CN1035321A - Method with composite extractant to produce high-pure gold - Google Patents
Method with composite extractant to produce high-pure gold Download PDFInfo
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- CN1035321A CN1035321A CN88103753A CN88103753A CN1035321A CN 1035321 A CN1035321 A CN 1035321A CN 88103753 A CN88103753 A CN 88103753A CN 88103753 A CN88103753 A CN 88103753A CN 1035321 A CN1035321 A CN 1035321A
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- gold
- organic phase
- tbp
- composite extractant
- fatty alcohol
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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
Abstract
With the method for composite extractant extracting and separating gold from gold-containing solution, comprise the room temperature extraction; Golden organic phase is carried in the mineral acid washing; Reduction; Operations such as organic phase regeneration.It is characterized in that said composite extractant is the mixed solution of long carbochain Fatty Alcohol(C12-C14 and C12-C18) with TBP, the mixed volume ratio of the two is 99~10: 1~90, and said reductive agent is an ammonium oxalate.The present invention is big to the percentage extraction height of gold, loading capacity, direct yield is more than 99%, can the High Purity Gold product of disposable acquisition 99.99% or more, and technology is simple, and flow process is lacked, less investment, economic benefit height.The present invention can be used for separating and recovering gold from acidic solution.
Description
The wet method that the present invention relates to precious metal is extracted metallurgical.
Solvent-applied extraction process separating and recovering gold from gold-containing solution promptly has the patent report in the sixties, because this kind technology has been compared many advantages with traditional electrolysis process, so the back development is very fast, now has been widely used in the wet extraction process of gold.The extraction agent of gold is of a great variety, but comparatively effectively, extraction agent commonly used is that neutrality contains oxygen extraction agent (as ketone, ethers, alcohols) and phosphoric acid ester (as tributyl phosphate, i.e. TBP).But the common drawback of ketone and ethers is water-soluble big, and boiling point is low, volatile loss.So, alcohols more usually." precious metal " 1984, Vol5NO3, P38 has commented with long carbochain Fatty Alcohol(C12-C14 and C12-C18), as the situation as extraction agent collection gold such as n-Octanol, secondary sad, isooctyl alcohol, primary isoamyl alcohol, isodecyl alcohol, also reported in dibutyl carbitol and added n-Octanol, can improve the extraction efficiency of dibutyl carbitol, improve its selectivity gold." precious metal " 1985, VOl6, NO4, P39 have also been commented with long carbochain Fatty Alcohol(C12-C14 and C12-C18), particularly isodecyl alcohol and alcohol mixture (ROH, R=C
3~C
11) situation of extracting gold.This article has also been reported with TBP and has been made extraction agent, and the situation with dodecane and chloroform give thinner extracting and separating gold can obtain 99.99% High Purity Gold." precious metal " 1978, NO2, the problem of TBP extracting and separating gold has been furtherd investigate in P19~28, points out that different thinners has very different influences to the selectivity of TBP collection gold, then can improve the selectivity of TBP collection gold the most significantly with the chloroform give thinner.But single long carbochain Fatty Alcohol(C12-C14 and C12-C18) as the weak point of extraction agent collection gold is, it is relatively poor to the hold facility of gold that golden organic phase is carried in the extraction back, and the eluting rate of gold is higher in acid cleaning process subsequently.Dibutyl carbitol costs an arm and a leg, and reagent is rare.The selectivity of TBP collection gold is relatively poor, can improve its selectivity significantly though add the chloroform dilution, and the chloroform water dissolubility is big, and is volatile, and toxicity is bigger, unsuitable industrial a large amount of uses.In addition, existing collection gold process, from the process of carrying golden organic phase reduction gold, oxalic acid commonly used, sodium oxalate, formic acid, sodium formiate, sulfurous acid, S-WAT, sulfurous gas etc. are made reductive agent.Use these reductive agents to reduce gold, need in reduction process, to add at any time the pH value that acid or alkali are adjusted solution, it is maintained between 4~5, gold is reduced effectively, otherwise the gold after the reduction reacts again together with other element.This just makes operation become complicated, the consumption that increases reagent.
The objective of the invention is to overcome the deficiency of prior art, a kind of composite extractant and reductive agent of efficient, inexpensive, low toxicity are provided, make its energy high-level efficiency, large vol, highly selective extracting and separating gold from gold-containing solution, and effectively with its reduction, simplify technology, obtain the High Purity Gold product more than 99.99% once.
Technical solution of the present invention is: the mixed solution with long carbochain Fatty Alcohol(C12-C14 and C12-C18) and TBP is made compound extraction agent; Select for use ammonium oxalate to make reductive agent, come reduction gold from carry golden organic phase.The combination of this composite extractant, long carbochain Fatty Alcohol(C12-C14 and C12-C18) and TBP are maximized favourable factors and minimized unfavourable ones separately, make up for each other's deficiencies and learn from each other, play " association's collection " effect, produced the new effect that single extraction agent did not have, both kept high percentage extraction and the highly selective of long carbochain Fatty Alcohol(C12-C14 and C12-C18), improved the hold facility of year golden organic phase by adding TBP again, greatly reduced the eluting rate of gold gold to gold.
