CN101328541A - Gold wet purification process - Google Patents
Gold wet purification process Download PDFInfo
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- CN101328541A CN101328541A CNA2008100319628A CN200810031962A CN101328541A CN 101328541 A CN101328541 A CN 101328541A CN A2008100319628 A CNA2008100319628 A CN A2008100319628A CN 200810031962 A CN200810031962 A CN 200810031962A CN 101328541 A CN101328541 A CN 101328541A
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- gold
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- oxalic acid
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to a process for purifying gold by the wet method. Firstly, aqua fortis is used to remove silver; secondly, nitric acid is used to remove impurities such as bismuth and copper, etc.; the separation is performed by filtering; in the richly contained gold solution, the gold is reduced to gold powder deposited by an oxalic acid reducing agent with strong reducibility, and the impurities such as platinum, the bismuth and the copper, which are reduced simultaneously, are redissolved by nitric acid added later and enter the solution, and the solution is subjected to the filtering separation to obtain pure gold powder; and the pure gold powder is made to be ingot-shaped by fushion casting, and the finished gold ingots with a gold content of 99.99 percent are obtained. In the invention, the reduction reaction is made by oxalic acid at a low temperature, so that the process of the invention has the advantages of not causing environmental pollution, favorability for the heath of operators, lowering cost, shortening the period and obvious economic and social benefits.
Description
Technical field
The present invention relates to precious metal and purify, specifically, is a kind of gold wet purification process.
Background technology
Gold is as a kind of precious metal, and gold has that exploitation is difficult for, cost of winning is high, good physical property is arranged, and shows as the fusing point height, reach 1064.43 degree Celsius, gold is not easy fusing, and density is big, be 19.31 gram/cubic centimetres (18 ℃ time), toughness and ductility are good, and very the property led is strong.The gold output of Chinese last year rises to the high point of 276 tons set a record, and rose 12% than 2006, and the output in South Africa is 272 tons.In the period of 2000 to 2007, price of gold rises to more than 850 dollars from about 270 dollars every ounce, created the beginning of the year in 2008 1033.9 dollars every ounce all-time high again, but global gold mining amount has descended 6.7%, it is imperative to strengthen comprehensive recovery and improve the gold added value.
At present, processing contains the gold and silver material following several method of employing usually:
The melt chlorination process, promptly about 1150 ℃, melting materials capable leads to chlorine then under this temperature, make silver wherein change silver chloride into, volatilization enters flue dust and reclaims, and is electrolyzed to produce proof gold behind the golden ingot casting, the aqua regia dissolution gold, with ferrous sulfate reduction back founding, the electrolysis proof gold will contain the gold and silver material and mix an amount of silver again, be electrolyzed to produce proof gold and fine silver again.This method finally will be passed through electrolytic process, just can produce proof gold, and the production cycle is long, and it is many to overstock the gold amount, and the electrolyzer investment is many, complicated operation, and scattered gold is more in the production process, difficult management.The general employing of electrolytic process worked continuously, and the enterprise few to output can only be interrupted production, reduced plant factor, increased cost.
Wet separation gold and silver method mostly is to adopt the chloroazotic acid extract technology, restores cake of gold with solid oxalic acid, makes proof gold after founding.Leached mud reduces with yellow soda ash, decomposes the gold and silver alloy with nitric acid again, uses zinc dust precipitation silver then.This method is separated the process of gold and silver and has been saved electrolytic process, has improved work efficiency, but has shown through production practice, and the used chloroazotic acid amount of this method is big, is the operation of heating with the oxalic acid reduction, produces and emits bubble in a large number, and long and contaminate environment of operational cycle awaits improving.
With the immediate prior art of the present invention be the application for a patent for invention CN87105051A on April 27th, 1988, the isolating novel method of a kind of gold and silver is disclosed, this method adopts three sections adverse current extract technologies of chloroazotic acid, restore cake of gold with oxalic acid solution, after founding contain gold greater than 99.9% proof gold, saved electrolytic process.Leached mud becomes silver-colored electrolytic anode with soda retailoring, and the electrolytic silver founding becomes fine silver, and argentiferous is greater than 99.9%.Because this method is at boiling state leaching for the third time, for keeping certain solid solution ratio, and constantly drip 1: 1 hydrochloric acid soln, the high temperature acid mist is big for environment pollution, and the loss of hydrochloric acid is many, the production cost height; And be still the operation of heating with the oxalic acid reduction.
