CN109913647A - A kind of wet treatment method recycling copper, zinc in bismuth chats - Google Patents

A kind of wet treatment method recycling copper, zinc in bismuth chats Download PDF

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CN109913647A
CN109913647A CN201910337857.5A CN201910337857A CN109913647A CN 109913647 A CN109913647 A CN 109913647A CN 201910337857 A CN201910337857 A CN 201910337857A CN 109913647 A CN109913647 A CN 109913647A
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copper
zinc
bismuth
chats
extraction
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CN109913647B (en
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詹有北
路永锁
宁建平
张源
符海
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JIANGXI SELF-INDEPENDENCE ENVIRONMENTAL PROTECTION TECHNOLOGY Co Ltd
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JIANGXI SELF-INDEPENDENCE ENVIRONMENTAL PROTECTION TECHNOLOGY Co Ltd
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The present invention relates to a kind of wet treatment method for recycling copper, zinc in bismuth chats is related to, bismuth chats wet-milling to -160 mesh is accounted for 98% powder, zinc electrolytic waste liquid pulp, preimpregnation after powder and dilution filter, and obtain filtrate and filter residue that acid eventually is 20~30g/L.Filter residue high-temperature roasting desulfurization forms thick bismuth at oxide, bismuth oxide and bismuth concentrate mixed smelting;With 20%+80%N902 kerosene through extracting through 3 stage countercurrents after filtrate tune pH to 1.5~2.0,2 grades of washings obtain copper-bath after 2 grades of back extraction, copper-bath enters copper electrodeposition system and is precipitated in cathode into 99.9% tough cathode;Extraction copper extraction raffinate, which neutralizes, removes iron, after the impurity elements such as zinc powder copper removal, cadmium, with liquid after the purification of 40%+60%P204 kerosene extraction, washs through the extraction of 4 stage countercurrents, 3 grades, obtains solution of zinc sulfate after 3 grades of back extraction.Solution of zinc sulfate oil in oil expeller absorbent solution, send Zinc electrolysis system electrowinning zinc.Material consumption is few, high degree of automation, and it is free of contamination cleaning procedure that production process, which does not generate waste water, discarded and waste residue,.