Technical process of the present invention is:
1. add TBP composite extractant extracting gold from contain auric acid solution with long carbon fatty alcohol under the room temperature.Said long carbochain Fatty Alcohol(C12-C14 and C12-C18) can be from n-Octanol, secondary octanol, isooctyl alcohol, isodecyl alcohol and alcohol mixture (ROH, R=C
7~C
11) in select a kind ofly, preferentially recommend isooctyl alcohol and alcohol mixture.The mixed volume of composite extractant two components is than being long carbochain Fatty Alcohol(C12-C14 and C12-C18): TBP=99~10: 1~90, and preferential ratio of mixture of recommending is 90~70: 10~30; The extraction temperature room temperature; Contact 1~10 minute time general 3~5 minutes; Compare (organic phase: water)=1: 1~25, be generally 1: 5~15; 3~8 grades of extraction progression, general 3~6 grades.
2. carry golden organic phase with the mineral acid washing.Mineral acid can be selected a kind of from sulfuric acid, hydrochloric acid, nitric acid, perchloric acid.
3. with the gold in the organic phase after the ammonium oxalate reduction washing.The reductive agent consumption is 1.5~3 times of stoichiometric quantity, 40~75 ℃ of reduction temperatures, preferably 40~60 ℃, 0.5~4 hour recovery time, general 0.5~2 hour.
4. the organic phase after the reduction contacts with above-mentioned a kind of mineral acid, makes organic phase regeneration.
5. regeneration organic extractant phase next batch gold-containing solution.
The said auric acid solution that contains can be hydrochloric acid, sulfuric acid, nitric acid, perchloric acid, chloroazotic acid or their mixture medium, also can contain chlorine, sodium chlorate, clorox, sodium-chlor, and the ion of platinum, palladium, rhodium, iridium, copper, nickel, iron, lead, selenium, tellurium etc.The advantage of selecting for use ammonium oxalate to make reductive agent is that the pH value of reduction back solution need not add other reagent and can maintain automatically between 4~5, does not influence later effect of extracting, and the reductive gold is precipitated out with the metallics form and obtains reclaiming.
Compare with prior art, the present invention has following advantage:
1. from various medium solutions, reclaim gold expeditiously, can once obtain 99.99% High Purity Gold product.
2. Jin percentage extraction can reach more than 99.9%, and direct yield reaches more than 99%.
3. Jin loading capacity is big, can reach more than 43.6 grams per liters.
4. the former liquid acidity of Shi Yinging is wider, and the selectivity of collection gold is good, and rate of extraction is fast.
5. simple to operate, flow process weak point, less investment, instant effect.
6. extraction agent source is wide, and inexpensive, loss of extractant is little, for already known processes is minimum at present, and each circulation of the loss of extraction agent only 1.2%.
7. carrying golden organic phase, to reduce golden speed fast, and the reductive agent consumption is low.
8. carry golden organic phase washing, the eluting rate of gold is low.
9. extraction agent stable performance, multiplexing performance is good.
Embodiments of the invention prove that purpose of the present invention reaches fully.
Embodiment 1
Copper anode mud after taking off Cu, Se, Te is at 0.5NH
2SO
4Add sodium chlorate oxidation dissolution gained solution in the medium, its main component is (grams per liter): Au1.72, Pd0.0253, Pt0.005, Ni0.54, Cu0.416, Fe0.063, Se0.75.Use isocaprylic acid: TBP=80 under the room temperature: 20 composite extractant extraction, contact 3 minutes time, compare 1: 10,4 grades of extraction progression.After carrying golden organic phase usefulness 0.5N sulfuric acid scrubbing, in 40~60 ℃ of temperature, reduce with ammonium oxalate.Totally 12 circulations.Handle 2272.52 milliliters of feed liquids, the percentage extraction of gold is on average greater than 99.2%, and the raffinate gold content is in 0.001~<0.0005 grams per liter scope.Drop into 3908.73 milligrams of gold altogether, real 3885.47 milligrams of the product gold that get, direct yield 99.4% product quantitative spectrometric analysis, purity is all greater than 99.99%.
Embodiment 2:
With pre-treating process gained composition (grams per liter) following solution: Au2.26, Pd0.020, Pt0.0058, Ni0.33, Cu0.610, Fe0.055.With the composite extractant extraction of using 12 times among the embodiment 1, with postprocessing working procedures with embodiment 1, totally 38 circulations (totally 50 circulations).Handle 3499.48 milliliters of feed liquids.The percentage extraction of gold is on average greater than 99.97%, and the raffinate gold content is in 0.0008~<0.0005 grams per liter scope.Drop into 10734.27 milligrams of gold altogether, real 10657.29 milligrams of product gold, the direct yield 99.28% of getting.Its purity of product quantitative spectrometric analysis is better than 99.99%.