Summary of the invention
Technical problem to be solved by this invention provides a kind of free of contamination gold wet purification process, and selecting method is simple, and the reduction gold and silver technology that is easy to grasp is used the oxalic acid low-temperature reduction, and is free from environmental pollution, helps health of operators; Reduce cost simultaneously, shortened the cycle, had tangible economic benefit and social benefit.
Basic ideas of the present invention are: owing to contain gold about 95% in the thick bronze, argentiferous is more than 4%, and all the other are that impurity such as bismuth, copper, platinum, lead are coated in the goldc grains less than 1%, and it is clean to use nitric acid to remove merely, influences the gold quality.The chloroazotic acid desilver is at first used in removal of impurities, secondly is to remove impurity such as bismuth, copper with nitric acid.Gold is dissolved in by nitric acid and hydrochloric acid and generates rich gold solution in the formulated chloroazotic acid of 1: 3～4 ratios, and silver is insoluble to chloroazotic acid, makes its separation with filter method.Rich gold solution becomes the bronze precipitation with the oxalic acid reductive agent reduction gold with strong reducing property, and impurity such as the platinum that is reduced simultaneously, bismuth, copper are then dissolved once more by the nitric acid that adds thereafter and enter solution, separate after filtration, have obtained pure bronze.The proof gold powder becomes the ingot shape through founding, contain gold 99.99% finished product ingot.
According to above-mentioned thinking, problem design to be solved by this invention is realized by following technical scheme: a kind of gold wet purification process is characterized in that: the purifying technique process is:
A, thick bronze is placed container, the ratio by weight 1: 3～4 adds chloroazotic acid and floods thick bronze, and thick bronze is partly dissolved, and is heated to 80 ℃ of remaining thick bronzes of dissolving then while stirring, and cooling was left standstill 1 hour, filters the separation filter residue;
B, filtrate is heated to 80 ℃ again, constantly adds hydrochloric acid slowly and catch up with nitric acid, observe the color of filtrate liquid level flue gas while stirring, stop to add the hydrochloric acid operation when not having brown cigarette;
C, will catch up with solution and isopyknic distilled water mixed diluting behind the nitric acid, under normal temperature condition, add saturated oxalic acid solution, the adding weight of oxalic acid is 120～150% of theoretical amount, observe the changing conditions of the red-brown resultant in the solution, when treating that solution gradually becomes light yellow by red-brown, reaction promptly reaches terminal point;
D, allow the reaction solution standing sedimentation, solid-liquid separation, cake of gold; Clean cake of gold repeatedly with hot aquae destillata, use 80 ℃ of temperature again, concentration is 20% rare nitric acid washing 2～3 times, and with hot aquae destillata clean repeatedly the proof gold powder, this proof gold powder melts down at 1200 ℃-1300 ℃, casts the ingot that contains gold 〉=99.99% again;
E, the washings that settlement separate liquid and this step of d step produced are concentrated and are reclaimed, and add saturated oxalic acid solution again, and the adding weight of oxalic acid is 120～150% of theoretical amount still, leave standstill 12 hours, and the filtering separation filter residue gets slightly that gold returns the molten gold of step a chloroazotic acid; The displacement of separated filtrate zincification silk refilters, the aquae destillata washing, and oven dry gets the platinum concentrate; Remaining filtrate and washings return step a;
F, above-mentioned a step to add weight in the isolating filter residue be the salpeter solution of theoretical value 130%, heated and stirred is not till have a precipitation; The zincification silk stirs displacement, and after filtration, the aquae destillata washing gets thick silver powder; Final filtrate and washings send geosyncline to store.
