CN100507029C - Method of extracting and enriching gold (I) from cyaniding gold containing leaching solution - Google Patents
Method of extracting and enriching gold (I) from cyaniding gold containing leaching solution Download PDFInfo
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- CN100507029C CN100507029C CNB2006100375794A CN200610037579A CN100507029C CN 100507029 C CN100507029 C CN 100507029C CN B2006100375794 A CNB2006100375794 A CN B2006100375794A CN 200610037579 A CN200610037579 A CN 200610037579A CN 100507029 C CN100507029 C CN 100507029C
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Abstract
The invention discloses an extracting method of gold (I) in the enriched cyanidation leached gold liquid, which comprises the following steps: blending extractant, extracting-assisting agent and diluent with bulk rate at 1-50:1-50:30-98 to form organic phase of extracting system; contacting organic phase and alkaline cyanidation leached gold liquid with bulk rate at 1: 1-25; stirring completely; extracting Au(CN)2- in the organic liquid; proceeding back extraction for organic phase with gold cyano ion and back extractant alkaline solution with bulk rate at 1-20: 1; transmitting gold cyano ion into back extractant; recycling leached gold and organic phase.
Description
Technical field
The present invention relates to smelting technology, relate in particular to the method for the gold in the expensive liquid of cyanide gold-leaching being carried out extracting and separating.
Background technology
China's gold resource is relatively abundanter, distributed more widely, but easily selects gold ore resource at full stretch, and difficulty is selected, difficulty is smelted and low-grade gold is more.Therefore, the difficulty that accounts for the suitable vast scale of China's gold reserve is selected comprehensive, reasonable, the effectively development and use of smelting gold resource, and the Sustainable development for China's gold resource has important and practical meanings.In the extraction of gold is smelted, in the smelting of particularly difficult choosing, difficult smelting and low-grade gold, still adopt the cyanide process extract technology at present.Therefore, adopt advanced practical new technology, gold (I) in the cyanide gold-leaching lean solution is carried out high efficiency separation extraction and enrichment, have great importance and act on for the technical progress that promotes China's gold smelting industry and cleaner production.
In the smelting for gold in difficulty choosing, difficult smelting and the low-grade gold, still adopt methods such as cyanide process leaching, zinc dust precipitation or the absorption of charcoal slurry at present, tediously long, the inefficiency of these method technologies.How efficiently extracting gold (I) from alkaline cyanide liquid is the focus that people pay close attention to always.Though use the tertiary amines extraction agent, the percentage extraction [document 1-2] that extracting gold obtains higher in acidity or neutral solution.But because of resulting cyanide gold-leaching liquid in the actual gold smelting is basic solution, for this alkalescence gold leachate, when adopting single tertiary amine extraction agent to extract, percentage extraction is very low, is difficult to accomplish the end in view.Therefore, adopt the tertiary amines extraction agent that the gold in the alkaline gold leachate (I) is carried out extracting and enriching, must improve this extraction system, so that the extracted organic phase after the improvement is extracted golden cyanogen complex ion in the alkaline environment, thereby be the separation and concentration of gold (I) in the cyanide gold-leaching liquid, a kind of practicable novel method is provided.
There are some researches show, in amine extractant, add suitable synergist, can improve the balance pH value of amine extractant, make amine extractant obtain effect preferably in extracting gold under the alkaline condition.Form organic phase with n-octyl amine and tbp (TBP) with kerosene as document [3], the gold (I) in the extraction aurous cyanide potassium solution has obtained higher percentage extraction.But when the gold in the organic phase (I) was carried out back extraction, back extraction ratio was very low, is difficult to get a desired effect.
Reference:
[1] Wang Wenming, Li Junheng, Zhang Jianmin etc. the back extraction of three-n-octyl amine extracting gold and gold. gold, 1987, (4): 52
[2] water hold quiet, Yang Tianjian, Bin Wanda. use TOA-CCl
4Gold in the extraction hydrochloric acid medium. precious metal, 1998,19 (2): 34
[3] Ma Liangbang, Fan Biwei, the gold [J] of .TBP such as Ning Lirong and amine extraction alkaline cyanide. precious metal .2004,25 (4): 6-11.
Summary of the invention
Existing problem during at the gold (I) of existing amine extractant in the expensive liquid of extraction cyanide gold-leaching, obtain higher percentage extraction as its extracting gold in acidity or neutral solution, but extraction efficiency is low under alkaline condition, and be difficult to problems such as back extraction, the invention provides in the expensive liquid of a kind of extracting and enriching cyanide gold-leaching the method for gold (I), it is low and be difficult for problem such as back extraction to gold (I) extraction efficiency under alkaline condition to have overcome in the past amine extractant.
