KR20090106067A - Precious metal collection method from scrap metals by dental technician - Google Patents
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- KR20090106067A KR20090106067A KR20080031561A KR20080031561A KR20090106067A KR 20090106067 A KR20090106067 A KR 20090106067A KR 20080031561 A KR20080031561 A KR 20080031561A KR 20080031561 A KR20080031561 A KR 20080031561A KR 20090106067 A KR20090106067 A KR 20090106067A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/06—Chloridising
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/205—Treatment or purification of solutions, e.g. obtained by leaching using adducts or inclusion complexes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
Description
본 발명은 치기공소 부산물인 폐금으로부터 금, 백금, 팔라듐 등의 귀금속을 신속하고 순도 높게 회수하는 방법에 관한 것이다. The present invention relates to a method for quickly and with high purity recovery of precious metals such as gold, platinum and palladium from waste gold which is a by-product of dental laboratories.
주지된 바와 같이 치기공소에서는 부산물인 폐금이 발생하는데, 이러한 폐금은 전체가 금으로 된 것이 아니라 여러 가지 금속성분이 혼합된 것이므로 이러한 폐금으로부터 필요한 성분을 순도 높게 회수하는 방안이 요구됨은 당연한 것이다.As is well known, waste gold, which is a by-product, is generated in the dental laboratories. Since such waste gold is not made of gold but is a mixture of various metals, it is natural that a high-purity recovery method is required.
종래 일반적인 회수방법에 의하면, 시간이 많이 소요되어 금과 백금 및 팔라듐까지 회수를 하려면 1주일 정도가 소요되는 단점이 있었고, 회수된 귀금속의 순도가 높지 않고 과정도 매우 복잡하여 회수에 의한 원가가 크게 상승하는 등 효율적인 회수작업이 이루어지지 않았던 것이다.According to the conventional general recovery method, it takes a long time to recover to gold, platinum, and palladium, which takes about one week. The purity of the recovered precious metal is not high and the process is very complicated, resulting in large cost. There was no efficient recovery work, such as a rise.
상기한 문제점을 감안하여 안출한 본 발명은 매우 효율적으로 금과 백금 및 팔라듐을 순차적으로 회수하는 방법을 제공하되, 회수에 소요되는 시간을 크게 단축하고 회수율과 순도를 향상시켜 매우 경제적이고 생산적인 회수가 이루어지도록 함을 목적으로 하는 것이다. The present invention devised in view of the above problems provides a method for recovering gold, platinum, and palladium sequentially in a very efficient manner, greatly reducing the time required for recovery and improving the recovery rate and purity, very economical and productive recovery The purpose is to make it happen.
본 발명은 반응시간을 줄이기 위해 폐금에 은을 합금하는 공정과 질산에 화학반응 시키는 공정을 실시한 다음, 왕수와 이루산소다 등을 이용하여 파우더 형태의 금을 회수하는 공을 실시하고, 아연반응으로 백금, 팔라듐 스폰지를 얻고 다시 왕수로 용해시키고 암모니아로 백금과 팔라듐을 분해하며 염화암모늄을 투여하여 백금 파우더를 생성시킴으로써 백금을 회수하는 공정과, 상기에서 남은 암모니아수 여액에 염산을 투여하여 팔라듐결정체를 얻음으로써 팔라듐을 회수하는 공정으로 이루어짐을 특징으로 한다. In order to reduce the reaction time, the present invention performs a process of alloying silver with waste gold and a process of chemically reacting with nitric acid, and then performing a ball for recovering powdered gold using aqua regia and soda isorate, followed by zinc reaction. Obtained platinum and palladium sponge, dissolve it again with aqua regia, decompose platinum and palladium with ammonia, and administer platinum solution by administering ammonium chloride to recover platinum. It characterized by consisting of a process for recovering palladium.
이러한 본 발명의 방법에 의하면 은이 합금된 상태로 질산처리되고 금과 백금이 파우더 상태가 되도록 한 다음에 왕수처리를 하게 되므로 매우 신속한 시간에 회수를 가능하게 해 주며, 회수되는 금속의 순도가 향상되는 효과도 있게 된다. According to the method of the present invention, the silver is nitrified in the alloyed state and the gold and platinum are powdered and then treated with aqua regia, which enables recovery at a very quick time and improves the purity of the recovered metal. It also works.
또한 백금을 회수하는 과정에서도 암모니아수를 이용하여 백금에게 불용성 착염반응을 일으키게 하고 파라듐은 흡수하는 작용을 하게 함으로써 이 또한 백금 의 회수에 소요되는 시간을 크게 단축하여 결국 3일 내지 4일 만에 금과 백금 및 팔라듐을 모두 회수할 수 있게 되므로 생산성을 크게 향상시키게 되는 효과가 있다. In addition, in the process of recovering platinum, by using ammonia water, platinum causes an insoluble complexing reaction, and paradium absorbs it, thereby greatly reducing the time required for the recovery of platinum. Since it is possible to recover both platinum and palladium has the effect of greatly improving the productivity.
