에 암모니아수(NH4OH)를 반응시켜 풀미네이팅 골드(Fulminating Gold)(Au2O33NH3)를 제조한 후 제조된 Fulminating Gold에 NH4OH와 환원제인 하이드라진(N2H4) 또는 과산화수소수와 동시 반응시켜 5N 이상의 초고순도 금으로 제조할 수 있는 저순도 금을 이용한 초고순도 금의 제조방법에 관한 것이다.The present invention relates to a method for producing ultra-high purity gold, and more particularly, after melting low-purity gold having a gold content of 60% to 75% in aqua regia, iron which is present as the largest impurity of ultra high purity. Removed with sodium hydroxide (NaOH) and reacted with ammonia water (NH 4 OH) on the gold-containing organic phase to produce a fully pulminating gold (Au 2 O 3 3 NH 3 ) NH 4 in the pulminating gold prepared The present invention relates to a method for preparing ultra-high purity gold using low purity gold which can be produced with ultra-high purity gold of 5N or more by simultaneously reacting with OH and a reducing agent hydrazine (N 2 H 4 ) or hydrogen peroxide solution.
일반적으로 산업용 금(金)은 금 도금업이나 인쇄회로기판, 인쇄업에 사용되고, 반도체 제조업이나 의약품과 같은 정밀분야에는 고순도의 금이 사용되고 있다. 상기 금은 그 순도가 99.995% 이상이어야만 한다.In general, industrial gold is used for gold plating, printed circuit boards, and printing industries, and high purity gold is used in precision fields such as semiconductor manufacturing and pharmaceuticals. The gold must be at least 99.995% pure.
초고순도 금(99.999%이상)의 종래 제조기술은 국내에서 아직 발표된 적이 없 는 것으로 사료되며, 고순도 금(99.99%) 정제방법으로는 다음과 같은 기술이 있다.Conventional manufacturing techniques of ultra high purity gold (99.999% or more) have not been announced in Korea yet. The high purity gold (99.99%) refining method includes the following techniques.
예컨대 종래 기술에 의한 고순도 금 정제방법은 85%∼98%의 지금(地金)을 왕수에 용해한 후 여과하여 불순물인 염화은을 제거하고 2차 불순물을 제거하기 위하여 염화금산용액에 유기 용매인 디부틸케비톨(DI-BUTHYL-CAPITOL)을 가하여 금이온을 용매추출하여 불순물을 제외하고 금이온만을 유기상으로 상분리한 후, 금이 함유된 유기상을 1.5N 농도의 염산으로 역추출한 금이온을 증발, 건고하여 금을 일차적으로 회수하고 회수된 금을 다시 진한 황산에 용해하여 그 용액을 200℃로 유지하여 아황산가스를 발생시켜 금을 선택적으로 환원, 석출시킨후 이를 여과, 세척 및 건조하여 순도가 99.995% 이상인 고순도금을 정제하는 방법과 상기의 일부 방법으로 지금을 용해하여 화학적 환원석출시켜 1차 정제한후 양극으로 주조한후 전기분해하여 정제하는 전해정련방법이 보고되었다.For example, the high-purity gold refining method according to the prior art dissolves 85% to 98% of Geum in aqua regia and then removes silver chloride as an impurity and dibutyl as an organic solvent in a gold chloride solution to remove secondary impurities. Gold ions were added to the solvent by adding DI-BUTHYL-CAPITOL to separate the gold ions into the organic phase except for impurities, and then the gold ions obtained by reverse extraction of the gold-containing organic phase with 1.5 N hydrochloric acid were evaporated and dried The gold is recovered first, and the recovered gold is dissolved again in concentrated sulfuric acid and the solution is maintained at 200 ° C. to generate sulfurous acid gas. The gold is selectively reduced and precipitated, and then filtered, washed and dried to obtain 99.995% purity. Electrolytic refining refinement by dissolving now and chemically precipitating by dissolving now by the above method of purifying high purity plating and some of the above method, casting it by anode, and then electrolytically purifying The law was reported.
