CN101985691B - Method for preparing high-purity gold - Google Patents
Method for preparing high-purity gold Download PDFInfo
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- CN101985691B CN101985691B CN2010105673476A CN201010567347A CN101985691B CN 101985691 B CN101985691 B CN 101985691B CN 2010105673476 A CN2010105673476 A CN 2010105673476A CN 201010567347 A CN201010567347 A CN 201010567347A CN 101985691 B CN101985691 B CN 101985691B
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Abstract
The invention discloses a method for preparing high-purity gold and relates to a method for preparing the high-purity gold from coarse gold powder prepared from copper anode slime and a copper-nickel alloy which serve as raw materials. The method is characterized by comprising the following steps of: performing electrolysis dissolution on coarse gold, performing dibutyl carbitol (DBC) extraction on dissolved liquid, washing impurities, performing back extraction with oxalic acid, performing acid boiling on the gold powder and casting an ingot. In the method of the invention, the process flows are connected smoothly, the advantages of two refining impurity removal processes are used for reference, the product quality is stable and the direct recovery of noble metal is improved; and the gold is dissolved by adopting an electrolysis dissolution mode, so the method slightly pollutes the environment and is favorable for energy conservation and emission reduction.
Description
Technical field
A kind of method for preparing High Purity Gold, relating to a kind of is the method that the thick bronze of raw material output prepares High Purity Gold from copper anode mud and cupronickel.
Background technology
The classical way of gold refining is pyrogenic process oxidation refining method, chlorination refining method and electrolytic process.Along with the variation that science and technology development and gold reclaim raw material, chemical refining method and extracting refining method also successively are applied to produce.And pyrogenic process oxidation refining method, chlorination refining method are difficult to output purity and reach 99.9% gold; Electrorefining desilver effect is relatively poor relatively, repeats electrolysis and also has defective; DBC (dibutyl carbitol) extraction process contains palladium, silver-colored higher owing to palladium, silver-colored easy formation are altogether come together in the back extraction bronze.State Administration for Quality Supervision and Inspection and Quarantine issues on November 3rd, 2003 and has implemented national golden product new standard---GB/T4134-2003; New standard has increased the control requirement of Pd, Si, Mg, Sn, As, Cr, Ni, Mn these 8 impurity elements, uses a kind of difficult requirement that reaches new standard IC-Au99.995 of golden quality product of refinery practice output separately.
Summary of the invention
The object of the invention is exactly the deficiency that exists to above-mentioned prior art, and a kind of complicated raw material to different process is provided, and the recovery is high; Technological process connects smooth and easy; The operation of no chloroazotic acid liquid making, good operational environment, the method for preparing High Purity Gold of constant product quality.
The objective of the invention is to realize through following technical scheme.
A kind of method for preparing High Purity Gold is characterized in that its preparation process at first with thick golden electrolysis dissolution, after the liquid making liquid through DBC extraction, washing impurity, back extraction reduction, the acid of reduction bronze boil, ingot casting, make High Purity Gold.
A kind of method for preparing High Purity Gold of the present invention is characterized in that its thick golden electrolysis dissolution process casts positive plate with thick gold and make anode, and the proof gold sheet is done negative electrode; Negative electrode overcoat unglazed crucible is positioned at electrolyzer, the volume ratio HCl:H of electrolyzer electrolyte inside
2O=2:1, the volume ratio HCl:H of solution in the unglazed crucible
2O=1:1; Liquid level is higher than liquid level 5-10mm in the groove in the unglazed crucible, and liquid making feeds pulsatory current, processing parameter: galvanic current density 250～320A/m
2, synergetic interchange is 1.1～1.5 times of direct currents, bath voltage 0.4～0.8V.
A kind of method for preparing High Purity Gold of the present invention is characterized in that the Au that gets off when from anode dissolution
3+In anolyte, accumulate and reach more than the 300g/L control concentration of hydrochloric acid 3mol/L, Cl
-Total concn is 6mol/L, carries out the DBC extraction.