이하 본 발명에 의한 방법을 순서에 의해 상세히 살펴보면 다음과 같다.Looking at the method according to the invention in detail as follows.
도 1은 본 발명에 의한 공정순서도, 도 2는 금 회수 공정도, 도 3은 백금 회수 공정도이다. 1 is a process flowchart according to the present invention, FIG. 2 is a gold recovery process diagram, and FIG. 3 is a platinum recovery process diagram.
은 혼합 합금 제조Silver mixed alloy manufacturing
우선 폐금을 수집하여 폐금 1: 은(Ag) 3의 비율(중량비)로 합금을 한다. First, the waste gold is collected and alloyed with the ratio (weight ratio) of waste 1: silver (Ag) 3.
이에 따라 합금된 금속은 금(Au) , 팔라듐(Pd) , 백금(Pt) , 구리(Cu), 은(Ag), 니켈(Ni)이 함유된 상태의 고체 합금덩어리 상태가 된다.Accordingly, the alloyed metal is in the state of a solid alloy mass containing gold (Au), palladium (Pd), platinum (Pt), copper (Cu), silver (Ag), and nickel (Ni).
이와 같은 합금을 먼저 실시하는 이유는 기존 폐금을 짧은 시간에 반응을 주기 위해서이다. The reason why such an alloy is first performed is to give an existing waste gold reaction in a short time.
질산반응Nitric acid reaction
합금덩어리를 질산(HNO3)에 화학 반응을 시킨다.The alloy mass is chemically reacted with nitric acid (HNO 3 ).
이러한 공정에 의하면 질산에 의해 고체(파우더)상태인 금과 백금, 그리고 액체상태인 구리, 은 및 팔라듐으로 분해되는 상태가 된다. According to this process, nitric acid decomposes into solid (powder) gold and platinum, and liquid copper, silver and palladium.
상기 금과 백금이 파우더 상태가 되므로 금속 상태일 때보다 반응속도가 빠르게 된다.Since the gold and platinum are in the powder state, the reaction rate is faster than in the metal state.
금(Au) 회수Au recovery
상기 질산(HNO3)에 염산(HCl)을 1:3의 비율로 혼합하여 왕수반응이 일어나도록 한다.Hydrochloric acid (HCl) is mixed with nitric acid (HNO 3 ) in a ratio of 1: 3 to cause aqua regia.
이러한 반응은 다음과 같다. This reaction is as follows.
H2NO3+3HCl→Cl2+NOCl+2H2O →Na2+Cl_ H 2 NO 3 + 3HCl → Cl 2 + NOCl + 2H 2 O → Na2 + Cl _
→ N2↑+O2 _ --->발생기 산소→ N2 ↑ + O 2 _ ---> Generator Oxygen
이러한 과정을 거치면 바닥에는 염화은(AgCl)이 백색 불용성 착염상태의 고체가 침전되고, 나머지는 염화금(AuCl_), 염화백금(PtCl_), 염화팔라듐(PdCl_), 염화구리(CuCl_) 등은 액체상태로 남는다.Through this process, silver chloride (AgCl) is precipitated with white insoluble complex salt, and the rest is gold chloride (AuCl _ ), platinum chloride (PtCl _ ), palladium chloride (PdCl _ ) and copper chloride (CuCl _ ). The back remains in a liquid state.
상기에서 고체상태인 염화은을 여과하여 별도의 회수공정으로 회수토록 하고, 나머지의 액체에 아루산소다를 첨가하면, 금(Au) 파우더가 생성되어 침전되고, 다시 금 파우더를 여과로 분리하여 용해 및 냉각하면 목적물의 하나인 금을 덩어리 상태로 회수하게 되는 것이다.The silver chloride in the solid state is filtered to be recovered by a separate recovery process, and when sodium arusate is added to the remaining liquid, gold (Au) powder is formed and precipitated, and the gold powder is separated by filtration to dissolve and cool. If you do, you will recover the gold, one of the targets in a lump.
상기에서 여과된 금 파우더는 질산, 황산, 염산 순으로 정제하여 불순물을 제거하면 더욱 순도 높은 금을 얻을 수 있으며, 정제시 단계별로 증류수를 사용하여 PH를 최대한 중성으로 만들어야 할 것이다.The filtered gold powder is purified in the order of nitric acid, sulfuric acid, hydrochloric acid to remove impurities to obtain a higher purity gold, and PH should be made as neutral as possible using distilled water in each step during purification.
백금(platinum( PtPt )회수)collection
상기 금 회수공정에 이어서 또는 공지된 금 회수공정에 의해 금 파우더를 여과하고 나머지 Pt, Pd, Cu, Ni로 이루어진 용액에서 백금을 회수할 수 있게 된다. Following the gold recovery process or by a known gold recovery process, the gold powder can be filtered and platinum can be recovered from the remaining solution consisting of Pt, Pd, Cu, and Ni.