The foregoing invention chloroazotic acid leaches thick bronze, forms gold perchloride solution, and its reaction equation is:
Au+HNO
3+ 3HCl=AuCl
3+ NO ↑+2H
2The O heating
Filtering separation is caught up with solution behind the nitric acid, and with the oxalic acid reduction, its reaction equation is:
2AuCl
3+3H
2C
2O
4＝2Au↓+8HCl+6CO
2↑
The a step the reaction of isolating leached mud and salpeter solution, zincification silk metathetical equation is:
Ag+HNO
3＝AgNO
3+H
2↑
Zn+2AgNO
3＝Zn(NO
3)
2+2Ag↓
Compared with prior art, the present invention has the following advantages: compare with the electrolytic refining of routine, chloroazotic acid parting method has that technology is simple and clear, product purity is high, production cost is low, the gold loss is little, it is little to pollute, toxicological harmless, economic benefit advantages of higher.Be traditional technology 25% man-hour of every purification 500g gold, and materials consumption only is 8% of a traditional technology.The operation of present method employing oxalic acid normal temperature is reduced golden, has to produce and emits bubble few, and acid mist is few, advantages such as reduction is thorough, the easy observation of terminal point.Technology of the present invention is also recyclable platinum, silver and bismuth on the basis of purifying gold, realizes comprehensive utilization of resources, improves added value of product, meets national industrial policies.
Description of drawings
Fig. 1 is a schematic flow sheet of the present invention.
Embodiment
The explanation that below is 1 pair of embodiment of the present invention is with reference to the accompanying drawings described, but must know that this embodiment can not be used for being construed as limiting the invention.
The purifying technique specific implementation process of this embodiment is:
A, thick bronze 41.9 grams are placed 250 ml beakers, adds 150 milliliters of chloroazotic acid and flood thick bronze, thick bronze is partly dissolved, be heated to 80 ℃ of remaining thick bronzes of dissolving then while stirring, cooling was left standstill 1 hour, filtration, separation filter residue;
B, filtrate is heated to 80 ℃ again, constantly adds hydrochloric acid slowly and catch up with nitric acid, observe the color of filtrate liquid level flue gas while stirring, stop to add the hydrochloric acid operation when not having brown cigarette;
C, will catch up with solution and isopyknic distilled water mixed diluting behind the nitric acid, under normal temperature condition, add saturated oxalic acid solution, the adding weight of oxalic acid is 130% of theoretical amount, observe the changing conditions of the red-brown resultant in the solution, when treating that solution gradually becomes light yellow by red-brown, reaction promptly reaches terminal point;
D, allow the reaction solution standing sedimentation, solid-liquid separation, cake of gold; Clean cake of gold repeatedly with hot aquae destillata, use 80 ℃ of temperature again, concentration is 20% rare nitric acid washing 3 times, and cleans to such an extent that proof gold powder 39.7 restrains repeatedly with hot aquae destillata, this proof gold powder is cast the ingot that contains gold 〉=99.99% again 1200 ℃-1300 ℃ fusings down;
E, the washings that settlement separate liquid and this step of d step produced are concentrated and are reclaimed, and add saturated oxalic acid solution again, and the adding weight of oxalic acid is 130% of theoretical amount still, leave standstill 12 hours, and the filtering separation filter residue gets slightly that gold returns the molten gold of step a chloroazotic acid; The displacement of separated filtrate zincification silk refilters, and the aquae destillata washing is dried to such an extent that platinum concentrate 0.2 restrains; Remaining filtrate and washings return step a;
F, above-mentioned a step to add weight in the isolating filter residue be the salpeter solution of theoretical value 130%, heated and stirred is not till have a precipitation; The displacement of zincification silk, through agitation and filtration, the aquae destillata washing gets thick silver powder 5 grams; Final filtrate and washings send geosyncline to store.
Main economic and technical indices of the present invention:
According to the throughput of present our company, one, two subsidiary factories of company add up to produce about 500 tons of thick silver every year, about 0.8 kilogram of thick silver-colored by-product gold amount per ton, and wherein thick silver on average contains golden 800g/t, and therefore thick silver-colored Gold Content is about 400 kilograms.Silver electrolysis and silver anode slime nitric acid divide the rate of recovery of gold process gold about 99.5%, and it is average 95% that thick bronze contains gold, calculates thus and should produce about 419 kilograms of thick bronze, and Gold Content is about 398 kilograms.At present thick bronze is sold as the finished product, is the 96% i.e. 202 yuan/g valuation of 210 yuan/g of existing 1# gold (Au99.99%) market price with unit price, can obtain 8,040 ten thousand yuan of annual sales revenues.If thick bronze is purified to containing the 1# gold of gold 99.99%, the purifying technique rate of recovery is calculated with 99.7%, can get 397 kilograms of 1# gold, and annual sales revenue is 8,337 ten thousand yuan, 8000 yuan of per kilogram increments, annual 2970000 yuan of the sales revenue that increase.