A kind of method for preparing High Purity Gold of the present invention, the processing condition that it is characterized in that the DBC extraction process are O/A=1, room temperature, 5 stage countercurrents extraction in centrifugal extractor, every grade of mixed phase time 8min.
A kind of method for preparing High Purity Gold of the present invention, the washing composition that it is characterized in that washing process is 0.5 mol/LHCl, O/A=2:1, room temperature, 4 stage countercurrents, every grade of mixed phase time 8min.
A kind of method for preparing High Purity Gold of the present invention is characterized in that reduction process is that consumption is 1.5～2 times of theoretical amount with the oxalic acid solution that carries golden organic phase adding 5%, and 76～82 ℃ of temperature stir reductase 12～3h.
A kind of method for preparing High Purity Gold of the present invention; It is characterized in that extraction agent dibutyl carbitol (dibutyl ethylene glycol ether) boiling point (252 ℃), flash-point (118 ℃) are higher, water-soluble lowly have only 0.3%, and partition ratio can reach 2500; Rate of extraction is very fast, and can reach balance 30 seconds.
A kind of method for preparing High Purity Gold of the present invention, thick gold is made anode, and proof gold is done negative electrode, carries out electrolysis dissolution, the Au that gets off from anode dissolution
3+Can not in anolyte, accumulate through crucible, reach 250-300g/L, hydrochloric acid 250-300 g/L, control concentration of hydrochloric acid 3mol/L, Cl
-Total concn 6mol/L can be connected with the DBC extraction process, and extraction raffinate contains Au＜0.005 g/L, and percentage extraction is higher than 99.5%.The gold of output can satisfy new standard after two kinds of technologies organically combined---the IC-Au99.995 trade mark of GB/T4134-2003.
Method of the present invention has been brought into play the characteristics of two kinds of refinery practices, has avoided single technology to repeat the shortcoming that multipass could the output High Purity Gold during production High Purity Gold; Technological design is smooth, is combined by electrolysis dissolution and DBC extraction; No aqua regia dissolution operation, the execute-in-place environment is better; Technological design is reasonable, and constant product quality property is high.In this case, should maximize favourable factors and minimize unfavourable ones, adopt process integration, and reasonably be connected, bring into play the advantage of removal of impurities separately, the defective of avoiding single technology to repeat, the highly purified gold of output is preferable selection.
Description of drawings
Fig. 1 is the process flow sheet of the inventive method.
Embodiment
A kind of method for preparing High Purity Gold is characterized in that its preparation process at first with thick golden electrolysis dissolution, and liquid boils and wash, casts the finished product ingot of various different sizes after the liquid making through DBC extraction, washing impurity, back extraction, bronze.
Embodiment 1
Make anode with two blocks of thick gold, 1 of proof gold is done negative electrode, negative electrode overcoat unglazed crucible, liquid making in Porcelain Jar, HCl:H in the cylinder
2O=2:1, HCl:H in the crucible
2O=1:1.Liquid level is higher than liquid level 5 ~ 10mm in the cylinder in the crucible.Feed pulsatory current, the Au that gets off from anode dissolution
3+Can not in anolyte, accumulate through crucible, after 7 days, Au
3+Reach 265g/L, hydrochloric acid 283g/L, control concentration of hydrochloric acid 3.2mol/L, Cl
-Total concn 6.5mol/L is connected with the DBC extraction process.Extraction: O/A=1 carries out 4 grades of extractions in separating funnel, each mixed phase time 5min.Extraction raffinate contains Au＜0.008 g/L, and percentage extraction is higher than 99.5%.Washing: washing composition is 0.5 mol/LHCl, O/A=2:1, room temperature, 3 grades of washings, every grade of mixed phase time 5min.Reduction: carry golden organic phase and in the 5L beaker, reducing, reductive agent is 5% oxalic acid solution, and 76 ~ 82 ℃ of temperature of reaction stir reductase 12 ~ 3h.Bronze boils through the hydrochloric acid of 1:1 and washes, and vitriol oil digestion quality exceeds new standard---the IC-Au99.995 trade mark of GB/T4134-2003.