Embodiment 3
The gold mud composition (Wt.%) of certain gold mine is: Au2.78, Ag0.16, Zn22.31, Pb17.60, Cu0.22.This gold mud is used rare aqua regia dissolution behind separation and concentration, a rare wang aqueous solution that contains golden 2.7 grams per liters.Use alcohol mixture: TBP=80 under the room temperature: 20 composite extractant extracts this liquid, contacts 3 minutes time, compares 1: 3,4 grades of extraction progression.Carry golden organic phase after 0.5N salt acid elution and ammonium oxalate reduction (50~60 ℃ of reduction temperatures), raffinate contains gold less than 0.0005 grams per liter, and the percentage extraction of gold is greater than 99.98%.Drop into 1564.04 milligrams of gold altogether, real 1548.4 milligrams of product gold, direct yield>99%, the product purity 99.99% of getting.
Claims (4)
1, a kind of from contain auric acid solution the method for extracting and separating gold, comprise that (a) is at room temperature with composite extractant extracting gold from said acidic solution, (b) organic phase of usefulness mineral acid wash load gold, (c) with the gold in the organic phase after the reductive agent reduction washing, (d) organic phase after the reduction contacts with mineral acid, make organic phase regeneration, (e) the organic extractant phase next batch gold-containing solution after the regeneration.The feature of said method is, said composite extractant is the mixed solution of long carbochain Fatty Alcohol(C12-C14 and C12-C18) and tributyl phosphate (TBP), its mixed volume is than being long carbochain Fatty Alcohol(C12-C14 and C12-C18): TBP=99~10: 1~90, the time of contacting during extraction is 1~10 minute, compare (organic phase: water)=1: 1~25,3~8 grades of extraction progression, said reductive agent is an ammonium oxalate, its consumption is 1.5~3 times of stoichiometric quantity, and reduction temperature is 40~75 ℃, 0.5~4 hour recovery time.
2, method as claimed in claim 1 is characterized in that, said long carbochain Fatty Alcohol(C12-C14 and C12-C18) is from n-Octanol, secondary octanol, isooctyl alcohol, isodecyl alcohol, alcohol mixture (ROH, R=C
7~C
10) in optional a kind of.
3, method as claimed in claim 1 is characterized in that, the ratio of mixture of said composite extractant is long carbochain Fatty Alcohol(C12-C14 and C12-C18): TBP=90~70: 10~30.
4, according to the method for claim 1, it is characterized in that reduction temperature is 40~60 ℃, the recovery time is 0.5~2 hour.
Priority Applications (1)
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CN88103753A CN1011420B (en) | 1988-06-15 | 1988-06-15 | Method using composite extractant to produce high-pure gold |
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CN88103753A CN1011420B (en) | 1988-06-15 | 1988-06-15 | Method using composite extractant to produce high-pure gold |
Publications (2)
Publication Number | Publication Date |
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CN1035321A true CN1035321A (en) | 1989-09-06 |
CN1011420B CN1011420B (en) | 1991-01-30 |
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CN88103753A Expired CN1011420B (en) | 1988-06-15 | 1988-06-15 | Method using composite extractant to produce high-pure gold |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1045794C (en) * | 1996-09-16 | 1999-10-20 | 昆明贵金属研究所 | Method for obtg. gold, silver and other noble metals from anode and contg. high concn. arsenic and lead |
CN1045796C (en) * | 1996-09-16 | 1999-10-20 | 昆明贵金属研究所 | Extraction of gold, silver and valued metals from arsenic-and copper-bearing anode sludge |
CN100354438C (en) * | 2004-06-30 | 2007-12-12 | 日矿金属株式会社 | Method for extracting metal solvent |
CN101619391B (en) * | 2009-08-10 | 2011-11-16 | 暨南大学 | Method for separating and extracting gold from cyanide gold-leaching barren solution |
CN104004921A (en) * | 2014-05-31 | 2014-08-27 | 北京工业大学 | Process for efficiently enriching and recovering precious metals platinum and palladium by using solvent extraction method |
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 |
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 |
-
1988
- 1988-06-15 CN CN88103753A patent/CN1011420B/en not_active Expired
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1045794C (en) * | 1996-09-16 | 1999-10-20 | 昆明贵金属研究所 | Method for obtg. gold, silver and other noble metals from anode and contg. high concn. arsenic and lead |
CN1045796C (en) * | 1996-09-16 | 1999-10-20 | 昆明贵金属研究所 | Extraction of gold, silver and valued metals from arsenic-and copper-bearing anode sludge |
CN100354438C (en) * | 2004-06-30 | 2007-12-12 | 日矿金属株式会社 | Method for extracting metal solvent |
CN101619391B (en) * | 2009-08-10 | 2011-11-16 | 暨南大学 | Method for separating and extracting gold from cyanide gold-leaching barren solution |
CN104004921A (en) * | 2014-05-31 | 2014-08-27 | 北京工业大学 | Process for efficiently enriching and recovering precious metals platinum and palladium by using solvent extraction method |
US9957587B2 (en) | 2014-05-31 | 2018-05-01 | Beijing University Of Technology | Process for efficiently enriching and recovering noble metals of platinum and palladium by solvent extraction |
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 |
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 |
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 |
Also Published As
Publication number | Publication date |
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CN1011420B (en) | 1991-01-30 |
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