For reaching above-mentioned purpose, patent of the present invention adopts following technical scheme:
The method of gold (I) is as follows in the expensive liquid of extracting and enriching cyanide gold-leaching of the present invention: extraction agent is carried out acidification with hydrochloric acid, sulfuric acid, phosphoric acid or the salpeter solution of 0.01～2.0mol/L, and then with 0.01～0.2mol/L sodium bicarbonate mixing contact equilibrium, promptly obtain the modification extraction agent; Modification extraction agent, synergist and thinner are mixed with the volume ratio of 1～50:1～50:50～98, form the organic phase of extraction system; Organic phase contacts and fully stirs with the volume ratio mixing of the expensive liquid of alkaline cyanide gold-leaching with 1:1～25, to the Au in the gold immersing liquid (CN)
2 -Extract, make the aurum cyanogen anionic complex Au (CN) in the expensive liquid of alkaline cyanide gold-leaching
2 -Be extracted in the organic phase; Load the organic phase of aurum cyanogen anionic complex mix to contact with the volume ratio of 1～20:1 with the reverse-extraction agent alkaline solution again and carry out back extraction, aurum cyanogen anionic complex is transferred in the strip liquor, gold leaching solution reuse after the raffinate continues to soak gold, and the organic phase after the back extraction also recycles;
Described extraction agent is preferred: any or any two the above mixture in trialkyl tertiary amine (N235), TNA trinonylamine, the trioctylamine;
Described synergist is neutral organophosphorus type or neutral phosphonic oxygen type extraction agent, and is preferred: any one or two kinds of mixture in trialkyl phosphine (TRPO), the trioctyl phosphine oxide (TOPO);
Described thinner is dissolved in wherein organic solvent for making described modification extraction agent and synergist, and is preferred: any one or two kinds of above mixtures in kerosene, sulfonated kerosene or the anthracite oil;
Described reverse-extraction agent is any or any two the above mixed ammonium/alkali solutions in sodium hydroxide solution, potassium hydroxide solution, sodium carbonate solution, the solution of potassium carbonate, and the concentration of the hydroxide ion in the alkaline solution is 0.01～5.0 mol.
As a preferred version, described modification extraction agent, synergist and thinner mix with the volume ratio of 5～30:5～30:50～90.
The alkaline golden cyanogen leach liquor of gained contained gold-cyanide complex when the expensive liquid of described alkaline cyanide gold-leaching leached auriferous Gold Ore breeze or auriferous slag for adopting cyanide process.
In gold smelting, the pH of cyanide process gold leaching solution is about 9～10 at present, and the concentration of gold (I) is low, and is general in the scope of several mg/L～tens mg/L.Method of the prior art is to adopt zinc powder reduction substitution method or active carbon adsorption etc., carries out separation and concentration through a series of more tediously long technologies.The problem of this method is that the loss of gold is big, the rate of recovery is low, cost recovery is high, technology is tediously long, and the enrichment extraction problem of low-concentration gold leach liquor is difficult to break through.When carrying out the extracting and enriching of alkaline golden cyanogen GOLD FROM PLATING SOLUTION (I) with N235 separately, percentage extraction is very low, and difficulty accomplishes the end in view.
Present method is to the gold (I) of lower concentration in the cyanide gold-leaching liquid, as golden starting point concentration in the feed liquid is about 10mg/L, when organic phase consists of 10%N235+10%TRPO+80% kerosene (being volume ratio), when the volume ratio V of organic phase and gold immersing liquid (O): V (A)=1:3, percentage extraction can reach 96.31%.When the sodium hydroxide solution of employing 0.05mol/L carried out back extraction, back extraction ratio can reach 91.47%, and gold (I) concentration is 26.43mg/L in the strip liquor.In addition, still can compare, the conditions such as concentration of alkali in extractant concentration, the back extraction mutually in the organic phase, obtain better enrichment method effect by change.Therefore, this novel method has advantages such as efficient, quick, energy-conservation.
Embodiment
Embodiment 1:
The hydrochloric acid soln that with concentration is 0.05mol/L contacts 5 minute by equal-volume than mixing with N235, and then with isopyknic concentration be that resulting organic phase is the modified amine extraction agent behind the sodium hydrogen carbonate solution contact equilibrium of 0.02mol/L.
