CN108823416A - The extracting method of gold, silver in a kind of clay-graphite crucible slag - Google Patents
The extracting method of gold, silver in a kind of clay-graphite crucible slag Download PDFInfo
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- CN108823416A CN108823416A CN201810738261.1A CN201810738261A CN108823416A CN 108823416 A CN108823416 A CN 108823416A CN 201810738261 A CN201810738261 A CN 201810738261A CN 108823416 A CN108823416 A CN 108823416A
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting 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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a kind of extracting methods of gold, silver in clay-graphite crucible slag, include the following steps：Clay-graphite crucible ground-slag end is reacted with sulfuric acid/silicofluoric acid mixed liquor, and through supercooling, filter residue and filtrate is obtained by filtration in washing；After filter residue and drying, high-temperature calcination, then cooling grinding obtains enrichment slag；Enrichment slag is placed in nitric acid solution, normal-temperature reaction, then dilute filtration obtains leached mud I and leachate I, and the reduction of leachate I mentions silver；Leached mud I is placed in chloroazotic acid, and dilute filtration obtains leached mud II and leachate II after fully reacting, and the reduction of leachate II mentions gold.The clay-graphite crucible slag of the application first react with sulfuric acid/fluosilicic acid mixed liquor before being calcined, can be avoided that clay-graphite crucible slag during calcining is blocking, is realized golden and silver-colored separating with other impurities, is improved the leaching rate of recovery of gold, silver.
Description
Technical field
The invention belongs to nonferrous metals recycling technical fields, and in particular to gold, silver mentions in a kind of clay-graphite crucible slag
Take method.
Background technique
When due to pyrometallurgical smelting metal, cast is carried out to the metal after melting commonly using clay-graphite crucible, is poured
Shi Huiyou a small amount of crude metal penetrates into crucible.Crucible is used for multiple times, in the metal of crucible internal walls meeting enriched.Especially
When smelting gold, it is enriched with more Jin Heyin in clay-graphite crucible used, gold, silver are the noble metals of high value, have pole
High economic recovery value.
Leaf will discloses clearly a kind of method (number of patent application that indium, germanium in pyrometallurgical smelting crucible residues are extracted using Whote-wet method
The method that CN201010169155.X Whote-wet method extracts indium, germanium in pyrometallurgical smelting crucible residues), indium is leached using dilute sulfuric acid, then
Using MnO2It does the oxidant concentrated sulfuric acid and leaches germanium, may be implemented that most of germanium, indium is separately recovered, and be able to maintain higher
The rate of recovery.It is less to the research for extracting metallic gold and silver from clay-graphite crucible slag, because containing in clay-graphite crucible slag
Clay component if directlying adopt nitric acid and chloroazotic acid leach and extracts gold and silver therein, or first passes through calcination processing and adds nitre again
Acid and chloroazotic acid leach, and all cannot effectively extract the Jin Heyin in clay-graphite crucible slag, and the rate of recovery is almost nil, therefore, existing
Gold and silver-colored certain technical difficulty are recycled from clay-graphite crucible slag with the presence of technology.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of extraction of gold, silver in clay-graphite crucible slag
Method.
The present invention provides a kind of extracting methods of gold, silver in clay-graphite crucible slag, include the following steps：
1) clay-graphite crucible ground-slag end is reacted at 50-70 DEG C with sulfuric acid/silicofluoric acid mixed liquor, after the reaction was completed
Filter residue is obtained by filtration in mixed solution；
2) filter residue is calcined at 900-1000 DEG C after drying, and then processing obtains powdered enrichment slag；
3) enrichment slag is placed in nitric acid solution, stirring at normal temperature carries out Leach reaction, the mixed solution warp after fully reacting
Dilution is crossed, leached mud I and leachate I is obtained by filtration, leachate I extracts silver by reduction；
4) leached mud I is placed in chloroazotic acid, and stirring carries out Leach reaction, the mixed solution after fully reacting at 50~80 DEG C
By dilution, leachate II is obtained by filtration, leachate II extracts gold by reduction.