그러나, 전술한 바와 같은 종래 기술에 의한 고순도 금 정제방법은 기존 왕수작업후 금이 함유된 유기상을 1.5N 농도의 염산으로 역추출한 금이온을 증발, 건고하여 금을 일차적으로 회수하고, 회수된 금을 다시 진한 황산에 용해하여 그 용액을 200℃로 유지하여 아황산가스를 발생시켜 금을 선택적으로 환원, 석출시킨후 이를 여과, 세척 및 건조하는 등의 일련정제공정이 복잡하고 금함유 유기상을 진한 황산에 용해하여 그 용액을 200℃로 유지하여 아황산가스를 발생시켜야 하는 등의 신속하고 용이하지 못하며 대용량의 처리를 할 수 없다는 문제점이 있어 현재 국내에서는 적용되지 않고 있다. 또한 전해정련방법은 불순물로 함유되어 있는 은이 양극표면에 염화은의 피막이 형성되어 부동태현상을 초래하므로 다량의 전력소모와 원료 금의 함량이 98.5% 이상이 되어야만 고순도금의 제조가 원활하다는 문제점이 보고되었다.However, the above-described high-purity gold purification method according to the prior art evaporates and dries the gold ions obtained by reverse extraction of the organic phase containing gold with hydrochloric acid at a concentration of 1.5 N after the conventional aqua reclamation, and recovers the gold first. Is dissolved in concentrated sulfuric acid and the solution is maintained at 200 ° C to generate sulfurous acid gas to selectively reduce and precipitate gold, which is then filtered, washed and dried. Dissolves in and maintains the solution at 200 ° C to generate sulfurous acid gas, such as quick and easy, there is a problem that can not be a large-capacity treatment is not currently applied in Korea. In addition, in the electrolytic refining method, a silver chloride film is formed on the surface of the anode, resulting in a passivation phenomenon. Therefore, it has been reported that a large amount of power consumption and the content of raw gold should be more than 98.5% to facilitate the manufacture of high purity plating. .
본 발명은 상기와 같은 문제점을 해결하기 위한 것으로, 금의 함량이 60%∼75%의 저순도 금을 간단하고 용이하며 경제적인 방법을 통해 5N(99.999%) 이상의 초고순도 금을 제조할 수 있는 저순도 금을 이용한 초고순도 금의 제조방법을 제공하려는데 그 목적이 있다.The present invention is to solve the above problems, it is possible to manufacture ultra-high purity gold of 5N (99.999%) or more by a simple, easy and economical method of low purity gold with a gold content of 60% to 75% The purpose of the present invention is to provide a method for producing ultra-pure gold using low-purity gold.
