CN106566928A - Method used for selective high-efficiency extraction of copper and bismuth from high-copper bismuth slag - Google Patents
Method used for selective high-efficiency extraction of copper and bismuth from high-copper bismuth slag Download PDFInfo
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- CN106566928A CN106566928A CN201610990078.1A CN201610990078A CN106566928A CN 106566928 A CN106566928 A CN 106566928A CN 201610990078 A CN201610990078 A CN 201610990078A CN 106566928 A CN106566928 A CN 106566928A
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
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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
The invention discloses a method used for selective high-efficiency extraction of copper and bismuth from high-copper bismuth slag. According to the method, high-copper bismuth slag is taken as a raw material; high-copper bismuth slag powder obtained via smashing, grinding, and sieving and a sulfuric acid solution are subjected to size mixing at a certain ratio, and are delivered into a high-pressure autoclave; rich oxygen is introduced into the high-pressure autoclave, and oxygen pressure in the high-pressure autoclave is controlled for oxidizing leaching, wherein in the oxidizing leaching process, leaching of Cu in the form of Cu2+ is realized, and selective separation of copper with other non-zero valent elements is realized; a copper-containing leachate is subjected to acid adjusting, and is subjected to rotational flow electrolysis directly so as to extract copper in the copper-containing leachate and obtain copper products; a leaching residue is subjected to leaching separation of bismuth with concentrated hydrochloric acid, sponge bismuth is obtained via electro-deposition, and product refined bismuth is obtained via refining of sponge bismuth; and the rest slag is delivered into a lead pyrometallurgy system for comprehensive recycling of non-zero valent elements such as Pb, Ag, and Au. No environment pollution is caused by the method, no three wastes are discharged, and the method is a clean metallurgy technology.
Description
Technical field
The present invention relates to selectivity efficient extracts copper, the technique of bismuth in a kind of bismuth slag from high-copper, belong to non-ferrous metal wet method
Field of metallurgy.
Background technology
During lead anode slurry reclaims gold, silver, in a kind of slag charge of precious metals containing lead refinement oxide later stage output, this slag charge is main
Containing valuable metals such as lead, bismuth, copper, antimony, gold, silver, its synthetical recovery value is considerable.Valuable gold inside synthetical recovery this slag
Category, to improving production economy benefit, making rational use of resources has great importance.
Chinese patent 200710034666.9 describes comprehensive extraction of valent metal in a kind of many metalliferous materials from bismuth-containing
Technique, the technique first leach copper, tellurium with sulphuric acid from many metalliferous materials of bismuth-containing；Add chlorinating agent and oxidant leaches bismuth, Ag
Then stayed in leached mud with PbSO4, PbCl2 form with AgCl forms, Pb, in leachate, be initially charged ammonia adjustment pH value and arrive
1.5 bismuth oxychloride slags for obtaining bismuth-containing 70%, the bismuth slag pyrometallurgical smelting is into thick bismuth or is directly processed into high-purity bismuth oxide；Leaching
Going out in liquid, copper is not deposited with ammonia complexation, pH being adjusted to 4.5 with Na2CO3, heavy tellurium obtains tellurium dioxide.Finally obtain copper-containing solution,
Copper electrodeposition output cupric is more than 90% copper powder again.
Chinese patent 200710035322 describes a kind of technique of reclaiming smelting essence bismuth in slag from bismuth, be a kind of pyrogenic process and
The technique that wet method is combined；Main technological route is first to leach bismuth hydrochloric acid for dreg, is leached into bismuth and copper in bismuth slag molten
Liquid, and the overwhelming majority such as lead, gold, silver, antimony in bismuth slag is entered in slag；Leached mud returns silver-colored smelting system, leachate Jing substeps
Hydrolysis respectively obtains chlorine oxygen bismuth and basic copper carbonate；Chlorine oxygen bismuth is further smart into after thick bismuth Jing converter or reduction smelting in reverberatory furnace
It is smelt smart bismuth；Basic copper carbonate is sold as copper metallurgy raw material.
Chinese patent 200510125630.2 describes valuable metal recovery technique in a kind of thick bismuth, and the technique adopts wet method
Being combined with pyrogenic process carries out the synthetical recovery of valuable metal, carries out water quenching, ball milling to material first, carries out leaching, washs and mistake
Filter, obtains antimony lead slag and leachate, and produced antimony lead slag is returned and turns lead smelting system after pyrogenic process system reclaims antimony, and produced leachate is used
Copper sponge replaces Au, Ag output gold silver mud therein, and output gold silver mud returns precious metal smelting system, to replacing after gold silver mud
Liquid is hydrolyzed heavy bismuth, is neutralized with lime water, chlorine oxygen bismuth is obtained after filtration, and Jing reduction melting is further refined into into thick bismuth
Smart bismuth, uses iron powder replacement Cu to filtrate, and heavy Cu, output copper sponge, the liquid after heavy Cu add Calx to be neutralized, Jing 2-3
Qualified discharge after level precipitation.
