CN106868545A - Normal pressure and temperature gold novel process for refining is accounted for without acid gas is low - Google Patents
Normal pressure and temperature gold novel process for refining is accounted for without acid gas is low Download PDFInfo
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- CN106868545A CN106868545A CN201710022240.5A CN201710022240A CN106868545A CN 106868545 A CN106868545 A CN 106868545A CN 201710022240 A CN201710022240 A CN 201710022240A CN 106868545 A CN106868545 A CN 106868545A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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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
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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
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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Abstract
Normal pressure and temperature gold novel process for refining is accounted for without acid gas is low the invention discloses one kind, electrolytic cell is isolated into anode region and cathodic region using anionic membrane, thick gold is used as anode, titanium net is used as negative electrode, anode region electrolyte is 10 200g/L hydrochloric acid and 10 30g/L sodium-chloride water solutions, cathodic region electrolyte is that the hydrochloric acid solution of 10 350g/L is electrolysed, in electrolytic process, in anode region, silver nitride precipitation is formed with the chlorion in solution, gold and other metal impurities discharge to form ion into the solution of anode region after silver electric discharge in thick gold.This method had both avoided the shortcoming that chloroazotic acid method or chloridising produce a large amount of harmful exhausts, electrolytic refining process is solved again and accounts for shortcoming more than pressure gold.Lower temperature of the overall production process below 50 DEG C is carried out, and solves the problems, such as that the hydrochloric acid in solution largely volatilizees at relatively high temperatures, while the gold in it also avoid solution is lost as acid gas is escaped.
Description
Technical field
The present invention relates to a kind of gold refining technology.
Background technology
The purpose of gold refining (purification) technique is exactly that the relatively low thick gold of taste containing gold is purified to higher degree.According to the people
With with different industrial uses, 99% or even 99.999% can be purified to.
Gold refining technology is with a long history, ancient times or even present folk art, usually using smelting process, using gold
The characteristics of not allowing oxidizable, various metal impurities are aoxidized in high temperature fused state, and slag making removal of impurities reaches the mesh for improving fineness of gold
's.
Gold refining is main by following several method in the prior art：
1) gold electrorefining：With thick gold to be refined as anode, and cover with anode, with proof gold plate or titanium plate as cloudy
Pole, as electrolyte, temperature passes to direct current electrolysis to the mixed solution with gold chloride and hydrochloric acid in 65-85 DEG C of scope.Electrolytic process
In, thick gold anode constantly dissolves, and silver falls in anode in silver nitride precipitation form.The metal impurities such as gold and copper, iron are with ion
State enters in electrolyte.Electrode potential gold ion higher (golden chlorine complex ion) is preferentially separated out in negative electrode, and electrode potential
The foreign ions such as relatively low copper, iron are stayed in the electrolytic solution, so as to reach the golden purpose for various impurity separate.
2) gold chloroazotic acid method refining：Thick Jinsui River to be refined is quenched efflorescence or compressing tablet, chloroazotic acid (salt is used in dissolution reactor
Acid+nitric acid) the thick gold of dissolving.Silver forms silver nitride precipitation, and the impurity such as gold and copper, iron is dissolved in wang aqueous solution with ionic condition
In, and nitric acid is reduced into oxides of nitrogen gas discharge.It is filtered to remove silver chlorate.Reducing agent is added to reduce containing golden wang aqueous solution.Electricity
Electrode potential gold ion higher (golden chlorine complex ion) is reduced into bronze preferential, and the impurity such as the relatively low copper of electrode potential, iron
Ion is stayed in the solution, so as to reach the golden purpose for various impurity separate.
3) gold chloridising refining：By thick golden high-temperature fusion to be refined, the gold that will be melted with water under high pressure in pulverizer
It is pulverized into bronze.Bronze is added in the dissolution reactor for preparing hydrochloric acid, is added sodium chlorate or is passed through chlorine, and bronze is dissolved.Silver
Silver nitride precipitation is formed, the impurity such as gold and copper, iron is dissolved in wang aqueous solution with ionic condition, and sodium chlorate or chlorine are a part of
It is reduced into chlorion, superfluous chlorine discharge (sodium chlorate is also to resolve into chlorine).It is filtered to remove silver chlorate.It is molten containing golden chloroazotic acid
Liquid adds reducing agent to reduce.Electrode potential gold ion higher (golden chlorine complex ion) is preferentially reduced into bronze, and electrode potential compared with
The foreign ions such as low copper, iron are stayed in the solution, so as to reach the golden purpose for various impurity separate.