Embodiment 2
Make anode with 3 blocks of thick gold, two of proof gold are done negative electrode, negative electrode overcoat unglazed crucible, liquid making in Porcelain Jar, HCl:H in the cylinder
2O=2:1, HCl:H in the crucible
2O=1:1.Liquid level is higher than liquid level 5 ~ 10mm in the cylinder in the crucible.Feed pulsatory current, the Au that gets off from anode dissolution
3+Can not in anolyte, accumulate through crucible, after 5 days, Au
3+Reach 295g/L, hydrochloric acid 263g/L, control concentration of hydrochloric acid 3.3mol/L, Cl
-Total concn 6.4mol/L is connected with the DBC extraction process.Extraction: O/A=1 carries out 4 grades of extractions in separating funnel, each mixed phase time 5min.Extraction raffinate contains Au＜0.0086g/L, and percentage extraction is higher than 99.5%.Washing: washing composition is 0.5 mol/LHCl, O/A=2:1, room temperature, 3 grades of washings, every grade of mixed phase time 5min.Reduction: carry golden organic phase and in the 5L beaker, reducing, reductive agent is 5% oxalic acid solution, and 76 ~ 82 ℃ of temperature of reaction stir reductase 12 ~ 3h.The extraction bronze boils through the hydrochloric acid of 1:1 and washes, and vitriol oil digestion quality exceeds new standard---the IC-Au99.995 trade mark of GB/T4134-2003.
Embodiment 3
Make anode with 6 blocks of thick gold, 4 of proof gold are done negative electrode, and negative electrode overcoat unglazed crucible adopts electrolysis dissolution, and electrolyzer uses rigid plastic sheet to make, HCl:H in the volume 60L, groove
2O=2:1, HCl:H in the crucible
2O=1:1.Liquid level is higher than liquid level 5 ~ 10mm in the groove in the crucible.Feed pulsatory current, the Au that gets off from anode dissolution
3+Can not in anolyte, accumulate through crucible, reach 302g/L at last, hydrochloric acid 245 g/L, control concentration of hydrochloric acid 2.9mol/L, Cl
-Total concn 6.2mol/L is connected with the DBC extraction process.Extraction: O/A=1, room temperature, 5 stage countercurrents extraction in centrifugal extractor, every grade of mixed phase time 8min.Extraction raffinate contains Au＜0.008g/L, and percentage extraction is higher than 99.5%.Washing: washing composition is 0.5 mol/LHCl, O/A=2:1, room temperature, 4 stage countercurrents, every grade of mixed phase time 8min.Reduction: carry golden organic phase and in 500L acid reaction kettle, reduce, reductive agent is 5% oxalic acid solution, and 76 ~ 82 ℃ of temperature of reaction stir reductase 12 ~ 3h.The extraction bronze of output boils through the hydrochloric acid of 1:1 and washes, and vitriol oil digestion quality can satisfy new standard---the IC-Au99.995 trade mark of GB/T4134-2003.
Embodiment 4
Make anode with 8 blocks of thick gold, 6 of proof gold are done negative electrode, and negative electrode overcoat unglazed crucible adopts electrolysis dissolution, and electrolyzer uses rigid plastic sheet to make, HCl:H in the volume 80L, groove
2O=2:1, HCl:H in the crucible
2O=1:1.Liquid level is higher than liquid level 5 ~ 10mm in the groove in the crucible.Feed pulsatory current, the Au that gets off from anode dissolution
3+Can not in anolyte, accumulate through crucible, reach 326g/L at last, hydrochloric acid 265 g/L, control concentration of hydrochloric acid 3.1mol/L, Cl
-Total concn 6.4mol/L is connected with the DBC extraction process.Extraction: O/A=1, room temperature, 5 stage countercurrents extraction in centrifugal extractor, every grade of mixed phase time 8min.Extraction raffinate contains Au＜0.01g/L, and percentage extraction is higher than 99.5%.Washing: washing composition is 0.5 mol/LHCl, O/A=2:1, room temperature, 4 stage countercurrents, every grade of mixed phase time 8min.Reduction: carry golden organic phase and in 500L acid reaction kettle, reduce, reductive agent is 5% oxalic acid solution, and 76 ~ 82 ℃ of temperature of reaction stir reductase 12 ~ 3h.The extraction bronze of output boils through the hydrochloric acid of 1:1 and washes, and vitriol oil digestion quality can satisfy new standard---the IC-Au99.995 trade mark of GB/T4134-2003.