Preferably, the partial size at the end of clay-graphite crucible ground-slag described in step 1) is 150-325 mesh.
Preferably, the concentration of sulfuric acid is 80-150g/L in sulfuric acid described in step 1)/silicofluoric acid mixed liquor, and silicofluoric acid is dense
Degree is 100-340g/L.
Preferably, the end of clay-graphite crucible ground-slag described in step 1) and sulfuric acid/silicofluoric acid mixed liquor mass volume ratio
It is 1:1-3g/ml.
Preferably, the reaction time described in step 1) is 6-12h.
Preferably, calcination time described in step 2) is 1.5-3h.
Preferably, the concentration of nitric acid solution described in step 3) is 63-130g/L.
Preferably, enrichment slag described in step 3) and the mass volume ratio of nitric acid solution are 1:1-5g/ml.
Preferably, the mass volume ratio of leached mud I described in step 4) and chloroazotic acid is 1:1-5g/ml.
Preferably, the time of Leach reaction described in step 4) is 4-6h.
The present invention provides a kind of extracting method of gold, silver in clay-graphite crucible slag, most preferred steps are as follows：
1) the clay-graphite crucible ground-slag end that partial size is 325 mesh is stirred instead with sulfuric acid/silicofluoric acid mixed liquor at 70 DEG C
6h is answered, mixed solution after the reaction was completed is washed to neutrality, filter residue and filtrate is obtained by filtration by being cooled to room temperature；Wherein sulphur
The concentration of sulfuric acid is 150g/L in acid/silicofluoric acid mixed liquor, and fluosilicic acid concentration is 340g/L；Clay-graphite crucible ground-slag end and sulphur
Acid/silicofluoric acid mixed liquor mass volume ratio is 1:1g/ml；
2) filter residue calcines 1.5h, calcined filter residue is ground through supercooling at 105 DEG C after dry 12h at 1000 DEG C
Mill, obtains powdered enrichment slag；
3) slag will be enriched with to be placed in the nitric acid solution that concentration is 130g/L, stirring at normal temperature carries out Leach reaction 6h, has reacted
Mixed solution after complete dilutes 5 times, and leached mud I and leachate I is obtained by filtration, and leachate I extracts silver by reduction；Wherein it is enriched with
Slag and the mass volume ratio of nitric acid solution are 1:1g/ml；
4) leached mud I is placed in chloroazotic acid, and stirring carries out Leach reaction 6h at 80 DEG C, the mixed solution warp after fully reacting
Dilution is crossed, leachate II and leached mud II is obtained by filtration, leachate II extracts gold by reduction；Wherein leached mud I and chloroazotic acid
Mass volume ratio is 1:1g/ml.
Using the recovery rate highest for the Jin Heyin that optimal step obtains.
Mixed solution after fully reacting described in step 3) of the present invention dilutes 3-5 times, and I He of leached mud is then obtained by filtration
Leachate I.
Filtering can obtain leachate II and leached mud II in step 4) of the present invention, and leached mud II can continue to back to step
Rapid 3) middle replacement enrichment slag, further extracts Jin Heyin.
Clay-graphite crucible ground-slag of the present invention end is ground up, sieved by clay-graphite crucible slag.
Clay-graphite crucible slag of the present invention is the pyrogenic process by scrapping to Chenzhou City Jingui Silver Industry Co., Ltd
Smelt what golden clay-graphite crucible crushed, wherein the mass percent of the metallic element in clay-graphite crucible slag is：
Golden (Au)：0.013%, silver (Ag) 5.284%, copper (Cu)：0.710%.
Clay-graphite crucible refers to using graphite, silicon carbide, silica, clay, pitch and tar as one made of raw material firing
Class crucible.Usually wherein the content of graphite is 35~55%, and the content of aggregate is (such as：Silicon carbide) 25-45%, the content of clay
For：15~25% and a small amount of pitch and tar.