Although the purpose that above-mentioned three kinds of methods can separate gold with various impurity, the above method all exists certain
Shortcoming, wherein：
1) gold electrorefining has the disadvantages that：
(1) to account for pressure amount relatively more for gold：Electrolyte will remain the concentration containing gold more than 80g/L in electrolytic refining process,
Just can guarantee that the quality (for example meeting 99.99% grade of Shanghai gold trade institute standard) of negative electrode gold product.It is every for one
Its 100 kilograms of workshop of gold of refining, will account for the gold of 30 kilograms of pressure all the time in electrolyte.The thick gold of anode is in electrolysis
Can not be completely dissolved, more than 5% anode scrap is also left at the end of electrolysis, to return to cast anode again.So the stream of electrolysis
To remain that larger amount of gold accounts for pressure in journey, increase the circulating fund amount of manufacturing enterprise.
(2) pollution of hydrochloric acid acid gas：To ensure the quality that negative electrode gold is separated out, Gold electrolysis will be carried out at 65-85 DEG C, higher
Temperature cause the volatile quantity of hydrochloric acid in electrolyte also than larger, influence workshop condition, also result in certain environmental pollution.
(3) golden loss ratio is more：At a temperature of 65-85, liquid containing Gold electrolysis is with the volatilization of hydrochloric acid, and some are vaporific
Escaped also with acid gas containing golden small water droplet.Although the gold in these acid gas can be reclaimed with major part, reclaimed from acid gas flue
During there is also gold loss.
2) shortcoming of gold chloroazotic acid method refining：
(1) pollution of nitrogen oxide containing gas：During aqua regia dissolution gold, nitric acid is reduced into oxides of nitrogen gas discharge.Nitrogen
Oxide is a kind of harmful gas, is one of important component of atmosphere pollution.Although method that can be using treatment is collected,
Pollution to environment cannot be avoided thoroughly, while also considerably increasing the cost of enterprise.
(2) pollution of hydrochloric acid acid gas：The molten gold reaction of chloroazotic acid will be carried out at 85-95 DEG C, and temperature higher causes electrolyte
The volatile quantity of middle hydrochloric acid also than larger, influences workshop condition, also results in certain environmental pollution.
(3) golden loss ratio is more：At a temperature of 85-95, with the discharge and the volatilization of hydrochloric acid of oxides of nitrogen gas,
Some are vaporific to escape containing golden small water droplet also with acid gas.Although the gold in these acid gas can be reclaimed with major part, from acid gas
The loss of gold is there is also in flue in removal process.
3) shortcoming of gold chloridising refining：
(1) pollution of chlorine：During chlorinating dissolution gold, superfluous chlorine is discharged from solution.Chlorine is a kind of to human body
Harmful hazardous gas, pollutes atmospheric environment.Although method that can be using treatment is collected, being to the pollution of environment cannot be thorough
What bottom avoided, while also increasing the cost of enterprise.
(2) pollution of hydrochloric acid acid gas：The molten gold reaction of chlorination will be carried out at 75-85 DEG C, and temperature higher causes electrolyte
The volatile quantity of middle hydrochloric acid also than larger, influences workshop condition, also results in certain environmental pollution.
(3) golden loss ratio is more：At a temperature of 85-95, with the discharge and the volatilization of hydrochloric acid of chlorine, some are vaporific
Containing golden small water droplet also with acid gas escape.Although the gold in these acid gas can be reclaimed with major part, returned from acid gas flue
The loss of gold is there is also during receipts.
Gold electrorefining is the technique of comparative maturity, and in the planned economy era, the gold refining enterprise of China all adopts
Use electrolytic refining process.But its maximum shortcoming is that the ratio of electrolyte and anode scrap the occupancy gold in production procedure is higher,
If mass producing the circulating fund, it is necessary to more.
