CN104404569B - The preparation technology of high pure gold - Google Patents
The preparation technology of high pure gold Download PDFInfo
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- CN104404569B CN104404569B CN201410627740.8A CN201410627740A CN104404569B CN 104404569 B CN104404569 B CN 104404569B CN 201410627740 A CN201410627740 A CN 201410627740A CN 104404569 B CN104404569 B CN 104404569B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/20—Electrolytic production, recovery or refining of metals by electrolysis of solutions of noble metals
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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
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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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Materials Engineering (AREA)
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- Life Sciences & Earth Sciences (AREA)
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- Electrolytic Production Of Metals (AREA)
Abstract
The invention discloses the preparation technology of high pure gold, returns the three-level purifying techniques such as extraction by electrolysis with ion-exchange film liquid making, extraction and reduction, can disposably obtain more than 99.999% high pure gold.First using the thick gold of amberplex electrochemical dissolution technology dissolving, chlorauric acid solution is prepared into, realize one-level purification while liquid making；Composite extractant is added, is washed after isolating Gold-loaded organic phase, realizes two level purification；Gold-loaded organic phase after washing is stripped through electronation, completes three-level purification, more than 99.999% high pure gold is can obtain after the melting of gained bronze, ingot casting.Three-level purifying technique of the present invention is simple, and flow is short, and the strong adaptability of thick golden raw material, production efficiency is high, realizes the energy-saving and emission-reduction of production, it is easy to accomplish automated production, it is thus possible to produce great economic benefit and social benefit.
Description
Technical field
The present invention relates to the preparation technology of precious metal hydrometallurgy technical field, more particularly to high pure gold.
Background technology
High Purity Gold is more and more extensive due to its unique performance, application.In recent years, with electronics, aircraft industry it is quick
Development, the purifying technique of High Purity Gold have obtained quick development.Preparing the method for High Purity Gold mainly has chemical reduction method, solvent extraction
Follow the example of and the methods of electrorefining, but various technologies of preparing have its specific scope of application and pros and cons.Electrorefining is thick
Gold purification important production method, because its process stabilizing, it is easily-controllable, be easy to the advantages that mass production obtained most widely should
With, but electrorefining has to carry out repeatedly, the big efficiency of energy consumption is low；Extraction often will be extracted repeatedly, and pollution is larger,
Labor intensity is big, and production cycle length, cost are high；Traditional chemical reduction method hardly results in the gold of high-purity.
In addition, no matter use which kind of technology when preparing High Purity Gold, the liquid making of gold is essential step, traditional handicraft
Frequently with the molten golden method of chloroazotic acid, such as a kind of preparation methods of High Purity Gold of CN102925679, a kind of production High Purity Golds of CN103757246
Method, a kind of wet underwater welding High Purity Gold new technologies of CN102703691, be required to the flooding process of redundant and complicated, or use pottery
Porcelain film is electrolysed, and high with tank voltage, and resistance is high, and liquid temperature is high, production cycle length, the shortcomings such as current efficiency is low, such as
A kind of methods for preparing High Purity Gold of CN101985691.
The content of the invention
It is an object of the invention to：For preparing the problem of High Purity Gold is present in the prior art, monotechnics is avoided to repeat
The shortcomings that multipass ability output High Purity Gold, give full play to the advantage of three kinds of technologies, there is provided a kind of preparation technology of high pure gold.
The present invention is achieved by the following technical solutions：
The preparation technology of high pure gold, comprises the following steps：
Step S1, first, No. 2 of No. 1 gold or content more than 99.95% that the purity by raw material gold is 99.99% are golden
Gold ingot carries out tabletting, and obtained gold plaque (paper tinsel) is positioned in the anode basket of electrolytic cell after being cleaned with pure water；
Step S2, pours into electrolyte in electrolytic cell, and electrolyte uses anolyte (8mol/L) and catholyte (6mol/L)
Hydrochloric acid solution；
Step S3, switches on power, and carries out 1~2h of electrolysis, and the condition of electrolysis is 30 DEG C, tank voltage 5V, electric current 60A of temperature,
With 15 ± 2cm of pole span；
Step S4, treat that the gold dissolving in anode basket finishes, produce anolyte AuCl4 -Solution, turn off the power switch；
Step S5, anolyte is put into extraction reactor from the outlet at bottom of electrolytic cell, adds composite extractant and carry out
Extraction, is washed after isolating Gold-loaded organic phase with hydrochloric acid solution；
Step S6, chemical reducing agent is added in Gold-loaded organic phase after washing and return extraction, the bronze of gained is scrubbed,
Drying, melting, ingot casting can disposably obtain more than 99.999% high pure gold.