Cost consumption of the present invention is about 120,000 yuan (containing disposable input), and 397 kilograms of purification 1# gold comprise the 50kg silver and the 2kg platinum of recovery, annually can obtain gross profit more than 3,000,000 yuan approximately.
Claims (1)
1, a kind of gold wet purification process is characterized in that: the purifying technique process is:
A, thick bronze is placed container, the ratio by weight 1: 3～4 adds chloroazotic acid and floods thick bronze, and thick bronze is partly dissolved, and is heated to 80 ℃ of remaining thick bronzes of dissolving then while stirring, and cooling was left standstill 1 hour, filters the separation filter residue;
B, filtrate is heated to 80 ℃ again, constantly adds hydrochloric acid slowly and catch up with nitric acid, observe the color of filtrate liquid level flue gas while stirring, stop to add the hydrochloric acid operation when not having brown cigarette;
C, will catch up with solution and isopyknic distilled water mixed diluting behind the nitric acid, under normal temperature condition, add saturated oxalic acid solution, the adding weight of oxalic acid is 120～150% of theoretical amount, observe the changing conditions of the red-brown resultant in the solution, when treating that solution gradually becomes light yellow by red-brown, reaction promptly reaches terminal point;
D, allow the reaction solution standing sedimentation, solid-liquid separation, cake of gold; Clean cake of gold repeatedly with hot aquae destillata, use 80 ℃ of temperature again, concentration is 20% rare nitric acid washing 2～3 times, and with hot aquae destillata clean repeatedly the proof gold powder, this proof gold powder melts down at 1200 ℃-1300 ℃, casts the ingot that contains gold 〉=99.99% again;
E, the washings that settlement separate liquid and this step of d step produced are concentrated and are reclaimed, and add saturated oxalic acid solution again, and the adding weight of oxalic acid is 120～150% of theoretical amount still, leave standstill 12 hours, and the filtering separation filter residue gets slightly that gold returns the molten gold of step a chloroazotic acid; The displacement of separated filtrate zincification silk refilters, the aquae destillata washing, and oven dry gets the platinum concentrate; Remaining filtrate and washings return step a;
F, above-mentioned a step to add weight in the isolating filter residue be the salpeter solution of theoretical value 130%, heated and stirred is not till have a precipitation; The zincification silk stirs displacement, and after filtration, the aquae destillata washing gets thick silver powder; Final filtrate and washings send geosyncline to store.
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| CN2008100319628A CN101328541B (en) | 2008-07-27 | 2008-07-27 | Gold wet purification process |
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|---|---|---|---|
| CN2008100319628A CN101328541B (en) | 2008-07-27 | 2008-07-27 | Gold wet purification process |
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| CN101328541B CN101328541B (en) | 2010-06-09 |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101736159B (en) * | 2009-09-02 | 2011-04-20 | 紫金矿业集团股份有限公司 | Method for recovering gold from alkaline waste water |
| CN102071323A (en) * | 2010-12-16 | 2011-05-25 | 惠州市奥美特环境科技有限公司 | Method for producing high-purity gold by utilizing electroplating waste liquid containing gold |
| CN102978407A (en) * | 2012-12-17 | 2013-03-20 | 四会市鸿明贵金属有限公司 | Method for recovering platinum from silver electrolyte |
| CN103074501A (en) * | 2013-02-22 | 2013-05-01 | 昆山鸿福泰环保科技有限公司 | Gold net recovery process |
| CN104404265A (en) * | 2014-12-02 | 2015-03-11 | 中条山有色金属集团有限公司 | Gold powder washing purification method |
| CN105274351A (en) * | 2015-10-12 | 2016-01-27 | 湖南金旺铋业股份有限公司 | Process for recycling high-purity gold from anode slime through organic reduction method |