Measuring 1 part of modified amine extraction agent, 1 part of TRPO and 8 parts of kerosene by volume respectively mixes in extraction tank, the starting point concentration that adds 30 parts of gold (I) is the expensive liquid of alkaline cyanide gold-leaching (feed liquid) of 10.00mg/L, stirring or oscillation extraction made and reach extraction equilibrium in 10 minutes, leave standstill phase-splitting, percentage extraction is 96.31%, and raffinate continues reuse; Use the sodium hydroxide solution back extraction of 10 parts of 0.05mol/L then, back extraction ratio reaches 91.5%, and the organic phase after the back extraction continues reuse.Obtained the concentration effect of good extraction, back extraction.
Embodiment 2:
Be that the sulphuric acid soln of 0.02mol/L mixes with isopyknic N235 and contacts 5 minutes with concentration, and then with isopyknic concentration be that resulting organic phase is described modified amine extraction agent behind the sodium hydrogen carbonate solution contact equilibrium of 0.01mol/L.
Measuring 2 parts of modified amine extraction agents, 1 part of TRPO and 7 parts of kerosene by volume respectively mixes in extraction tank, the starting point concentration that adds 50 parts of gold (I) is the expensive liquid of alkaline cyanide gold-leaching (feed liquid) of 5.44mg/L, stirring or oscillation extraction made and reach extraction equilibrium in 10 minutes, leave standstill phase-splitting, percentage extraction is 96.17%, and raffinate continues reuse; Then, with the sodium hydroxide solution back extraction of 10 parts of 0.05mo1/L, back extraction ratio reaches 90.01%, and the organic phase after the back extraction continues reuse.Obtained the concentration effect of good extraction, back extraction.Under lower gold (I) starting point concentration, also can obtain good extraction, back extraction concentration effect.
Embodiment 3:
The salpeter solution that with concentration is 1.0mol/L contacts 5 minute by equal-volume than mixing with N235, and then with isopyknic concentration be that resulting organic phase is described modified amine extraction agent behind the sodium hydrogen carbonate solution contact equilibrium of 0.1 mol.
Form with the same organic phase of embodiment one and volume in, adding 20 parts of gold (I) starting point concentration is the gold immersing liquid of 21.74mg/L, reach extraction equilibrium after, leave standstill phase-splitting, measuring after the calculating percentage extraction to be 97.37%; Use the sodium hydroxide back extraction of 10 parts of 0.05mol/L again, back extraction ratio is 90.7%.Under higher starting point concentration, good extraction, concentration effect have been obtained equally.
Embodiment 4:
Be that the salpeter solution of 0.02mol/L contacts with the mixture of isopyknic trioctylamine and TNA trinonylamine and mixed 5 minutes with concentration, and then with isopyknic concentration be that resulting organic phase is the modified amine extraction agent behind the sodium hydrogen carbonate solution contact equilibrium of 0.01 mol.
Modified amine extraction agent, TRPO and kerosene mixed in extraction tank by the volume ratio of 15:10:75 becomes organic phase, by the ratio of organic phase and feed liquid is that the starting point concentration that 1:4 adds 40 parts of gold (I) is the expensive liquid of alkaline cyanide gold-leaching (feed liquid) of 5.44mg/L, extract to make in 10 minutes and reach extraction equilibrium, leave standstill phase-splitting, recording percentage extraction is 95.40%, and raffinate continues reuse; And then with the potassium hydroxide solution back extraction of 10 parts of 0.05mol/L, recording back extraction ratio is 95.2%, and the organic phase after the back extraction continues reuse.Obtained the concentration effect of good extraction, back extraction.Under lower gold (I) starting point concentration, also can obtain good extraction, back extraction concentration effect
Embodiment 5:
Be that the salpeter solution of 2mol/L contacts with the mixture of isopyknic trioctylamine and TNA trinonylamine and mixed 5 minutes with concentration, and then with isopyknic concentration be that resulting organic phase is the modified amine extraction agent behind the sodium hydrogen carbonate solution contact equilibrium of 0.2 mol.
Modified amine extraction agent, TOPO, anthracite oil are mixed in extraction tank by the volume ratio of 10:5:85, the starting point concentration that adds 30 parts of gold (I) is the expensive liquid of alkaline cyanide gold-leaching (feed liquid) of 10.00mg/L, extract to make in 10 minutes and reach extraction equilibrium, leave standstill phase-splitting, recording percentage extraction is 95.50%, and raffinate continues reuse; Then, the sodium carbonate solution back extraction with 10 parts of 0.15mol/L records back extraction ratio and reaches 93.16%, and the organic phase after the back extraction continues reuse.Obtained the concentration effect of good extraction, back extraction.Under lower gold (I) starting point concentration, also can obtain good extraction, back extraction concentration effect.