Techniques described above method is required for being hydrolyzed, in and/or the operation such as displacement, have that technological process is complicated, production
The problems such as cycle length, high supplies consumption and high production cost.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the invention provides one kind is extracted from selectivity efficient in high-copper bismuth slag
The technique of copper, bismuth, the technology have environmentally safe, without " three wastes " discharge, belong to clean metallurgical technology, flow process simply, behaviour
Work is convenient, reagent consumption is few, and running cost is low, synthetical recovery degree high, Selective Separation effect is good, scale is changeable, tool
There is stronger practicality.
In a kind of bismuth slag from high-copper, selectivity efficient extracts copper, the technique of bismuth, and substantially thinking is：It is with bismuth slag as raw material, first
Oxidation Leaching is carried out with sulfuric acid solution to which first, leachate Jing cyclone electrolytic cells reclaim copper；Leached mud uses salt Ore Leaching, leachate again
Jing cyclone electrolytic cells reclaim bismuth；Remaining slag is lead antimony silver slag, returns converter melting and reclaims other metals；Comprise the following steps：
A, broken pulverizing；By bulk high-copper bismuth slag material broken pulverizing to -100 mesh of granularity；
B, the high-copper bismuth ground-slag end for taking step a and sulphuric acid are poured in autoclave after sizing mixing, and controlling corresponding technical conditions carries out oxygen
Change and leach, during Oxidation Leaching, the Cu in high-copper bismuth slag is then with Cu2+Form is leached, so as to realize copper and other valuable gold
The separation of category；
C, the cupric leachate obtained by step b is directly carried out Jing after acid adjustment cyclone electrolytic cell extract copper therein, obtain qualified the moon
Pole copper products；
D, the leached mud obtained by step b is leached with a certain amount of hydrochloric acid solution, so as to realize that bismuth is separated with other metals；
E, it is bismuth chloride solution by the leachate obtained by step d, with zine plate as anode, titanium plate is negative electrode, control tank voltage 0.5～
0.8V, 600～1000 A/m of electric current density2, 8～1h of electrolysing period carries out the heavy bismuth of electrodeposition, obtains the sponge of purity more than 94.5%
Bismuth, the pyro-refining of sponge bismuth Jing obtain the smart bismuth of purity more than 99.99%；
F, by the remaining slag obtained by step d be lead antimony silver slag, return converter smelting reclaim lead, antimony, gold, silver valuable metal；
G, the useless electric effusion obtained by step e is neutralized, obtains basic zinc chloride product.
The composition of the high-copper bismuth slag is：Bi：20～45%；Pb：15～40%；Cu：10～25%；Ag：0.6～1.2%；
Sb3～8%.
The high-copper bismuth ground-slag end adopts oxygen-enriched for oxide isolation in autoclave Oxidation Leaching, its oxygen content more than 60%.
In the high-copper bismuth slag autoclave during Oxidation Leaching, its corresponding technical conditions of control is：Sulfuric acid concentration 60～
110g/L, liquid solid product 4～6: 1 L/kg of mass ratio, 75～90 DEG C of temperature, 0.4～1.0MPa of pressure in kettle, mixing speed
500～700 r/min, 1.5～3h of response time.
The step c cyclone electrolytic cell extracts the optimum process condition of copper：1.8～2.8V of tank voltage, electric current density 500～
800 A/m2, 48～72h of electrolysing period.
A certain amount of hydrochloric acid solution leaching condition of step d is：Concentration of hydrochloric acid be 90～150 g/L, liquid solid product matter
Amount ratio 3～5:1 L/kg, 2～3 h of extraction time, 70～90 DEG C of extraction temperature.
The nertralizer that electrodeposition waste liquid after the step e electro-deposition recovery bismuth is added when being processed is Calx, is adjusted
Endpoint pH 6～9, controls 65～85 DEG C of temperature, you can basic zinc chloride product is obtained, and zinc chloride product can add as feedstuff
Agent.
Above-mentioned concentrated sulphuric acid, hydrochloric acid, Calx and oxygen-enriched it is technical grade reagent.
Compared with the prior art, the present invention have environmentally safe, without " three wastes " discharge, belong to clean metallurgical technology,
Strong to adaptability to raw material, easy to operate, reagent consumption is few, and running cost is low, synthetical recovery degree high, Selective Separation effect
Well, scale is changeable, has the advantages that stronger practicality.
Description of the drawings
Fig. 1 is the process chart of the present invention.