Gold not only has many industrial uses, it may have the critical function of investment and wealth deposit.As China is national
Expanding economy, the growth of people's wealth, China has become maximum golden production state and country of consumption in the world.The gold of China
The production scale of refining have developed rapidly, and with the rapid concentration at economy and finance center, and gold refining enterprise was from former
The situation in various regions mine is dispersed in, coastal economically developed metropolis is gradually focused on.Gold refining belongs to chemical metallurgy class,
With the increasingly reinforcement of state treatment environmental pollution policy, the environmental issue that the industry faces becomes increasingly conspicuous.The new green of exploitation
The gold refining technique of environmental protection, benefits the nation and the people.
The content of the invention
The gold novel process for refining that the present invention is combined using electrochemistry instant gold high and oxalic acid reduction metallographic, both avoids king
Water law or chloridising produce the shortcoming of a large amount of harmful exhausts, electrolytic refining process is solved again and accounts for shortcoming more than pressure gold.It is all raw
Lower temperature of the product process below 50 DEG C is carried out, and solves the problems, such as that the hydrochloric acid in solution largely volatilizees at relatively high temperatures,
The gold that it also avoid simultaneously in solution is lost as acid gas is escaped.
To reach above-mentioned purpose, the technical solution adopted by the present invention is：
It is a kind of to account for normal pressure and temperature gold novel process for refining without acid gas is low, comprise the following steps：
S1：Thick gold is pre-processed, the surface area of the thick gold of raw material is increased；
S2：Electrolytic cell is isolated into anode region and cathodic region using anionic membrane, used as anode, titanium net is used as the moon for thick gold
Pole, anode region electrolyte is 10-200g/L hydrochloric acid and 10-30g/L sodium-chloride water solutions, and cathodic region electrolyte is 10-350g/L
Hydrochloric acid solution；
S3：Start electrolysis, wherein electrolyte temperature is 10-50 DEG C；
S4：After the completion of electrolysis, by the filtering of anode region solution, the precipitated impurities such as silver chlorate are stayed in filter residue, wash filter residue；
S5：In gold-containing solution feeding reduction reactor after filtering reduce and obtain reducing bronze；
S6：Reduction bronze drying is cast into gold ingot.
In electrolytic process, in anode region, silver nitride precipitation is formed with the chlorion in solution after the silver electric discharge in thick gold,
Gold and other metal impurities (being referred to as Me) electric discharge form ion (complex ion) and enter in the solution of anode region.Due to cathodic coating
Cut-off is acted on, and these metal ions can not enter cathodic region, and in the continuous cumulative rises in anode region, gold ion concentration is 10-
500g/L。
Anode region electrode reaction：
Au-3e-=Au3+
Ag++Cl-=AgCl ↓
Me-ne-=Men+
In cathodic region, hydrogen ion discharge separates out hydrogen.Superfluous chlorion passes through cathodic coating, supplement the chlorine of anode region from
Son.
Cathodic region electrode reaction：
2H++2e-=H2 ↑
Pernicious gas will not be produced in whole electrolytic process.
As of the present invention without a kind of low preferred scheme for accounting for normal pressure and temperature gold novel process for refining of acid gas, described step
It is thin slice or particle after thick gold is pre-processed in rapid S1, it is therefore an objective to increase the surface area of the thick gold of raw material, make the electrochemical molten of next step
Gold can be carried out quickly, meet the demand of large-scale production.
As of the present invention without a kind of low preferred scheme for accounting for normal pressure and temperature gold novel process for refining of acid gas, described step
During thick golden clothes enter titanium basket in rapid S2, titanium basket is connected to the anode output end of rectifier as anode, and wherein titanium basket is POROUS TITANIUM basket.
As of the present invention without a kind of low preferred scheme for accounting for normal pressure and temperature gold novel process for refining of acid gas, described step
Cathode/anode current density is 300-5000A/m in electrolytic process in rapid S32。
As of the present invention without a kind of low preferred scheme for accounting for normal pressure and temperature gold novel process for refining of acid gas, described step
Reduced using oxalic acid in rapid S5, according to the purity requirement to product, adjust the pH value of gold-containing solution, the electricity of control oxalic acid reduction
Position, obtains the reduction bronze of 99-99.999%.
Chemical equation：2H[AuCl4]+3H2C2O4=2Au+8HCl+6CO2↑
Pernicious gas is not produced in the reduction process, in addition, tail washings is by proper treatment, hydrochloric acid therein can be reclaimed again
Utilize.