Embodiment 6:
Similarly to Example 4 modified amine extraction agent, trioctyl phosphine oxide, sulfonated kerosene are mixed in extraction tank by the volume ratio of 15:15:70, is the alkaline cyanide gold-leaching expensive liquid (feed liquid) of 10.0mg/L with material liquid volume than the starting point concentration that adds 40 parts of gold (I) for 1:4 by organic phase, extract to make in 10 minutes and reach extraction equilibrium, leave standstill phase-splitting, recording percentage extraction is 93.9%, and raffinate continues reuse; Then, the sodium carbonate solution back extraction with 10 parts of 0.1mol/L records back extraction ratio and reaches 92.5%, and the organic phase after the back extraction continues reuse.Obtained the concentration effect of good extraction, back extraction.Under lower or higher gold (I) starting point concentration, also can obtain good extraction, back extraction concentration effect.
Embodiment 7:
Measuring 1 part of N235 extraction agent, 1 part of TRPO and 8 parts of kerosene respectively for 1:1:8 by volume mixes in extraction tank and is organic phase, the starting point concentration that adds 15 parts of gold (I) is the expensive liquid of alkaline cyanide gold-leaching (feed liquid) of 10.0mg/L, stirring or oscillation extraction made and reach extraction equilibrium in 10 minutes, and left standstill phase-splitting.Residue gold (I) concentration knows that percentage extraction is 97.1% in surveying raffinate, and raffinate continues reuse; Use the sodium hydroxide solution back extraction of 10 parts of 0.06mol/L then, back extraction ratio reaches 91.4%, and the organic phase after the back extraction continues reuse.Under lower or higher gold (I) starting point concentration, also can obtain good extraction, back extraction concentration effect.
Claims (5)
1, the method for gold (I) in the expensive liquid of a kind of extracting and enriching cyanide gold-leaching, it is characterized in that: extraction agent is carried out acidification with hydrochloric acid, sulfuric acid, phosphoric acid or the salpeter solution of 0.01～2.0mol/L, and then with 0.01～0.2mol/L sodium bicarbonate mixing contact equilibrium, promptly obtain the modification extraction agent; Modification extraction agent, synergist and thinner are mixed with the volume ratio of 1～50:1～50:30～98, form the organic phase of extraction system; Organic phase contacts and fully stirs with the volume ratio mixing of the expensive liquid of alkaline cyanide gold-leaching with 1:1～25, to the Au in the gold immersing liquid (CN)
2 -Extract, make the aurum cyanogen anionic complex Au (CN) in the expensive liquid of alkaline cyanide gold-leaching
2 -Be extracted in the organic phase; Load the organic phase of aurum cyanogen anionic complex mix to contact with 1～20:1 volume ratio with the reverse-extraction agent alkaline solution again and carry out back extraction, aurum cyanogen anionic complex is transferred in the strip liquor, the gold leaching solution reuse after the raffinate continues to soak gold, the organic phase after the back extraction also recycles;
Described extraction agent is any or any two the above mixture in trialkyl tertiary amine, TNA trinonylamine, the trioctylamine;
Described synergist is neutral organophosphorus type or neutral phosphonic oxygen type extraction agent;
Described thinner is dissolved in wherein organic solvent for making described modification extraction agent and synergist;
Described reverse-extraction agent is any or any two the above mixed ammonium/alkali solutions in sodium hydroxide solution, potassium hydroxide solution, sodium carbonate solution, the solution of potassium carbonate, and the concentration of the hydroxide ion in the alkaline solution is 0.01～5.0 mol.
2, method according to claim 1 is characterized in that: described synergist is the mixture of any or this two kinds of materials in trialkyl phosphine, the trioctyl phosphine oxide;
3, method according to claim 1 is characterized in that: described thinner is any or any two the above mixture in kerosene, sulfonated kerosene or the anthracite oil.
4, method according to claim 1 is characterized in that: described modification extraction agent, synergist and thinner are to mix with the volume ratio of 5～30:5～30:50～90.
5, method according to claim 1 is characterized in that: the alkaline golden cyanogen leach liquor of gained when the expensive liquid of described alkaline cyanide gold-leaching leaches auriferous Gold Ore breeze or auriferous slag for adopting cyanide process, contain gold-cyanide complex.
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| TBP与胺萃取碱性氰化物中的金. 马亮帮，范必威，宁丽荣，刘文宏.贵金属，第25卷第4期. 2004 * |
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