Specific embodiment
Embodiment 1：
A, take 500g high-copper bismuth slag (Bi 32.49%；Cu 16.56%；Pb 30.37%；Sb 1.14%；Ag 9.32 kg/t；Au
It is -100 mesh 1.98g/t) to crush and be milled to granularity, pours in autoclave and aoxidized after sizing mixing with the sulfuric acid solution of 100 g/L
Leach decopper(ing), control technology condition：Liquid solid product mass ratio is 5:It is 0.8MPa, leaching that 1 L/kg, extraction time are 2h, oxygen is pressed
85 ± 3 DEG C of temperature control；Filter after leaching, the filtering residue for obtaining is as follows into lease making assay result：Bi 36.08%, Cu
2.32 g/t of 0.32%, Pb33.12%, Sb 1.82%, Ag9.97 kg/t, Au, slag rate are 90.68%, and copper leaching rate is
98.25%；
5000 ml of leachate volume of b, step a, containing 32.36 g/L of Cu, send copper cyclone electrolytic cell to extract copper；Copper cyclone electrolytic cell groove
Voltage is 2.5V, and electric current density is 600A/m2, electrolysis time is 2h, obtains electrolytic copper foil, and cupric is 99.95%；
C, by the leached mud of step a, leached with the hydrochloric acid solution that concentration is 130 g/L, liquid solid product mass ratio is 5:1 L/kg,
Extraction time is 3h, and extraction temperature control is at 85 DEG C；Filter after leaching, the filtering residue composition for obtaining is as follows：Bi 1.96%, Cu
4.16 g/t of 18.56 kg/t of 0.18%, Pb 53.12%, Sb 2.40%, Ag, Au, slag rate are 50.80%, and bismuth leaching rate is
96.95%；Leached mud returns silver-colored smelting system and reclaims silver, gold, lead etc.；
Leachate volume 4500ml of d, step c, bismuth-containing 65.24g/L, with zine plate as anode, titanium plate is negative electrode, controls tank voltage
0.8 V, 800 A/m of electric current density2, electrolysing period 10h carries out the heavy bismuth of electrodeposition, obtain sponge bismuth Jing assay and obtain bismuth-containing be
92.03%, sponge bismuth obtains smart bismuth Jing after pyro-refining, and bismuth-containing is 99.993%.
Embodiment 2：
A, take 500g high-copper bismuth slag (Bi 31.76%；Cu 15.42%；Pb 30.99%；Sb 1.18%；Ag 6.17 kg/t；Au
It is -100 mesh 1.71g/t) to crush and be milled to granularity, pours in autoclave and aoxidized after sizing mixing with the sulfuric acid solution of 100 g/L
Leach decopper(ing), control technology condition：Liquid solid product mass ratio is 5:It is 0.6MPa, leaching that 1 L/kg, extraction time are 2h, oxygen is pressed
80 ± 3 DEG C of temperature control；Filter after leaching, the filtering residue for obtaining is as follows into lease making assay result：Bi 35.84%, Cu
2.03 g/t of 0.45%, Pb34.01%, Sb 1.45%, Ag7.80 kg/t, Au, slag rate are 89.73%, and copper leaching rate is
97.74%；
5000 ml of leachate volume of b, step a, containing 30.17 g/L of Cu, send copper cyclone electrolytic cell to extract copper；Copper cyclone electrolytic cell groove
Voltage is 2.5V, and electric current density is 600A/m2, electrolysis time is 2h, obtains electrolytic copper foil, and cupric is 99.96%；
C, by the leached mud of step a, leached with the hydrochloric acid solution that concentration is 150 g/L, liquid solid product mass ratio is 4:1L/kg,
Extraction time is 3h, and extraction temperature control is at 80 DEG C；Filter after leaching, the filtering residue composition for obtaining is as follows：Bi 1.23%, Cu
4.16 g/t of 18.56 kg/t of 0.29%, Pb 50.91%, Sb 2.79%, Ag, Au, slag rate are 51.75%；Bismuth leaching rate is
98.0%；Leached mud returns silver-colored smelting system and reclaims silver, gold, lead；
Leachate volume 4500ml of d, step c, bismuth-containing 70.26g/L, with zine plate as anode, titanium plate is negative electrode, controls tank voltage
0.6 V, 700 A/m of electric current density2, electrolysing period 12h carries out the heavy bismuth of electrodeposition, obtain sponge bismuth Jing assay and obtain bismuth-containing be
91.72%, sponge bismuth obtains smart bismuth Jing after pyro-refining, and bismuth-containing is 99.991%.