전술한 바와 같은 목적을 달성하기 위한 본 발명에 의한 저순도 금 함유물을 왕수(Aqua Regia)용액에 첨가하여 90~100°C 에서 30분간 가열한 후 실온(25°C) 까지 냉각한 다음 수산화나트륨(NaOH)를 첨가하여 불순물로 존재하는 철을 제거하여 불순물이 제거된 금함유 왕수(Aqua Regia)용액을 얻는 단계와;
상기 불순물이 제거된 금함유 왕수(Aqua Regia) 용액에 용매추출제인 디에틸렌 글라이콜 디엔부틸 에테르(Diethylene Glycol Di-n-butyl Ether= (CH3 (CH2)3 O CH- 2)2)O)와 30분간 반응시켜 금이온을 분리한 후 염산(HCl)을 이용하여 30분간 세정하고 8mole의 암모니아수와 1:1의 부피비로 90~100°C 에서 30분간 교반하면서 풀미네이팅 골드(Fulminating Gold)를 제조하는 단계와;
상기 제조된 풀미네이팅 골드(Fulminating Gold)에 8mole의 암모니아수와 1:1의 부피비로 교반시키고 동시에 환원제인 하이드라진(N2H4) 또는 과산화수소(H2O2)와 반응시켜 금파우더(Gold Powder)를 제조하는 단계와;
상기 제조된 금파우더(Gold Powder)를 질산(HNO3)용액에 45~55°C 에서 25~35분간 반응시켜 극미량의 불순물을 제거한 후 여과하여 금 파우더(Gold Powder)를 회수한 후 도가니에 넣고 전기로 등을 이용하여 1200°C 이상까지 용융시켜 초고순도의 금을 정련하는 단계를 포함하여 이루어진 것을 특징으로 한다.The low purity gold content according to the present invention for achieving the above object is added to an aqua regia solution, heated at 90-100 ° C. for 30 minutes, cooled to room temperature (25 ° C.), and then hydrated. Adding sodium (NaOH) to remove iron as an impurity to obtain a gold-containing Aqua Regia solution from which impurities are removed;
Diethylene Glycol Di-n-butyl Ether = (CH 3 (CH 2 ) 3 O CH - 2 ) 2 ) as a solvent extractant in the gold-containing Aqua Regia solution from which the impurities are removed After reacting with O) for 30 minutes to separate the gold ions, it was washed with hydrochloric acid (HCl) for 30 minutes, and stirred with 90 moles of ammonia water of 8 mole at 90-100 ° C for 30 minutes. Gold);
Gold powder (Gold Powder) by stirring with a volume ratio of 1: 1 with ammonia water of 8 mole in the prepared pulminating gold (Fulminating Gold) and at the same time reacted with hydrazine (N 2 H 4 ) or hydrogen peroxide (H 2 O 2 ) as a reducing agent Preparing);
The prepared gold powder was reacted with nitric acid (HNO 3 ) solution at 45-55 ° C for 25-35 minutes to remove extremely small amounts of impurities, followed by filtration to recover the gold powder and put it in the crucible. Melting to 1200 ° C or more using an electric furnace, characterized in that comprising a step of refining ultra-high purity gold.
본 발명에 의한 저순도 금을 이용한 초고순도 금의 제조방법에 의하면, 가장 큰 불순물로 존재하는 철을 수산화나트륨(NaOH)을 이용하여 간단히 제거하고, 금 함유 유기상에 암모니아수(NH4OH)를 반응시켜 풀미네이팅 골드(Fulminating Gold)를 제조하며, 제조된 풀미네이팅 골드(Fulminating Gold)에 암모니아수(NH4OH)와 환원제인 하이드라진(N2H4) 또는 과산화수소수와 동시 반응시켜 금의 함량이 60%∼75%의 저순도 금을 99.999% 이상의 초고순도 금으로 제조함으로써 작업속도의 향상 및 공정의 간편화를 통해 종래의 방법에 비해 비용적인 면과 금의 순도향상 면에서 현저한 효과가 있다.According to the method for producing ultra high purity gold using low purity gold according to the present invention, iron, which is the largest impurity, is simply removed using sodium hydroxide (NaOH), and ammonia water (NH 4 OH) is reacted with a gold-containing organic phase. To produce pulminating gold, and simultaneously react with fluorinated gold with ammonia water (NH 4 OH) and reducing agent hydrazine (N 2 H 4 ) or hydrogen peroxide solution. Since the 60% to 75% low purity gold is made of 99.999% or more ultra-high purity gold, it has a remarkable effect in terms of cost and improvement of gold purity compared to conventional methods through the improvement of the working speed and the simplification of the process.