The condition of filter residue and drying is in step 3) in the extracting method of gold, silver in clay-graphite crucible slag of the present invention：
105 DEG C of drying temperature, drying time 12h.
Silicofluoric acid of the present invention is the electrolyte of Chenzhou City Jingui Silver Industry Co., Ltd lead electrolysis.
Sulfuric acid of the present invention/silicofluoric acid mixed liquor is to be mixed to get the concentrated sulfuric acid, silicofluoric acid and deionized water.
Currently, everybody is less to the metal recovery research in the crucible residues of pyrometallurgical smelting metal, number of patent application
CN201010169155.X discloses a kind of method that Whote-wet method extracts indium, germanium in pyrometallurgical smelting crucible residues, is soaked using dilute sulfuric acid
Then indium out uses MnO2It does the oxidant concentrated sulfuric acid and leaches germanium, may be implemented that most of germanium, indium is separately recovered, and energy
Keep the higher rate of recovery.Recycled from metal smelt slag at present Jin Heyin be nitric acid and chloroazotic acid is directlyed adopt to leach, therefore
On the basis of the prior art, those skilled in the art are it is conceivable that using in wet underwater welding the application clay-graphite crucible slag
Gold, silver, but the inventor of the present application found through research that, directly leached in clay-graphite crucible slag with nitric acid and chloroazotic acid
Gold, silver can make the recovery rate of Jin Heyin substantially reduce, and impurity is more, and obtained metal purity is not high, and practical value reduces.
In addition, if directly calcining to clay-graphite crucible slag, clay-graphite crucible slag can be sintered blocking, influence later period gold, silver
Extraction effect.Therefore present inventor expects the clay component in clay-graphite crucible slag to be removed, and removes at present viscous
The conventional method of soil is to be leached with hydrofluoric acid, but the method pollution is larger, and leaching effect is bad.The application first uses sulfuric acid/fluosilicic
Sour mixed liquor at 50-70 DEG C with clay-graphite crucible slag powdered reaction, wherein in sulfuric acid/silicofluoric acid mixed liquor sulfuric acid concentration
For 80-150g/L, fluosilicic acid concentration is 100-340g/L, can effectively remove clay component therein, avoid forging in the later period
It is blocking during burning, influence the extraction effect of later period gold, silver.
The application combines the Jin Heyin extracted in clay-graphite crucible slag using pyrogenic process and wet process, compared to only with wet
The recovery rate of method, the application gold and silver greatly improves.And the clay-graphite crucible slag of the application before calcining first with
Sulfuric acid/fluosilicic acid mixed liquor reaction, then calcined at 900-1000 DEG C, the method finally leached respectively with acid and chloroazotic acid by gold and
Silver is separated, compared to the dinectly bruning without the processing of persulfuric acid/fluosilicic acid mixed liquor, the application elder generation and sulphur before being calcined
The reaction of acid/fluosilicic acid mixed liquor, can be avoided during calcining that clay-graphite crucible ground-slag end is blocking, eliminate graphite earthenware
Most copper in crucible slag, realization gold and silver are separated with other impurities, improve the leaching rate of recovery of gold, silver, and this
Such operation order is taken in invention, and gold and silver can be made to separate to the greatest extent with other impurities, and the leaching for improving gold, silver is returned
Yield.
The beneficial effects of the invention are as follows：
1, the application combines the Jin Heyin extracted in clay-graphite crucible slag using pyrogenic process and wet process, compared to only with
The recovery rate of wet process, the application gold and silver greatly improves.
2, the application first use sulfuric acid/silicofluoric acid mixed liquor at 50-70 DEG C with clay-graphite crucible slag powdered reaction, wherein
The concentration of sulfuric acid is 80-150g/L in sulfuric acid/silicofluoric acid mixed liquor, and fluosilicic acid concentration is 100-340g/L, can effectively be removed
Clay component therein, avoids blocking in the calcination process in later period, influences the extraction effect of later period gold, silver.