Claims (9)
1. in a kind of bismuth slag from high-copper, selectivity efficient extracts copper, the technique of bismuth, is with high-copper bismuth slag as raw material；Its feature includes
Following steps：
A, broken pulverizing；By bulk high-copper bismuth slag material broken pulverizing to -100 mesh of granularity；
B, the high-copper bismuth ground-slag end for taking step a and sulphuric acid are poured in autoclave after sizing mixing, and controlling corresponding technical conditions carries out oxygen
Change and leach, during Oxidation Leaching, the Cu in high-copper bismuth slag is then with Cu2+Form is leached, so as to realize copper and other valuable gold
The separation of category；
C, the cupric leachate obtained by step b is directly carried out Jing after acid adjustment cyclone electrolytic cell extract copper therein, obtain qualified the moon
Pole copper products；
D, the leached mud obtained by step b is leached with a certain amount of hydrochloric acid solution, so as to realize that bismuth is separated with other metals；
E, it is bismuth chloride solution by the leachate obtained by step d, with zine plate as anode, titanium plate is negative electrode, control tank voltage 0.5～
0.8V, 600～1000 A/m of electric current density2, 8～1h of electrolysing period carries out the heavy bismuth of electrodeposition, obtains the sponge of purity more than 94.5%
Bismuth, the pyro-refining of sponge bismuth Jing obtain the smart bismuth of purity more than 99.99%；
F, by the remaining slag obtained by step d be lead antimony silver slag, return converter smelting reclaim lead, antimony, gold, silver valuable metal；
G, the useless electric effusion obtained by step e is neutralized, obtains basic zinc chloride product.
2. in the bismuth slag from high-copper according to claim 1, selectivity efficient extracts copper, the technique of bismuth, it is characterised in that：It is high
The composition of copper bismuth slag is：Bi：20～45%；Pb：15～40%；Cu：10～25%；Ag：0.6～1.2%；Sb3～8%.
3. in the bismuth slag from high-copper according to claim 1, selectivity efficient extracts copper, the technique of bismuth, it is characterised in that：Institute
State high-copper bismuth ground-slag end and adopt oxygen-enriched for oxide isolation in autoclave Oxidation Leaching, its oxygen content more than 60%.
4. in the bismuth slag from high-copper according to claim 1, selectivity efficient extracts copper, the technique of bismuth, it is characterised in that：It is high
In copper bismuth slag autoclave during Oxidation Leaching, the corresponding technical conditions of the control are：60～110g/L of sulfuric acid concentration, liquid solid product
4～6: 1 L/kg of mass ratio, 75～90 DEG C of temperature, 0.4～1.0MPa of pressure in kettle, 500～700 r/min of mixing speed, instead
1.5～3h between seasonable.
5. in the bismuth slag from high-copper according to claim 1, selectivity efficient extracts copper, the technique of bismuth, it is characterised in that：Step
Suddenly the optimum process condition of c cyclone electrolytic cells extraction copper is：1.8～2.8V of tank voltage, 500～800 A/m of electric current density2, electrolysis
48～72h of cycle.
6. in the bismuth slag from high-copper according to claim 1, selectivity efficient extracts copper, the technique of bismuth, it is characterised in that：Step
Suddenly a certain amount of hydrochloric acid solution leaching conditions of d are：Concentration of hydrochloric acid be 90～150 g/L, liquid solid product mass ratio 3～5:1 L/
Kg, 2～3 h of extraction time, 70～90 DEG C of extraction temperature.
7. in the bismuth slag from high-copper according to claim 1, selectivity efficient extracts copper, the technique of bismuth, it is characterised in that：Step
The optimum process condition of bismuth is reclaimed in rapid e electro-deposition：With zine plate as anode, titanium plate is negative electrode, controls 0.8 V of tank voltage, electric current
800 A/m of density2, electrolysing period 10h.
8. in the bismuth slag from high-copper according to claim 1, selectivity efficient extracts copper, the technique of bismuth, it is characterised in that：It is right
The nertralizer that electrodeposition waste liquid after step e electro-deposition recovery bismuth is added when being processed is Calx, adjusts endpoint pH 6～9,
65～85 DEG C of temperature of control, you can basic zinc chloride product is obtained, zinc chloride product can be used as feed additive.
9. in the bismuth slag from high-copper according to claim 1, selectivity efficient extracts copper, the technique of bismuth, it is characterised in that：Cross
Concentrated sulphuric acid, hydrochloric acid, Calx described in journey and oxygen-enriched it is technical grade reagent.
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| CN107268032A (en) * | 2017-06-27 | 2017-10-20 | 中国科学院过程工程研究所 | A kind of method of copper and zinc in Recycling of waste liquid |
| CN107828971A (en) * | 2017-12-16 | 2018-03-23 | 郴州市金贵银业股份有限公司 | A kind of method that valuable metal is separated and recovered from high bismuth copper ashes |
| CN107937725A (en) * | 2017-11-28 | 2018-04-20 | 郴州市金贵银业股份有限公司 | A kind of technique that valuable metal is recycled from silver-zinc crust |
| CN108149020A (en) * | 2018-01-12 | 2018-06-12 | 四川大学 | The technique for preparing bismuth using zinc anode sludge waste residue |
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