첨언하면, 이로 인해 기존 금함유 유기상을 진한 황산에 용해하여 그 용액을 200℃로 유지하여 아황산가스를 발생시켜야 하는 등의 신속하고 용이하지 못하며 대용량의 정제처리를 할 수 없어 국내에 적용되지 않고 있다는 문제점과 아울러 전해정련방법은 금함량이 98.5% 이상이 되어야만 원활하다는 문제점을 동시에 해결할 수 있으며 또한 작업공정을 단순화하여 제조시간이 짧고 용이하게 99.999% 이상의 반도체용 및 의료용 초고순도 금을 제조할 수 있는 경제적효과와 수입대체할 수 있는 효과가 있다.Incidentally, due to this, the existing gold-containing organic phase was dissolved in concentrated sulfuric acid, and the solution was maintained at 200 ° C. to generate sulfurous acid gas. In addition to the problem, the electrolytic refining method can solve the problem that the gold content should be more than 98.5% at the same time. In addition, it is possible to manufacture the ultra high purity gold for semiconductor and medical use more than 99.999% by simplifying the work process. There is an economic effect and a substitution effect on imports.
도 1은 본 발명에 따른 저순도 금을 이용한 초고순도 금의 제조방법의 공정도로서, 이하, 본 발명에 의한 구체적인 공정을 설명한다.1 is a process chart of a method for producing ultra-high purity gold using low-purity gold according to the present invention. Hereinafter, a specific process according to the present invention will be described.
(S10) 철 불순물 제거(S10) Iron Impurity Removal
60%∼75%의 저순도 금 함유물을 왕수(Aqua Regia)용액(HCl:HNO3=3:1)에 첨가하여 90∼100℃의 상온에서 30분간 가열하여 용해하고 실온(25℃)까지 냉각하여 여과한 용액에 3 Mole의 수산화나트륨(NaOH)을 첨가하면서 pH 농도를 3.5로 조절하면 철 불순물(Goethite, FeOOH)이 침전되므로 이를 여과하여 제거하고 pH가 3.5로 조절된 금 함유 용액에 기 첨가한 수산화나트륨(NaOH)과 동일한 Mole량 만큼의 HCl을 첨가하여 pH를 0으로 조절한다.A low purity gold content of 60% to 75% was added to an Aqua Regia solution (HCl: HNO 3 = 3: 1), dissolved by heating for 30 minutes at a temperature of 90-100 ° C to room temperature (25 ° C). Adjusting the pH to 3.5 while adding 3 Mole of sodium hydroxide (NaOH) to the cooled and filtered solution precipitates iron impurities (Goethite, FeOOH), so it is filtered and removed. The pH is adjusted to 0 by adding the same amount of HCl as the added sodium hydroxide (NaOH).
(S20) Fulminating Gold(Au2O33NH3)제조(S20) Manufacture of Fulminating Gold (Au 2 O 3 3NH 3 )
상기 철 불순물이 제거된 금함유 왕수(Aqua Regia)용액에 용매추출제인 디에틸렌 글리콜 디엔부틸 에테르(Diethylene Glycol Di-n-butyl Ether=(CH3(CH2)3OCH- 2)2)O=218.33;이하 DGDE)를 금 함량 50g당 1L를 첨가하여 30분간 반응시켜 유기상 금 이온를 분리하고 2M의 염산(HCl)을 이용하여(HCl:DGDE=2:1) 금을 함유한 DGDE를 30분간 세정하고 분리한다. Diethylene Glycol Di-n-butyl Ether = (CH 3 (CH 2 ) 3 OCH − 2 ) 2 ) O = as a solvent extractant in the gold-containing Aqua Regia solution from which the iron impurities were removed 218.33; hereinafter DGDE) is added to 1L per 50g of gold content and reacted for 30 minutes to separate organic phase gold ions and washed DGDE containing gold for 30 minutes using 2M hydrochloric acid (HCl) (HCl: DGDE = 2: 1) And separate.
상기 분리된 금 함유 유기상에 암모니아수(25%, 8M)와 1:1의 부피비로 상온에서 30분 100rpm의 속도로 교반하면서 반응시키고 여과하면 노란색 침전물의 풀미 네이팅 골드(Fulminating Gold)가 제조된다.The separated gold-containing organic phase was reacted with ammonia water (25%, 8M) at a volume ratio of 1: 1 at room temperature with stirring at a rate of 100 rpm for 30 minutes, and filtered to prepare a pulminating gold of a yellow precipitate.
