CN106367609B - A kind of thick golden vacuum refining method of purification - Google Patents

A kind of thick golden vacuum refining method of purification Download PDF

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Publication number
CN106367609B
CN106367609B CN201610965709.4A CN201610965709A CN106367609B CN 106367609 B CN106367609 B CN 106367609B CN 201610965709 A CN201610965709 A CN 201610965709A CN 106367609 B CN106367609 B CN 106367609B
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gold
thick
temperature
purification
refining method
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CN106367609A (en
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杨斌
邓勇
张丁川
徐宝强
熊恒
刘大春
郁青春
王飞
戴永年
曲涛
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00Obtaining noble metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/02Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The present invention relates to a kind of thick golden vacuum refining method of purifications, belong to metallurgical technology field.Thick gold is cut into small pieces first, it is placed in vacuum drying oven and is evacuated to 30~100Pa, being warming up to temperature is 1550 DEG C~1650 DEG C, and constant temperature distills 60min, period obtains distillation to 400 DEG C~800 DEG C by the temperature of circulating cooling water management condensing cover, after obtain residue.The thick golden vacuum refining method of purification overcomes the problems such as operating process in prior art is complicated, the production cycle is long, environmental pollution is big, at high cost, so that Ag, Zn, Cu, Ni impurity element effectively remove.

Description

A kind of thick golden vacuum refining method of purification
Technical field
The present invention relates to a kind of thick golden vacuum refining method of purifications, belong to metallurgical technology field.
Background technique
Gold is the metal that the mankind more early have found and utilize, and since it is rare, special and precious, is considered as five since ancient times First of gold, there is the title of the king of metal.It has high erosion-resisting stability;Good electric conductivity and thermal conductivity;Gold Atomic nucleus has the effective cross-section of larger capture neutron;There are various catalyst properties in the alloy of gold.In recent years, with integrated The development of circuit, the gold of the best superconductor as electronic integrated board, purity is higher, and data transmission efficiency is higher, at present The gold that space flight and aviation technically uses all is High Purity Gold.
Currently, most of gold manufacturing enterprises, thick gold refining purifying technique mainly based on wet process, has electrorefining to mention Pure, high-temp chlorination Refining, chloroazotic acid Refining and secondary chlorination-secondary reduction refining and purification process.
Baiyin Nonferrous Metal Group Co., Ltd.'s patent application 201310533395.7 discloses Wang Yinxiang, Feng Zhibing et al. A kind of method for improving gold precipitation grade in Gold electrolysis refinery practice is invented.The method is characterized in using thick golden plate as anode, Using proof gold plate as cathode, electrorefining is carried out by electrolyte of gold trichloride solution, the outer cover of the anode is equipped with by third Pocket shape diaphragm made of synthetic fibre, the mesh of diaphragm are 800~850 mesh.The cathode is made of following methods: being with thick golden plate Anode is electrolysed with titanium alloy sheet using gold trichloride solution as electrolyte, and in titanium alloy sheet two sides, precipitation is pure after a period of time Layer gold removes proof gold layer up to Gold electrolysis cathode plate.When preparing Gold electrolysis cathode plate, silver plate is replaced to make with titanium alloy sheet There is good corrosion resistance in the electrolytic solution, and be electrolysed since Titanium has good chemical stability for cathode Titanium alloy sheet surface is capable of forming the oxidation film of continuous dense uniform in journey, so that proof gold layer is easily peeled off so that golden starting sheet It makes easier.But since electrolysis technology condition requires height, golden backlog is big, high production cost, and uses in production process Concentrated acid, highly basic etc., so that production equipment seriously corroded, working environment is poor, and there are certain risk.Ministry of Metallurgical Industry Changchun is yellow The CN01100059.7 of golden research institute application disclose a kind of Amminochloride process of purifying gold its including the following steps: Nitric acid removal of impurities, filtration washing, chlorination leaching gold, filtration washing, golden reduction, filtration washing, golden melting.The method it is complicated for operation and The reagent that strong acid etc. has certain risk is used in production, and production environment is poor, there is certain limitation for large-scale promotion.
High-temp chlorination refining and purification process environmental pollution is big, and product quality is difficult to stably reaching standard, and operating process complicated difficult To grasp, it is desirable that the index of control is more, is not easy to realize that automation, scale are only suitable for small-scale production.Chloroazotic acid Refining It is most ancient refining and purification process, the production cycle is long, and environmental pollution is big, and has a large amount of liquid to need to handle.Therefore urgently New process high-efficient, investment is small, environmental pollution is small, easy to operate to be developed.Thick gold vacuum distillation refining mentions after study It is pure that there is good effect.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of thick golden vacuum refining method of purification.It should Thick gold vacuum refining method of purification overcomes that operating process in prior art is complicated, the production cycle is long, environmental pollution is big, at high cost etc. Problem, so that Ag, Zn, Cu, Ni impurity element effectively remove, the invention is realized by the following technical scheme.
A kind of thick golden vacuum refining method of purification is placed in vacuum drying oven the specific steps of which are as follows: thick gold is cut into small pieces first Be evacuated to 30~100Pa, be warming up to temperature be 1550 DEG C~1650 DEG C after, constant temperature distill 60min, during which pass through circulating cooling The temperature of water management condensing cover obtains distillation to 400 DEG C~800 DEG C, after obtain residue.
The mass percent containing gold is 90~95% in the thick gold, also includes Ag, Zn, Cu and Ni impurity.
The vacuum drying oven heating rate is 10 DEG C/min.
The beneficial effects of the present invention are: operation of the present invention process is simple, low energy consumption, imitates on environment almost without influence, removal of impurities Fruit is good, applied widely, easy to implement and industrialization promotion.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
The thick golden vacuum refining method of purification, the specific steps of which are as follows: first will thick gold (the slightly mass percent containing gold in gold It is 93.98%, also includes impurity A g2.25wt%, Zn0.3wt%, Cu3.454wt% and Ni0.205wt%) it is cut into small pieces, it is placed in true Be evacuated to 60Pa in empty furnace, with 10 DEG C/min heating rate be warming up to temperature be 1550 DEG C after, constant temperature distill 60min, during which Temperature by adjusting circulating cooling water management condensing cover obtains distillation to 800 DEG C, after obtain residue.
Residue obtained above mass percent golden after glow discharge mass spectroscopy detects is 99%, impure Ag0.000005wt%, Zn0.000599wt%, Cu0.88wt% and Ni0.036wt%.
Embodiment 2
The thick golden vacuum refining method of purification, the specific steps of which are as follows: first will thick gold (the slightly mass percent containing gold in gold It is 91.20%, also includes impurity A g3.06wt%, Zn0.5wt%, Cu2.89wt% and Ni2.35wt%) it is cut into small pieces, it is placed in vacuum 30Pa is evacuated in furnace, with 10 DEG C/min heating rate be warming up to temperature be 1600 DEG C after, constant temperature distill 60min, during which lead to Cross the temperature of circulating cooling water management condensing cover and obtain distillation to 400 DEG C, after obtain residue.
Residue obtained above mass percent golden after glow discharge mass spectroscopy detects is 99%, impure Ag0.000047wt%, Zn0.000517wt%, Cu0.62wt% and Ni0.046wt%.
Embodiment 3
The thick golden vacuum refining method of purification, the specific steps of which are as follows: first will thick gold (the slightly mass percent containing gold in gold It is 97.79%, also includes impurity A g1.25wt%, Zn0.3wt%, Cu0.454wt% and Ni0.205wt%) it is cut into small pieces, it is placed in true Be evacuated to 100Pa in empty furnace, with 10 DEG C/min heating rate be warming up to temperature be 1625 DEG C after, constant temperature distill 60min, during which Obtain distillation to 600 DEG C by the temperature of circulating cooling water management condensing cover, after obtain residue.
Residue obtained above mass percent golden after glow discharge mass spectroscopy detects is 99%, impure Ag0.000121wt%, Zn0.000429wt%, Cu0.18wt% and Ni0.040wt%.
Embodiment 4
The thick golden vacuum refining method of purification, the specific steps of which are as follows: first will thick gold (the slightly mass percent containing gold in gold It is 93.98%, also includes impurity A g2.25wt %, Zn0.3wt %, Cu3.454wt% and Ni0.205wt%) it is cut into small pieces, it is placed in 80Pa is evacuated in vacuum drying oven, with 10 DEG C/min heating rate be warming up to temperature be 1650 DEG C after, constant temperature distill 60min, the phase Between distillation obtained to 650 DEG C by the temperature of circulating cooling water management condensing cover, after obtain residue.
Residue obtained above mass percent golden after glow discharge mass spectroscopy detects is 99%, impure Ag0.00015wt%, Zn0.000617wt%, Cu0.37wt% and Ni0.082wt%.
Above the embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment party Formula can also be made without departing from the purpose of the present invention within the knowledge of a person skilled in the art Various change out.