Claims (2)
1. method for preparing High Purity Gold is characterized in that its preparation process at first casts positive plate with thick gold and carry out electrolysis dissolution, and liquid is through DBC extraction, washing impurity, oxalic acid back extraction with bronze acid is boiled, the casting ingot after the liquid making; Its thick golden electrolysis dissolution process is made anode with thick gold bullion, and the proof gold sheet is done negative electrode; Negative electrode overcoat unglazed crucible is positioned at electrolyzer, the volume ratio HCl:H of electrolyzer electrolyte inside
2O=2:1, the volume ratio HCl:H of solution in the unglazed crucible
2O=1:1; Liquid level is higher than liquid level 5-10mm in the groove in the unglazed crucible, and electrolytic process feeds pulsatory current; As the Au that gets off from anode dissolution
3+Accumulation reaches 326g/L in anolyte, during hydrochloric acid 265 g/L, and control concentration of hydrochloric acid 3.1mol/L, Cl
-Total concn is 6.4mol/L, carries out the DBC extraction; The processing condition of its DBC extraction process are O/A=1, room temperature, 5 stage countercurrents extraction in centrifugal extractor, every grade of mixed phase time 8min; Its bronze acid process of boiling is with the oxalic acid solution that carries golden organic phase adding 5%, temperature 76-82 ℃, stirs reductase 12-3h.
2. a kind of method for preparing High Purity Gold according to claim 1, the washing composition that it is characterized in that washing process is 0.5 mol/LHCl, O/A=2:1, room temperature, 4 stage countercurrents, every grade of mixed phase time 8min.
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| CN2010105673476A CN101985691B (en) | 2010-12-01 | 2010-12-01 | Method for preparing high-purity gold |
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| CN103757246A (en) * | 2014-01-02 | 2014-04-30 | 紫金矿业集团股份有限公司 | Method for producing high-purity gold |
| CN104404569B (en) * | 2014-11-04 | 2018-02-23 | 常州钇金环保科技有限公司 | The preparation technology of high pure gold |
| CN104480322A (en) * | 2014-12-07 | 2015-04-01 | 金川集团股份有限公司 | Method for extracting gold and palladium from silver anode slime |
| CN105441689A (en) * | 2015-11-18 | 2016-03-30 | 金川集团股份有限公司 | Method for preparing high-purity gold |
| CN105441690A (en) * | 2015-11-18 | 2016-03-30 | 金川集团股份有限公司 | Method for extracting gold from material liquid with high gold content |
| 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 |
| CN111363920A (en) * | 2020-04-07 | 2020-07-03 | 金川集团股份有限公司 | Method for extracting gold from silver-containing liquid |
| MX2023002015A (en) | 2020-08-18 | 2023-04-11 | Enviro Metals Llc | Metal refinement. |
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| CN101122032A (en) * | 2007-05-21 | 2008-02-13 | 江西铜业集团公司 | One-step producing technique for high-purity gold |
| CN101748276A (en) * | 2009-12-31 | 2010-06-23 | 中国科学院成都有机化学有限公司 | Process for extracting, separating and purifying Ag, Au, Pd and Pt |
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Owner name: JINCHUAN GROUP CO., LTD. Free format text: FORMER NAME: JINCHUAN GROUP CORP., LTD. |
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Address after: 737103 Jinchuan Road, Gansu, China, No. 98, No. Patentee after: Jinchuan Group Co., Ltd. Address before: 737103 Jinchuan Road, Gansu, China, No. 98, No. Patentee before: Jinchuan Group Corp., Ltd. |