Beneficial effect：
1. primary benefits of the invention are environmental benefits, are produced without waste gas in whole gold refining process.And it is domestic existing
Several gold refining technologies having：Electrorefining, chloroazotic acid refining, chlorination refining, all different degrees of waste gas that has are produced.In environmental protection
Under the increasingly strict situation of policy, new gold refining construction project in some cities is difficult to be examined by environmental protection, and some are former
Some refining enterprises have to move out of urban area, or can only go into operation at night.Present invention nothing in gold refining process
Waste gas is produced, and while social enviroment protection benefit is created, also meets environmental requirement for the normal production of gold refining enterprise is provided
Guarantee.
2. the loss of gold refining technology gold of the invention is fewer.With electrolysis (more than 65 degree of electrolyte temperature), king
Water law (more than 85 degree of molten golden reaction temperature), chloridising (more than 75 degree of molten golden reaction temperature) are compared, the hydrometallurgy of this technique
Part is all carried out in lower temperature (less than 50 degree), and the acid volatilizing loss containing gold solution is fewer.
3. compared with electrolysis, in gold refining technology of the invention gold account for pressure ratio example it is fewer.Such as production daily
The gold electrorefining workshop of 100 kilograms of scale, accounts for about 40-100 kilograms of the gold (electrolysis of pressure in electrolyte and anode scrap
It is different that current density difference accounts for pressure amount).This technique accounts for pressure under equal production scale in molten golden slag and secondary reduction bronze
Gold about 0.5-3 kilograms, with chloroazotic acid method and chloridising in account for pressure gold amount it is essentially identical.
Specific embodiment
Embodiment 1
It is a kind of to account for normal pressure and temperature gold novel process for refining, 5 kilograms of gold of every batch of refining without acid gas is low
(1) 5 kilograms of gold are pressed into the thin slice that thickness is 0.01-0.1mm using milling train, are completed in 30min.
(2) electrolytic cell is isolated into anode region and cathodic region using anionic membrane, gold plaque is loaded into porous anode titanium basket
In, the anode region of electrolytic cell is put into, the anode output end of rectifier is connected to, negative electrode is titanium net.Anode region electrolyte is hydrochloric
150g/L, sodium chloride 10g/L, the hydrochloric 200g/L of cathodic region electrolyte.Start rectifier and start electrolysis, Faradaic current control exists
520-550A, decomposition voltage is 3-10V, electrolysis time 240min.
(3) anode region electrolyte is filtered in vacuum filter, is washed, the time is 15min.
(4) by the electrolyte after filtering in reduction reactor, pH is adjusted, adds oxalic acid reduction, the time is 30min.
(5) reduction bronze is used into pure water in vacuum filter, then is dried in an oven, drying time is 30min.
(6) bronze founding will be reduced into ingot using intermediate frequency or Efco-Northrup furnace, the time is 30min.
Plus pilot process, a refining for batch can be completed within 480min (8h).
Embodiment 2
30 kilograms of gold of every batch of refining
(1) 30 kilograms of gold are pulverized into the small of diameter 1mm or so using high-temperature fusion-high pressure water quenching type ingot efflorescence machine
Particle.
(2) electrolytic cell is isolated into anode region and cathodic region using anionic membrane, gold plaque is loaded into porous anode titanium basket
In, the anode region of electrolytic cell is put into, the anode output end of rectifier is connected to, negative electrode is titanium net.Anode region electrolyte is hydrochloric
100g/L, sodium chloride 20g/L, the hydrochloric 300g/L of cathodic region electrolyte.Start rectifier and start electrolysis, Faradaic current control exists
820-850A。
(3) anode region electrolyte is filtered in vacuum filter, is washed.
(4) by the electrolyte after filtering in reduction reactor, pH is adjusted, adds oxalic acid reduction, the time is 50min.
(5) reduction bronze is used into pure water in vacuum filter, then is dried in an oven, drying time is 30min.
(6) bronze founding will be reduced into ingot using intermediate frequency or Efco-Northrup furnace, the time is 30min.
Although being illustrated to embodiments of the present invention in specification, these implementation methods are intended only as prompting,
Should not limit protection scope of the present invention.It is equal that various omission, substitution, and alteration are carried out without departing from the spirit and scope of the present invention
Should be comprising within the scope of the present invention.