3, the clay-graphite crucible slag of the application is first reacted with sulfuric acid/fluosilicic acid mixed liquor before calcining, then
It calcines, is finally respectively separated Jin Heyin with the method that acid and chloroazotic acid leach, compared to without over cure at 900-1000 DEG C
Acid/fluosilicic acid mixed liquor is handled and dinectly bruning, and the application is first reacted with sulfuric acid/fluosilicic acid mixed liquor before being calcined, can
It avoids clay-graphite crucible slag during calcining blocking, realizes gold and silver-colored separating with other impurities, improve gold, silver
Leach the rate of recovery.
4, using operation order of the invention, gold and silver can be made to separate to the greatest extent with other impurities, improve it is golden,
The leaching rate of recovery of silver.
5, sufficient raw of the invention, cheap, production cost is low.
6, gold, silver do not disperse in extraction process of the invention, leach in two steps in enrichment slag, the first step leaches silver dollar
Element, second step leach gold element, can recycle gold, and can recycle silver, and be able to maintain higher recovery efficiency.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this hair
Bright further description.
Embodiment 1
1) the clay-graphite crucible ground-slag end that partial size is 150 mesh is stirred instead with sulfuric acid/silicofluoric acid mixed liquor at 50 DEG C
12h is answered, mixed solution after the reaction was completed is washed to neutrality, filter residue and filtrate is obtained by filtration by being cooled to room temperature；Wherein sulphur
The concentration of sulfuric acid is 80g/L in acid/silicofluoric acid mixed liquor, and fluosilicic acid concentration is 100g/L；Clay-graphite crucible ground-slag end and sulphur
Acid/silicofluoric acid mixed liquor mass volume ratio is 1:3g/ml；
2) filter residue after dry 12h, calcines 3h at 105 DEG C at 950 DEG C, and calcined filter residue is obtained through supercooling, grinding
To powdered enrichment slag；
3) slag will be enriched with to be placed in the nitric acid solution that concentration is 100g/L, stirring at normal temperature carries out Leach reaction 5h, has reacted
Mixed solution after complete dilutes 3 times, and leached mud I and leachate I is obtained by filtration, and leachate I extracts silver by reduction；Wherein it is enriched with
Slag and the mass volume ratio of nitric acid solution are 1:5g/ml；
4) leached mud I is placed in chloroazotic acid, and stirring carries out Leach reaction 5h at 50 DEG C, the mixed solution warp after fully reacting
Dilution is crossed, leachate II and leached mud II is obtained by filtration, leachate II extracts gold by reduction；Wherein leached mud I and chloroazotic acid
Mass volume ratio is 1:5g/ml.
Embodiment 2
1) the clay-graphite crucible ground-slag end that partial size is 200 mesh is stirred instead with sulfuric acid/silicofluoric acid mixed liquor at 60 DEG C
8h is answered, mixed solution after the reaction was completed is washed to neutrality, filter residue and filtrate is obtained by filtration by being cooled to room temperature；Wherein sulphur
The concentration of sulfuric acid is 100g/L in acid/silicofluoric acid mixed liquor, and fluosilicic acid concentration is 220g/L；Clay-graphite crucible ground-slag end and sulphur
Acid/silicofluoric acid mixed liquor mass volume ratio is 1:2g/ml；
2) filter residue after dry 12h, calcines 2h at 105 DEG C at 900 DEG C, and calcined filter residue is obtained through supercooling, grinding
To powdered enrichment slag；
3) slag will be enriched with to be placed in the nitric acid solution that concentration is 63g/L, stirring at normal temperature carries out Leach reaction 4h, fully reacting
Mixed solution afterwards dilutes 4 times, and leached mud I and leachate I is obtained by filtration, and leachate I extracts silver by reduction；Wherein it is enriched with slag
Mass volume ratio with nitric acid solution is 1:3g/ml；
4) leached mud I is placed in chloroazotic acid, and stirring carries out Leach reaction 4h at 60 DEG C, the mixed solution warp after fully reacting
Dilution is crossed, leachate II and leached mud II is obtained by filtration, leachate II extracts gold by reduction；Wherein leached mud I and chloroazotic acid
Mass volume ratio is 1:2g/ml.