| CN105463195A (en) * | 2015-12-04 | 2016-04-06 | 无锡英特派金属制品有限公司 | Purification method for gold in gold-nickel alloy |
| CN105907985A (en) * | 2016-06-29 | 2016-08-31 | 贵州银花妆开发有限公司 | Method for extracting and purifying gold in gold ore |
| CN105965030A (en) * | 2016-06-20 | 2016-09-28 | 昆山鸿福泰环保科技有限公司 | Technique for recovering gold from gold iodide liquid waste |
| CN107641721A (en) * | 2017-09-29 | 2018-01-30 | 云南驰宏锌锗股份有限公司 | A kind of method of thick gold purification |
| CN110643827A (en) * | 2019-10-22 | 2020-01-03 | 贵州大学 | Green method for dissolving and extracting gold element |
| CN114669754A (en) * | 2022-03-04 | 2022-06-28 | 金川集团股份有限公司 | Method for efficiently purifying gold from alloyed gold |
| CN115323175A (en) * | 2022-08-12 | 2022-11-11 | 肇庆市新荣昌环保股份有限公司 | Wet extraction process and device for recycling electronic waste nonferrous metal |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87105051A (en) * | 1987-08-01 | 1988-04-27 | 东北工学院 | Sepaation method of gold and siluer |
| CN1025922C (en) * | 1990-10-22 | 1994-09-14 | 滕先第 | Gold and silver separation method |
| CN1377983A (en) * | 2002-01-23 | 2002-11-06 | 山西宏艺首饰股份有限公司 | Quick dissolving and purifying method for crude gold or alloy |
| CN100424201C (en) * | 2006-03-01 | 2008-10-08 | 张勇 | Method for purifying golden and silver by fast wetting optimization |
-
2008
- 2008-07-27 CN CN2008100319628A patent/CN101328541B/en not_active Expired - Fee Related
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|---|---|---|---|---|
| CN101736159B (en) * | 2009-09-02 | 2011-04-20 | 紫金矿业集团股份有限公司 | Method for recovering gold from alkaline waste water |
| CN102071323A (en) * | 2010-12-16 | 2011-05-25 | 惠州市奥美特环境科技有限公司 | Method for producing high-purity gold by utilizing electroplating waste liquid containing gold |
| CN102978407A (en) * | 2012-12-17 | 2013-03-20 | 四会市鸿明贵金属有限公司 | Method for recovering platinum from silver electrolyte |
| CN102978407B (en) * | 2012-12-17 | 2014-09-03 | 四会市鸿明贵金属有限公司 | Method for recovering platinum from silver electrolyte |
| CN103074501A (en) * | 2013-02-22 | 2013-05-01 | 昆山鸿福泰环保科技有限公司 | Gold net recovery process |
| CN104404265A (en) * | 2014-12-02 | 2015-03-11 | 中条山有色金属集团有限公司 | Gold powder washing purification method |
| CN105274351B (en) * | 2015-10-12 | 2017-07-07 | 湖南金旺铋业股份有限公司 | The technique that a kind of organic reducing method reclaims High Purity Gold from the earth of positive pole |
| CN105274351A (en) * | 2015-10-12 | 2016-01-27 | 湖南金旺铋业股份有限公司 | Process for recycling high-purity gold from anode slime through organic reduction method |
| CN105463195A (en) * | 2015-12-04 | 2016-04-06 | 无锡英特派金属制品有限公司 | Purification method for gold in gold-nickel alloy |
| CN105965030A (en) * | 2016-06-20 | 2016-09-28 | 昆山鸿福泰环保科技有限公司 | Technique for recovering gold from gold iodide liquid waste |
| CN105907985A (en) * | 2016-06-29 | 2016-08-31 | 贵州银花妆开发有限公司 | Method for extracting and purifying gold in gold ore |
| CN105907985B (en) * | 2016-06-29 | 2017-10-24 | 贵州银花妆开发有限公司 | Gold and the method purified are extracted in a kind of gold mine |
| CN107641721A (en) * | 2017-09-29 | 2018-01-30 | 云南驰宏锌锗股份有限公司 | A kind of method of thick gold purification |
| CN107641721B (en) * | 2017-09-29 | 2019-10-18 | 云南驰宏锌锗股份有限公司 | A kind of method of thick gold purification |
| CN110643827A (en) * | 2019-10-22 | 2020-01-03 | 贵州大学 | Green method for dissolving and extracting gold element |
| CN110643827B (en) * | 2019-10-22 | 2022-02-18 | 贵州大学 | Green method for dissolving and extracting gold element |
| CN114669754A (en) * | 2022-03-04 | 2022-06-28 | 金川集团股份有限公司 | Method for efficiently purifying gold from alloyed gold |
| CN115323175A (en) * | 2022-08-12 | 2022-11-11 | 肇庆市新荣昌环保股份有限公司 | Wet extraction process and device for recycling electronic waste nonferrous metal |
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