Claims (5)
1. one kind accounts for normal pressure and temperature gold novel process for refining without acid gas is low, it is characterised in that comprise the following steps：
S1：Thick gold is pre-processed, the surface area of the thick gold of raw material is increased；
S2：Electrolytic cell is isolated into anode region and cathodic region using anionic membrane, used as anode, titanium net is used as negative electrode, sun for thick gold
Polar region electrolyte is 10-200g/L hydrochloric acid and 10-30g/L sodium-chloride water solutions, and cathodic region electrolyte is the salt of 10-350g/L
Acid solution；
S3：Start electrolysis, wherein electrolyte temperature is 10-50 DEG C；
S4：After the completion of electrolysis, by the filtering of anode region solution, the precipitated impurities such as silver chlorate are stayed in filter residue, wash filter residue；
S5：In gold-containing solution feeding reduction reactor after filtering reduce and obtain reducing bronze；
S6：Reduction bronze drying is cast into gold ingot.
It is 2. according to claim 1 to account for normal pressure and temperature gold novel process for refining without acid gas is low, it is characterised in that：It is thick in step S1
It is thin slice or particle after gold pretreatment.
It is 3. according to claim 1 to account for normal pressure and temperature gold novel process for refining without acid gas is low, it is characterised in that：It is thick in step S2
Golden clothes enter in titanium basket, and titanium basket is connected to the anode output end of rectifier as anode, and wherein titanium basket is POROUS TITANIUM basket.
It is 4. according to claim 1 to account for normal pressure and temperature gold novel process for refining without acid gas is low, it is characterised in that：Electricity in step S3
Cathode/anode current density is 300-5000A/m in solution preocess2。
It is 5. according to claim 1 to account for normal pressure and temperature gold novel process for refining without acid gas is low, it is characterised in that：Adopted in step S5
Reduced with oxalic acid.
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| CN201710022240.5A CN106868545A (en) | 2017-01-12 | 2017-01-12 | Normal pressure and temperature gold novel process for refining is accounted for without acid gas is low |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111299607A (en) * | 2020-04-13 | 2020-06-19 | 紫金矿业集团黄金冶炼有限公司 | Preparation method of 5N-level micron conductive gold ball |
| CN112144077A (en) * | 2019-06-26 | 2020-12-29 | 西南科技大学 | Electro-chlorination extraction method of gold in gold-containing material |
| US11319613B2 (en) | 2020-08-18 | 2022-05-03 | Enviro Metals, LLC | Metal refinement |
| CN114959755A (en) * | 2021-02-24 | 2022-08-30 | 中国科学院上海硅酸盐研究所 | Device and method for efficiently preparing hydrogen and silver halide |
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| CN1442498A (en) * | 2003-04-11 | 2003-09-17 | 山东黄金集团有限公司焦家金矿 | Method of crude gold purification |
| CN104404569A (en) * | 2014-11-04 | 2015-03-11 | 常州钇金环保科技有限公司 | Preparation technology of high purity gold |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1442498A (en) * | 2003-04-11 | 2003-09-17 | 山东黄金集团有限公司焦家金矿 | Method of crude gold purification |
| CN104404569A (en) * | 2014-11-04 | 2015-03-11 | 常州钇金环保科技有限公司 | Preparation technology of high purity gold |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112144077A (en) * | 2019-06-26 | 2020-12-29 | 西南科技大学 | Electro-chlorination extraction method of gold in gold-containing material |
| CN112144077B (en) * | 2019-06-26 | 2022-07-15 | 西南科技大学 | Method for extracting gold from gold-containing material by electro-chlorination |
| CN111299607A (en) * | 2020-04-13 | 2020-06-19 | 紫金矿业集团黄金冶炼有限公司 | Preparation method of 5N-level micron conductive gold ball |
| CN111299607B (en) * | 2020-04-13 | 2022-06-07 | 紫金矿业集团黄金冶炼有限公司 | Preparation method of 5N-level micron conductive gold ball |
| US11319613B2 (en) | 2020-08-18 | 2022-05-03 | Enviro Metals, LLC | Metal refinement |
| US11578386B2 (en) | 2020-08-18 | 2023-02-14 | Enviro Metals, LLC | Metal refinement |
| CN114959755A (en) * | 2021-02-24 | 2022-08-30 | 中国科学院上海硅酸盐研究所 | Device and method for efficiently preparing hydrogen and silver halide |
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Application publication date: 20170620 |