Embodiment 3
1) the clay-graphite crucible ground-slag end that partial size is 325 mesh is stirred instead with sulfuric acid/silicofluoric acid mixed liquor at 70 DEG C
6h is answered, mixed solution after the reaction was completed is washed to neutrality, filter residue and filtrate is obtained by filtration by being cooled to room temperature；Wherein sulphur
The concentration of sulfuric acid is 150g/L in acid/silicofluoric acid mixed liquor, and fluosilicic acid concentration is 340g/L；Clay-graphite crucible ground-slag end and sulphur
Acid/silicofluoric acid mixed liquor mass volume ratio is 1:1g/ml；
2) filter residue calcines 1.5h, calcined filter residue is ground through supercooling at 105 DEG C after dry 12h at 1000 DEG C
Mill, obtains powdered enrichment slag；
3) slag will be enriched with to be placed in the nitric acid solution that concentration is 130g/L, stirring at normal temperature carries out Leach reaction 6h, has reacted
Mixed solution after complete dilutes 5 times, and leached mud I and leachate I is obtained by filtration, and leachate I extracts silver by reduction；Wherein it is enriched with
Slag and the mass volume ratio of nitric acid solution are 1:1g/ml；
4) leached mud I is placed in chloroazotic acid, and stirring carries out Leach reaction 6h at 80 DEG C, the mixed solution warp after fully reacting
Dilution is crossed, leachate II and leached mud II is obtained by filtration, leachate II extracts gold by reduction；Wherein leached mud I and chloroazotic acid
Mass volume ratio is 1:1g/ml.
Comparative example 1
1) the clay-graphite crucible ground-slag end that partial size is 200 mesh after dry 12h, is calcined at 105 DEG C at 900 DEG C
2h, calcined filter residue obtain powdered enrichment slag through supercooling, grinding；
2) slag will be enriched with to be placed in the nitric acid solution that concentration is 63g/L, stirring at normal temperature carries out Leach reaction 4h, fully reacting
Mixed solution afterwards dilutes 4 times, and leached mud I and leachate I is obtained by filtration, and leachate I extracts silver by reduction；Wherein it is enriched with slag
Mass volume ratio with nitric acid solution is 1:3g/ml；
3) leached mud I is placed in chloroazotic acid, and stirring carries out Leach reaction 4h at 60 DEG C, the mixed solution warp after fully reacting
Dilution is crossed, leachate II and leached mud II is obtained by filtration, leachate II extracts gold by reduction；Wherein leached mud I and chloroazotic acid
Mass volume ratio is 1:2g/ml.
Comparative example 2
1) the clay-graphite crucible ground-slag end that partial size is 200 mesh is placed in concentration is in the nitric acid solution of 63g/L, and room temperature stirs
It mixes and carries out Leach reaction 4h, leached mud I and leachate I, leachate is obtained by filtration by dilution in the mixed solution after fully reacting
I extracts silver by reduction；Wherein the mass volume ratio of clay-graphite crucible ground-slag end and nitric acid solution is 1:3g/ml；
2) leached mud I is placed in chloroazotic acid, and stirring carries out Leach reaction 4h at 60 DEG C, the mixed solution warp after fully reacting
Dilution is crossed, leachate II and leached mud II is obtained by filtration, leachate II extracts gold by reduction；Wherein leached mud I and chloroazotic acid
Mass volume ratio is 1:2g/ml.
The clay-graphite crucible ground-slag end for measuring embodiment 2 respectively obtains after persulfuric acid/silicofluoric acid mixed liquor Leach reaction
The mass change and calcined state of the clay-graphite crucible ground-slag end of the filter residue arrived and comparative example 1 calcining front and back, as a result
Such as table 1.