Preferably, the composite extractant in the step S5 is dibutyl carbitol (DBC) (DBC) and tributyl phosphate (TBD)
Mixture.
Preferably, process conditions are：
Composite extractant VDBC∶VTBD=4: 1；Compared to R: O/A=1: 1；
Extraction temperature：50℃；Rate of extraction：60s；Loading capacity：50g/LAu(III)；
Impurity cleaning solution：0.5mol/L hydrochloric acid solutions.
Preferably, the chemical reducing agent in the step S6 is sodium sulfite, in oxalic acid, ammonium oxalate, ascorbic acid
It is a kind of.
In summary, by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
The present invention compared with prior art, the three-level purifying technique such as film electrolysis dissolution, extraction and electronation of use, is kept away
The problem of having exempted from the high energy consumption poor efficiency of conventional electrolytic methods；Avoid chloroazotic acid it is molten golden when catch up with nitre to bring trivial operations, work
The situations such as bad environments, electrolysis with ion-exchange film technology is employed, integrate thick gold dissolving with purifying.Gold with trivalent gold from
Sub- form is retained in anolyte after entering solution, and partial impurities ion enters catholyte, real while gold dissolves liquid making
The one-level purification of gold is showed；The present invention use composite extractant, when compensate for using single DBC, because distribution ratio greatly and caused by
Back extraction it is difficult, and remove the deficiencies of not thorough using foreign ion during single TBP, played again respective advantage and both
Extraction ability is excellent in compared with highly acidity hydrochloric acid solution the characteristics of, single extraction process is only needed, is not required to carry out reextraction
Reach required ingot grade, metal recovery rate is effectively improved；In addition, the present invention uses electronation reverse-extraction method,
The purification process of gold is furthermore achieved that, has reached the set goal, to meet the needs of fields such as electronics and aviation.
Brief description of the drawings
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein：
Fig. 1 is the preparation technology schematic process flow diagram of the high pure gold of the present invention.
Embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive
Feature and/or step beyond, can combine in any way.
Any feature disclosed in this specification (including any accessory claim, summary and accompanying drawing), except non-specifically chatting
State, can alternative features equivalent by other or with similar purpose replaced.I.e., unless specifically stated otherwise, each feature
It is an example in a series of equivalent or similar characteristics.
As shown in figure 1, the preparation technology of high pure gold, comprises the following steps：
Step S1, first, No. 2 of No. 1 gold or content more than 99.95% that the purity by raw material gold is 99.99% are golden
Gold ingot carries out tabletting, and obtained gold plaque (paper tinsel) is positioned in electrolytic cell after being cleaned with pure water；
Step S2, pours into electrolyte in electrolytic cell, and electrolyte uses anolyte (8mol/L) and catholyte (6mol/L)
Hydrochloric acid solution；
Step S3, switches on power, and carries out 1~2h of electrolysis, and the condition of electrolysis is 30 DEG C, tank voltage 5V, electric current 60A of temperature,
With 15 ± 2cm of pole span；(primary purification of gold is completed while ion-exchange film method liquid making, because entering the gold in solution
It is positively retained in anolyte, impurity cationic enters catholyte to be separated with gold by amberplex.)
Step S4, the gold dissolving in groove to be electrolysed finish, and produce anolyte AuCl4- solution, is turned off the power switch；
Step S5, anolyte is moved into extraction reactor from the outlet at bottom of electrolytic cell, adds composite extractant and fill
Divide vibration, it is static to treat that solution is divided into two-phase, Gold-loaded organic phase is washed with hydrochloric acid solution, obtains the load gold after purification extraction
Organic phase；
Step S6, the solution after washing is being stirred continuously lower addition oxalic acid (or sodium sulfite, ammonium oxalate, ascorbic acid
In one kind) carry out reduction reextraction, obtain cake of gold precipitation, then with distillation water washing 5~6 times, drain, be put into drying box
In, ingot casting after 80~100 DEG C of drying, obtain the High Purity Gold that content is more than 99.999%.
The present invention uses electrolysis with ion-exchange film, extraction and chemical reduction method process integration, realizes liquid making and three-level carries
Pure continuous processing, the high pure gold that purity is more than 99.999% is disposably obtained.Compared with prior art, present invention process is set
Meter is smooth rationally to catch up with the complicated processes such as nitre, concentration when avoiding aqua regia dissolution, avoid using ceramic membrane and caused by tank voltage
Height, resistance is high, and liquid temperature is high, production cycle length, and the shortcomings such as current efficiency is low, execute-in-place environment is preferable, product quality stability
It height, can effectively reduce environmental pollution, improve production efficiency, realize the energy-saving and emission-reduction of production；Using composite extractant, compensate for
Using the deficiency of single extractant, respective advantage has been played again, has only needed single extraction process, is not required to carry out reextraction
Reach required ingot grade, metal recovery rate is effectively improved, it is thus possible to produces great economic benefit and society
Can benefit.