상기 금 회수공정에서 얻어진 용액 또는 공지된 금 회수공정에 의해 남은 용액에 아연(Zn)으로 환원반응을 주어 백금·팔라듐 이온을 반금속 상태인 스폰지(sponge) 형태로 얻을 수 있게 된다.The solution obtained in the gold recovery process or the remaining solution by a known gold recovery process is subjected to a reduction reaction with zinc (Zn) to obtain platinum and palladium ions in the form of a semimetal sponge.
Ptcl_ Pdcl_ + Zn --> H2PtCl4 H2PdCl4 Ptcl _ Pdcl _ + Zn-> H 2 PtCl 4 H 2 PdCl 4
상기에서 얻어진 스폰지형태의 파우더를 여과하여 걸러내고 여액을 폐기하며, 여과된 스폰지는 다시 왕수에 용해시킨다.The sponge-like powder obtained above is filtered off and the filtrate is discarded, and the filtered sponge is again dissolved in aqua regia.
왕수에 용해된 상태의 백금과 팔라듐에 암모니아수(NH4OH)를 첨가하게 되면, 암모니아수에 의해 용액상태의 백금에게 불용성 착염반응이 일어나게 되고 팔라듐은 흡수하는 작용을 한다. 따라서 백금이 파우더 형태로 침전되고 팔라듐은 용액상태로 유지된다. When ammonia water (NH 4 OH) is added to platinum and palladium dissolved in aqua regia, insoluble complex salt reaction occurs to solution platinum by ammonia water, and palladium absorbs palladium. Thus, platinum precipitates in powder form and palladium remains in solution.
상기에서 백금 파우더를 여과하여 걸러내고 여액은 이후의 팔라듐을 회수하는 공정에 이용토록 하며, 걸러진 백금파우더는 다시 왕수에 용해시키고 용해된 왕수를 가열하여 최대한 농축시킨다.The filtered platinum powder is filtered in the above, and the filtrate is used for the process of recovering the subsequent palladium, and the filtered platinum powder is dissolved again in aqua regia and concentrated by heating the dissolved aqua regia.
농축된 용액에 염화암모늄(NH4Cl)을 투입함으로써 노란 결정체 즉 백금파우더를 생성하게 된다.Ammonium chloride (NH 4 Cl) is added to the concentrated solution to produce yellow crystals, that is, platinum powder.
H2PtCl6 + 2NH4Cl → (NH4)2PtCl6 형성H 2 PtCl 6 + 2 NH 4 Cl → (NH 4 ) 2 PtCl 6 formation
여기서 생성된 백금 파우더는 여과하여 20% 염화암모늄(NH4Cl) 수용액으로 충분히 세척을 한 다음, 붕사 코팅을 한 후 용해하여 목적물인 백금을 얻을 수 있게 된다.The platinum powder produced here is filtered and sufficiently washed with 20% ammonium chloride (NH 4 Cl) aqueous solution, and then subjected to borax coating to dissolve to obtain the target platinum.
팔라듐(Palladium ( PdPd ) 회수) Recovery
상기 백금 회수 공정에서 백금 파우더를 회수하고 남은 팔라듐 용액을 이용하여 팔라듐을 회수하는데, 염산(HCl)을 투여하여 팔라듐 결정체를 얻을 수 있게 된다.The platinum powder is recovered in the platinum recovery process, and the palladium is recovered using the remaining palladium solution. Thus, palladium crystals can be obtained by administering hydrochloric acid (HCl).
PdCl_ + HCl --> (NH2)2PdCl2 형성PdCl _ + HCl-> (NH 2 ) 2 PdCl 2 formation
생성된 팔라듐 파우더는 여과하여 증류수에 충분히 세척을 한 후 붕사 코팅을 한 후 용해하여 목적물인 팔라듐을 얻을 수 있다.The resulting palladium powder may be filtered and washed sufficiently in distilled water and then coated with borax to dissolve to obtain a target palladium.
도 1은 본 발명에 의한 전체 제조공정을 나타낸 순서도1 is a flow chart showing the entire manufacturing process according to the present invention
도 2는 본 발명의 금 회수 공정을 도시한 공정도2 is a process chart showing a gold recovery process of the present invention
도 3은 본 발명의 백금 회수 공정을 도시한 공정도Figure 3 is a process diagram showing the platinum recovery process of the present invention
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KR101579498B1 (en) | 2015-02-24 | 2015-12-22 | (주) 유천테크 | Method for recovering palladium of waste pastes containing palladium |
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KR101426518B1 (en) * | 2012-10-08 | 2014-08-05 | 한국지질자원연구원 | Method for Recovering Precious Metals from Printed Circuit Boards Scrap of End-of-Life Mobile Phones |
KR101579498B1 (en) | 2015-02-24 | 2015-12-22 | (주) 유천테크 | Method for recovering palladium of waste pastes containing palladium |
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CN113528849B (en) * | 2021-06-02 | 2022-12-23 | 云南滇金投资有限公司 | Method for extracting refined gold from palladium-silver-containing alloy gold |
KR102498447B1 (en) * | 2022-09-22 | 2023-02-10 | 노상균 | Method for extracting palladium from palladium-containing stainless steel |
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