The mass change and calcined state at 1 clay-graphite crucible ground-slag end of table and filter residue calcining front and back
From the data in table 1 it is found that the clay-graphite crucible ground-slag end of embodiment 2 is soaked through persulfuric acid/silicofluoric acid mixed liquor
After calcining, quality is reduced, and illustrates at the clay-graphite crucible ground-slag end of obtained filter residue and comparative example 1 after reacting out
In calcination process, inflammable component therein is eliminated, has achieved the purpose that calcination removal of impurities.In addition, the clay graphite earthenware of embodiment 2
The filter residue that crucible ground-slag end obtains after persulfuric acid/silicofluoric acid mixed liquor Leach reaction, the quality after 900 DEG C of high-temperature calcinations subtract
A small amount of Mass lost amount being significantly greater than after 1 clay-graphite crucible ground-slag end of comparative example is calcined as former state, and the clay of comparative example 1
It is blocking that graphite crucible ground-slag end is easy sintering；Illustrate to improve clay-graphite crucible slag through persulfuric acid/silicofluoric acid mixed liquor processing
The combustion rate of oxidizable combustion components in powder, improves calcining dust removal rate, and will not be sintered by high-temperature calcination it is blocking,
Improve the recovery rate of later period gold, silver.
Measure clay-graphite crucible ground-slag end in embodiment 1, leached mud I, leachate I, leached mud II and leachate II this 5
The content of golden (Au), silver (Ag) and copper (Cu) in kind substance, and thus calculate in embodiment 2 in clay-graphite crucible ground-slag end
The recovery rate of Au, Ag, as a result such as table 2.
The content of Au, Ag and Cu and the recovery rate of Au, Ag in each substance of table 2
| Substance | The content of Au | The content of Ag | The content of Cu |
| Clay-graphite crucible ground-slag is last (50g) | 0.013% | 5.284% | 0.71% |
| Leachate I (75mL) | 0.06mg/L | 33.113g/L | 0.07mg/L |
| Leached mud I (22.355g) | 0.0288% | 0.71% | 0% |
| Leachate II (50mL) | 0.119g/L | 4.01mg/L | 0mg/L |
| Leached mud II (22.349g) | 0.002% | 0.704% | 0% |
| Recovery rate (%) | 91.54% | 94.00% | — |
From the data in table 2 it is found that from clay-graphite crucible ground-slag end in the present invention is through persulfuric acid/silicofluoric acid mixed liquor
After reason, copper therein is largely removed, and realizes the separation of copper and Jin Heyin well, improves final gold and silver
Extraction efficiency, the recovery rate of gold and silver is respectively 92.54% He in clay-graphite crucible ground-slag end in the embodiment of the present invention 1
94.00%, recovery rate is high, can effectively be recycled respectively to the gold, silver in clay-graphite crucible slag.
The recovery rate for measuring gold and silver in the clay-graphite crucible ground-slag end of embodiment 1-3 and comparative example 1-2, as a result such as table
3。
The recovery rate of gold and silver in 3 clay-graphite crucible ground-slag end of table
| Embodiment | Au plasma rate (%) | The recovery rate (%) of silver |
| Embodiment 1 | 90.04% | 92.87% |
| Embodiment 2 | 91.54% | 94.00% |
| Embodiment 3 | 92.26% | 94.87% |
| Comparative example 1 | 7.66% | 4.34% |
| Comparative example 2 | 6.49% | 2.38% |
From the data in table 3 it is found that compared with comparative example, using method of the invention from clay-graphite crucible ground-slag end
The recovery rate for extracting gold and silver greatly improves, and most preferably embodiment 3, golden in clay-graphite crucible ground-slag end to mention
Rate is taken to reach 92.26%, silver-colored recovery rate reaches 94.87%.Illustrate that the application combines extraction clay using pyrogenic process and wet process
Jin Heyin in graphite crucible slag is greatly improved compared to only with wet process, the application gold and silver-colored recovery rate.And the application
Clay-graphite crucible slag first reacted with sulfuric acid/fluosilicic acid mixed liquor before being calcined, then calcined at 900-1000 DEG C,
Finally Jin Heyin is separated with the method that acid and chloroazotic acid leach respectively, at without persulfuric acid/fluosilicic acid mixed liquor
It manages and dinectly bruning, the application is first reacted with sulfuric acid/fluosilicic acid mixed liquor before being calcined, can be avoided during calcining
Clay-graphite crucible ground-slag end is blocking, eliminates copper most in graphite crucible slag, realizes gold and silver and other impurities
Separation, improves the leaching rate of recovery of gold, silver, and the present invention takes such operation order, can make Jin Heyin utmostly
Separated with other impurities, improve the leaching rate of recovery of gold, silver.