Particular embodiments described above, the purpose of the present invention, technical scheme and beneficial effect are carried out further in detail
Describe in detail it is bright, should be understood that the foregoing is only the present invention specific embodiment, be not intended to limit the invention.This
Invention expands to any new feature disclosed in this manual or any new combination, and any new method for disclosing or
The step of process or any new combination.
Claims (1)
1. the preparation technology of high pure gold, it is characterised in that the preparation technology carries out liquid making, tool using ion-exchange film method
Have the following steps：
Step S1, first, No. 1 gold or content that the purity by raw material gold is 99.99% are more than 99.95% No. 2 golden gold
Ingot carries out tabletting, and obtained gold plaque is positioned in the anode basket of electrolytic cell after being cleaned with pure water；
Step S2, electrolyte is poured into electrolytic cell, electrolyte does anolyte using 8mol/L hydrochloric acid, and 6mol/L hydrochloric acid is done
Catholyte；
Step S3, switches on power, and carries out 1~2h of electrolysis, and the condition of electrolysis is 30 DEG C, tank voltage 5V, electric current 60A of temperature, homopolarity
Away from 15 ± 2cm；
Step S4, treat that the gold dissolving in anode basket finishes, produce anolyte AuCl4 -Solution, turn off the power switch；
Step S5, anolyte is put into extraction reactor from the outlet at bottom of electrolytic cell, adds composite extractant and extracted,
Washed after isolating Gold-loaded organic phase with hydrochloric acid solution；
Step S6, chemical reducing agent is added in Gold-loaded organic phase after washing and return extraction, the bronze of gained is scrubbed, baking
Dry, melting, ingot casting can disposably obtain more than 99.999% high pure gold；
Composite extractant in the step S5 is a kind of oxygen-containing extractant of alcohols and a kind of mixture of phosphorus-contained extractant, specifically
For：Dibutyl carbitol (DBC) DBC and tributyl phosphate TBP mixture, process conditions are：Composite extractant VDBC∶VTBP=4: 1,
Extraction temperature：50 DEG C, rate of extraction：60s, loading capacity：50g/LAu；Chemical reducing agent in step S6 is sodium sulfite, grass
Acid is pressed, one kind in ascorbic acid.
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| CN201410627740.8A CN104404569B (en) | 2014-11-04 | 2014-11-04 | The preparation technology of high pure gold |
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| CN201410627740.8A CN104404569B (en) | 2014-11-04 | 2014-11-04 | The preparation technology of high pure gold |
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| CN104404569A CN104404569A (en) | 2015-03-11 |
| CN104404569B true CN104404569B (en) | 2018-02-23 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105887123A (en) * | 2016-05-04 | 2016-08-24 | 常州钇金环保科技有限公司 | Method for preparing PdCl2 |
| CN106868545A (en) * | 2017-01-12 | 2017-06-20 | 包小玲 | Normal pressure and temperature gold novel process for refining is accounted for without acid gas is low |
| CN108677029B (en) * | 2018-03-28 | 2020-07-07 | 贵研铂业股份有限公司 | Preparation method of high-purity gold regular particles for integrated circuit |
| CN110724973A (en) * | 2019-11-19 | 2020-01-24 | 安徽焦冲矿业有限公司 | Efficient environment-friendly high-purity gold preparation method |
| CN114231753A (en) * | 2021-12-21 | 2022-03-25 | 厦门金路通新材料有限公司 | Method for industrial clean production of high-purity gold |
| CN114934178B (en) * | 2022-06-21 | 2023-03-24 | 中国地质科学院郑州矿产综合利用研究所 | Method for recovering gold from gold smelting slag chloridizing roasting leacheate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1035321A (en) * | 1988-06-15 | 1989-09-06 | 中国有色金属工业总公司昆明贵金属研究所 | Method with composite extractant to produce high-pure gold |
| CN101985691A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for preparing high-purity gold |
-
2014
- 2014-11-04 CN CN201410627740.8A patent/CN104404569B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1035321A (en) * | 1988-06-15 | 1989-09-06 | 中国有色金属工业总公司昆明贵金属研究所 | Method with composite extractant to produce high-pure gold |
| CN101985691A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for preparing high-purity gold |
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