Diethylene Glycol Di-n-butyl Ether=(CH3(CH2)3OCH- 2)2)O=218.33Diethylene Glycol Di-n-butyl Ether = (CH 3 (CH 2 ) 3 OCH - 2 ) 2 ) O = 218.33
1) DEGE-AuCl4 Reacion formula1) DEGE-AuCl 4 Reacion formula
2) Fulminating gold formation2) Fulminating gold formation
(S30) Gold powder 제조(S30) Gold powder manufacturing
풀미네이팅 골드(Fulminating Gold)(Au2O33NH3)로 제조된 금에 암모니아수(NH4OH)(25%, 8M)를 상기 S20에서 첨가한 양만큼 투입하여 교반시키고 동시에 환원제(N2H4 or H2O2)를 금의 함량비 만큼 천천히 첨가하면 갈색의 금 용액이 제조되며 이를 20분간 정치하여 여과하면 초고순도 금 파우더(Gold powder)가 제조된다. Ammonia water (NH 4 OH) (25%, 8M) was added to the gold made of Fulminating Gold (Au 2 O 3 3NH 3 ) by the amount added in S20 and stirred, and at the same time, a reducing agent (N 2 When H 4 or H 2 O 2 ) is slowly added as the content ratio of gold, a brown gold solution is prepared. When the mixture is filtered for 20 minutes, ultra-high purity gold powder is produced.
Au reduction processAu reduction process
상기 금 파우더(Gold powder)를 질산(HNO3)용액(Gold 1kg/질산 1L)에 45∼55℃에서 25~35분간 반응시켜 극미량의 불순물을 제거한 후 여과하여 금 파우더(Gold powder)를 회수한 후 Quartz 도가니에 넣고 전기로 등을 이용하여 1200℃이상까지 용융시켜 반도체용 초고순도의 금을 정련한다. The gold powder was reacted with nitric acid (HNO 3 ) solution (Gold 1kg / nitric acid 1L) at 45-55 ° C. for 25-35 minutes to remove trace impurities, followed by filtration to recover gold powder. After that, it is put into a quartz crucible and melted to 1200 ℃ or higher using an electric furnace to refine ultra-high purity gold for semiconductors.
이하, 본 발명의 구체적인 실시예들을 상세히 설명한다.Hereinafter, specific embodiments of the present invention will be described in detail.
[실시예 1]Example 1
저순도 금(시중 14k, 18k) 25g을 0.5L의 왕수(Aqua Regia)용액에 용해한 후 원자흡광분석법(Atomic Absorption Spectrophotometer,이하 AAS)를 이용해 정량 분석한 결과가 아래의 표와 같다.25g of low-purity gold (14k, 18k) was dissolved in 0.5L of Aqua Regia solution and quantitatively analyzed by Atomic Absorption Spectrophotometer (AAS).
상기 성분조성을 갖는 저순도금 25g을 분말화하여 왕수(Aqua Regia)용액 0.5L에 넣고 100℃까지 30분간 완전히 용해하고 실온(25℃)까지 냉각시켜 여과한 용액에 3M의 수산화나트륨(NaOH)을 첨가하면서 pH를 3.5로 조절하면 불순물인 Geothite (FeOOH)가 침전되고 이를 여과하여 제거한 다음 상기 NaOH 투입량 만큼의 염산(HCl)(10M)을 첨가하여 왕수(Aqua Regia)용액의 pH를 "0"이하로 조절하였다. 25 g of the low-purity plating powder having the above composition was pulverized and placed in 0.5 L of Aqua Regia solution, completely dissolved for 30 minutes to 100 ° C., cooled to room temperature (25 ° C.), and 3M sodium hydroxide (NaOH) was added to the filtered solution. While adjusting the pH to 3.5, the impurity Geothite (FeOOH) precipitates and is filtered and removed, and then the pH of the Aqua Regia solution is lowered to "0" or less by adding hydrochloric acid (HCl) (10M) as the NaOH input amount. Adjusted.