Claims (10)
1. the extracting method of gold, silver in a kind of clay-graphite crucible slag, which is characterized in that include the following steps：
1) clay-graphite crucible ground-slag end is reacted at 50-70 DEG C with sulfuric acid/silicofluoric acid mixed liquor, mixing after the reaction was completed
Filter residue is obtained by filtration in solution；
2) filter residue is calcined at 900-1000 DEG C after drying, and then processing obtains powdered enrichment slag；
3) enrichment slag is placed in nitric acid solution, stirring at normal temperature carries out Leach reaction, and the mixed solution after fully reacting is by dilute
It releases, leached mud I and leachate I is obtained by filtration, leachate I extracts silver by reduction；
4) leached mud I is placed in chloroazotic acid, and stirring carries out Leach reaction at 50~80 DEG C, and the mixed solution after fully reacting passes through
Dilution, is obtained by filtration leachate II, and leachate II extracts gold by reduction.
2. the extracting method of gold, silver in clay-graphite crucible slag as described in claim 1, which is characterized in that described in step 1)
The partial size at clay-graphite crucible ground-slag end is 150-325 mesh.
3. the extracting method of gold, silver in clay-graphite crucible slag as claimed in claim 1 or 2, which is characterized in that institute in step 1)
The concentration for stating sulfuric acid in sulfuric acid/silicofluoric acid mixed liquor is 80-150g/L, and fluosilicic acid concentration is 100-340g/L.
4. the extracting method of gold, silver in clay-graphite crucible slag as claimed in claim 1 or 2, which is characterized in that institute in step 1)
It states clay-graphite crucible ground-slag end and sulfuric acid/silicofluoric acid mixed liquor mass volume ratio is 1:1-3g/ml.
5. the extracting method of gold, silver in clay-graphite crucible slag as claimed in claim 1 or 2, which is characterized in that institute in step 1)
Stating the reaction time is 6-12h.
6. the extracting method of gold, silver in clay-graphite crucible slag as claimed in claim 1 or 2, which is characterized in that institute in step 2)
Stating calcination time is 1.5-3h.
7. the extracting method of gold, silver in clay-graphite crucible slag as claimed in claim 1 or 2, which is characterized in that institute in step 3)
The concentration for stating nitric acid solution is 63-130g/L.
8. the extracting method of gold, silver in clay-graphite crucible slag as claimed in claim 1 or 2, which is characterized in that institute in step 3)
The mass volume ratio for stating enrichment slag and nitric acid solution is 1:1-5g/ml.
9. the extracting method of gold, silver in clay-graphite crucible slag as claimed in claim 1 or 2, which is characterized in that institute in step 4)
The mass volume ratio for stating leached mud I and chloroazotic acid is 1:1-5g/ml.
10. the extracting method of gold, silver in clay-graphite crucible slag as claimed in claim 1 or 2, which is characterized in that in step 4)
The time of the Leach reaction is 4-6h.
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| CN106119548A (en) * | 2016-07-26 | 2016-11-16 | 招金矿业股份有限公司 | A kind of Whote-wet method smelting process of gold silver mud |
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| JP4399633B2 (en) * | 2004-03-19 | 2010-01-20 | Ｄｏｗａメタルマイン株式会社 | Processing method of workpiece |
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