Claims (1)

1. a kind of thick golden vacuum refining method of purification, it is characterised in that specific step is as follows: thick gold being cut into small pieces first, is placed in true It is evacuated to 30~100Pa in empty furnace, is warming up to after temperature is 1550 DEG C~1650 DEG C, constant temperature distills 60min, during which by following The temperature of ring cooling water control condensing cover obtains distillation to 400 DEG C~800 DEG C, after obtain residue;
The mass percent containing gold is 90~95% in the thick gold, also includes Ag, Zn, Cu and Ni impurity;
The vacuum drying oven heating rate is 10 DEG C/min.
CN201610965709.4A 2016-10-28 2016-10-28 A kind of thick golden vacuum refining method of purification Active CN106367609B (en)

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MX2023002015A (en) 2020-08-18 2023-04-11 Enviro Metals Llc Metal refinement.
CN112322904A (en) * 2020-10-12 2021-02-05 昆明鼎邦科技股份有限公司 Method for vacuum separation of gold, silver and copper alloy

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RU2082787C1 (en) * 1994-06-10 1997-06-27 Государственный научный центр вирусологии и биотехнологии "Вектор" Apparatus for separation of metals by distillation in vacuum
JP3725621B2 (en) * 1996-06-21 2005-12-14 同和鉱業株式会社 High-purity silver wire for recording or sound or image transmission
CN101560606B (en) * 2009-05-19 2012-02-08 昆明鼎邦科技有限公司 Deleading method through vacuum distillation of noble lead materials
CN101696469A (en) * 2009-10-29 2010-04-21 昆明理工大学 Method for separating multi-element alloy of lead, bismuth, gold, silver and copper
ES2733066T3 (en) * 2013-07-30 2019-11-27 Ikoi S P A Method for the separation of gold-silver alloys by vacuum distillation and device for its realization

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