상기 철 불순물이 제거된 왕수(Aqua Regia)용액에 DGDE 0.5L와 30분간 교반시켜 금이온을 DGDE에 흡장시켜 분리하고 2M의 염산(HCl)을 1L 첨가하여 30분간 세정하고 분리하였다.The iron impurity (Aqua Regia) solution was removed by stirring for 0.5 minutes with DGDE 0.5L DGDE was separated by occluding gold ions in DGDE, washed with 30M by adding 1L of 2M hydrochloric acid (HCl).
상기 분리된 금 함유 유기상에 암모니아수(NH4OH, 25%, 8M) 0.5L를 실온에서 30분 100rpm의 속도로 교반, 반응시키고 여과하여 노란색 침전물의 풀미네이팅 골드(Fulminating Gold)를 제조하였다.0.5 L of ammonia water (NH 4 OH, 25%, 8M) was separated, stirred, and reacted at a rate of 100 rpm for 30 minutes at room temperature to prepare a pulminating gold of a yellow precipitate.
상기 풀미네이팅 골드(Fulminating Gold)로 제조된 금에 암모니아수 0.5L를 투입하면서 교반시키고 여기에 환원제(N2H4 or H2O2) 25ml를 천천히 첨가하면 갈색의 금 파우더(Powder)가 제조되고 이를 20분간 정치, 여과하여 고순도 금 파우더(Gold powder)를 제조하였다. 0.5L of ammonia water was added to the gold produced by the pulminating gold (Fulminating Gold) while stirring, and slowly adding 25 ml of reducing agent (N 2 H 4 or H 2 O 2 ) to the brown gold powder (Powder) was prepared. This was allowed to stand for 20 minutes and filtered to prepare a high purity gold powder.
상기 금 파우더(Gold powder)를 3M의 질산(HNO3) 0.5L에 50℃에서 30분간 반응시켜 여과하고 Quartz 도가니에 넣은 다음 전기로를 이용하여 1200℃이상까지 용융시켜 초고순도의 금을 정련하였고 정제 제조된 금의 순도는 ICP-MS 분석 결과 99.99975%의 순도였다. 이때, 금 파우더(Gold Powder) 중의 불순물로는 구리(Cu) 45ppb가 함유되어 있었다.The gold powder was reacted with 0.5 ml of 3M nitric acid (HNO 3 ) at 50 ° C. for 30 minutes, filtered, placed in a quartz crucible, and then melted to 1200 ° C. or more using an electric furnace to refine ultra-high purity gold. The purity of the gold produced was 99.99975% pure by ICP-MS analysis. At this time, 45 ppm of copper (Cu) was contained as an impurity in the gold powder.
[실시예 2]Example 2
저순도금 50g을 1L의 왕수(Aqua Regia)에 용해한 후 AAS를 이용해 정량 분석한 결과가 아래의 표와 같다.After dissolving 50g of low-purity plating in 1L of aqua regia, the result of quantitative analysis using AAS is shown in the table below.
상기 성분조성을 갖는 저순도금을 실시예 1과 동일한 방법과 상대적 비율의 시약첨가로 실시한 결과, 금 파우더(Gold Powder) 중의 불순물로는 구리(Cu) 90ppb가 함유되어 있어 99.99978%의 순도를 나타냈다.As a result of the low purity plating having the above composition, the same method as in Example 1 and the addition of reagents in relative proportions showed that the impurities in the gold powder contained 90 ppb of copper (Cu), indicating a purity of 99.99978%.
[실시예 3]Example 3
저순도금 100g을 2L의 왕수(Aqua Regia)에 용해한 후 AAS를 이용해 정량 분석한 결과가 아래의 표와 같다.After dissolving 100g of low purity gold in 2L of aqua regia, the result of quantitative analysis using AAS is shown in the table below.
상기 성분조성을 갖는 저순도금을 실시예 1과 같은 동일한 방법과 상대적 비율의 시약첨가로 실시한 결과, 금 파우더(Gold Powder) 중의 불순물로는 Cu 450ppb가 함유되어 있어 99.9994%의 순도를 나타냈다.As a result of the low purity plating having the above composition, the same method as in Example 1 and the addition of reagents in relative proportions showed that the impurities in the gold powder contained 450 ppb, resulting in a purity of 99.9994%.
[실시예 4]Example 4
저순도금 21g을 0.5L의 왕수(Aqua Regia)용액에 용해한 후 AAS를 이용해 정량 분석한 결과가 아래의 표와 같다.After dissolving 21g of low-purity plating in 0.5L Aqua Regia solution, the result of quantitative analysis using AAS is shown in the table below.
상기 성분조성을 갖는 저순도금을 실시예 1과 같은 동일한 방법과 상대적 비율의 시약첨가로 실시한 결과, 금 파우더(Gold Powder) 중의 불순물로는 백금(Pt) 95ppb, 팔라듐(Pd) 4ppb가 함유되어 있어 99.9993%의 순도를 나타냈다.As a result of low purity plating having the above composition, the same method as in Example 1 and the addition of reagents in relative proportions, the impurities in the gold powder contained 95ppb of platinum (Pt) and 4ppb of palladium (Pd). Purity of% is indicated.
[실시예 5]Example 5
저순도금 10g을 0.2L의 왕수(Aqua Regia)용액에 용해한 후 AAS를 이용해 정량 분석한 결과가 아래의 표와 같다.After dissolving 10g of low purity plating in 0.2L of Aqua Regia solution, the result of quantitative analysis using AAS is shown in the table below.
상기 성분조성을 갖는 저순도금을 실시예 1과 같은 동일한 방법과 상대적 비율의 시약첨가로 실시한 결과, Gold Powder 중의 불순물로는 구리(Cu) 47ppb가 함유되어 있어 99.9993%의 순도를 나타냈다.As a result of low purity plating having the above composition, the same method as in Example 1 and the addition of reagents in relative proportions showed that the impurities in the gold powder contained 47 ppb of copper (Cu), indicating a purity of 99.9993%.
도 1은 본 발명에 따른 저순도 금을 이용한 초고순도 금의 제조공정도.1 is a manufacturing process of ultra-high purity gold using low-purity gold according to the present invention.
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| JPS6056030A (en) * | 1983-09-08 | 1985-04-01 | Nippon Mining Co Ltd | Method for recovering high purity gold |
| JPS63128136A (en) * | 1986-11-17 | 1988-05-31 | Tanaka Kikinzoku Kogyo Kk | Refining method for au |
| JPS63128135A (en) | 1986-11-17 | 1988-05-31 | Tanaka Kikinzoku Kogyo Kk | Refining method for au |
| JPH11229053A (en) | 1998-02-20 | 1999-08-24 | Sumitomo Metal Mining Co Ltd | Production of high purity gold |
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| JPS6056030A (en) * | 1983-09-08 | 1985-04-01 | Nippon Mining Co Ltd | Method for recovering high purity gold |
| JPS63128136A (en) * | 1986-11-17 | 1988-05-31 | Tanaka Kikinzoku Kogyo Kk | Refining method for au |
| JPS63128135A (en) | 1986-11-17 | 1988-05-31 | Tanaka Kikinzoku Kogyo Kk | Refining method for au |
| JPH11229053A (en) | 1998-02-20 | 1999-08-24 | Sumitomo Metal Mining Co Ltd | Production of high purity gold |
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