Description

A kind of wet treatment method recycling copper, zinc in bismuth chats
Technical field
The present invention relates to non-ferrous metallurgy field, the wet treatment method of copper, zinc in especially a kind of recycling bismuth chats.
Background technique
Bismuth seldom individually generates mineral deposit, the metallic elements symbiosis such as most of and copper, zinc, lead, tin, iron.For the mine of bismuth-containing Object generally uses ore-dressing technique, generates the higher bismuth concentrate of bismuth-containing and low-grade bismuth chats.Bismuth concentrate reduction melting generates thick bismuth, Thick bismuth obtains refined bismuth by two methods of pyro-refining and electrorefining.As thick refining technology improves, thick bismuth Quality advance is miscellaneous Matter is reduced, and pyro-refining is gradually instead of electrorefining, and only a small number of minorities Lian Bi enterprise uses electrorefining less at present.
Bismuth chats bismuth-containing is low, and impurity metallic elements content is high, big with the pyrometallurgical smelting quantity of slag, equipment capacity decline, if Standby production capacity declines, and metal recovery rate is low, and at high cost, China generally uses Wet-process metallurgy method to handle.Industrially mostly use Hydrochloric acid liquor ferri trichloridi leaches, and refining is refined bismuth after the displacement of leachate iron.The many years production practices of this method have preferable Economic and technical norms.
Based on copper, zinc, lead, tin, bismuth etc. exist with sulphided form in bismuth chats, bismuth chats wet-treating mostly uses greatly three Iron chloride leaches or chlorine leaching, and especially hydrochloric acid ferric trichloride leaches bismuth chats to bismuth leaching rate height, extraction temperature 98~106 ℃;Extraction time 2 hours;- 200 mesh of granularity of concentrate accounts for 90% or more;Fe3+70~90g/L of concentration;Liquid-solid ratio: 3~2:1;It leaches Liquid acidity: 20~30g/L of HCl concentration.It is disadvantageous in that in leachate that ferrous ion content is larger with ferric trichloride leaching, Difficulty is brought to leachate isolation of purified, higher chlorine ion concentration also requires equipment to have anti-corrosion capability in solution.
The prior art be related to bismuth processing as, CN201110297150.X " from tin bismuth waste material Separation of Tin, bismuth, copper and The technique of zinc ", generated solid waste will be recycled by sn-bi alloy electroplating effluent and is known as tin bismuth waste material, pass through roasting, powder Broken, acidleach neutralizes heavy bismuth, replaces heavy copper, heavy zinc, efficiently separated tin, bismuth, copper, four element of zinc, and high income respectively reaches 99.2%, 97.8%, 95.4%, 93.2%, good product quality.
Obtained thick bismuth is carried out pyrogenic process essence by a kind of for another example CN201410362043.4 " method of bismuth is recycled in precious metals containing lead " Refining, in thick bismuth plus sulphur copper removal, oxidation arsenic removal antimony, logical chlorine remove lead, zincification desilver, are eventually adding caustic soda, nitre is refined, The bismuth ingot product of output national standard.This method process flow refining is succinct.
For another example CN201710334589.2 " technique of valuable element in a kind of low-grade sulphide ore of Whote-wet method recycling complexity ", It will be sieved after raw material crushing grinding, carry out pressure oxidation leaching after being sized mixing with sodium hydroxide solution, obtain alkali immersion liquid and alkali phase analysis;Alkali Immersion liquid is acidified to obtain lead sulfate product and heavy lead liquid, and heavy lead liquid substep controlling potential restores to obtain liquid after impure selenium powder, coarse tellurium powder and reduction; Alkali phase analysis soaks copper with sulfuric acid solution, must soak copper ashes and copper leaching liquid;Soak copper ashes with chloride ion-containing Acidic Liquid soak antimony bismuth, must soak antimony liquid with Antimony slag is soaked, leaching antimony slag send noble metal to recycle, and leaching antimony liquid adjusted stepwise pH obtains antimony slag and bismuth slag;Copper leaching liquid adjusts pH and obtains scum and remove Iron liquid, scum is wastewater treatment additive, except iron liquid obtains copper powder and displaced liquid with zinc dust precipitation;Liquid and displaced liquid after reduction Merge, condensing crystallizing obtains white vitriol.
Summary of the invention
The purpose of the present invention is to solve defect of the existing technology, copper in a kind of recycling bismuth chats, zinc are provided Wet treatment method.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of wet treatment method recycling copper, zinc in bismuth chats, this method comprises the following steps:
(1) it roughly grinds
Bismuth chats obtains the ore pulp that -160 mesh account for 98% through overflowball mill ball milling and cyclosizer.Ore pulp is pumped into sedimentation Slot concentration, underflow are pumped into ceramic filter with underflow pump and are separated by solid-liquid separation, and obtain the powder of moisture content 18%~20% or so.
(2) oxygen leaching
Above-mentioned powder enters slurrying tank pulp together with zinc electrolyte, while 0.5%~1% calcium lignosulfonate is added, sufficiently It is pumped into pre- leaching tanks preimpregnation after mixing and is warming up to 80~85 DEG C.Slurry is pumped into horizontal reacting kettle by diaphragm pump after heating, together When carry out pressure leaching for oxygen rich gas is counter into reaction kettle, after leaching slurry flashed down be discharged, through plate and frame filter press solid-liquid Separation send melting after leached mud washing.Leachate enters copper, zinc recovering process.
(3) extraction-electrodeposition recycles copper
Leachate obtained by step (2) adjusts pH to 1.5~2.0 with agstone, filters to obtain supernatant 20%+80%N902 kerosene Copper-bath is obtained through the extraction of 3 stage countercurrents, 2 grades of washings, 2 grades of back extraction, the concentrated evaporation of copper-bath prepares five water sulfuric acid Copper, copper-bath enter copper electrodeposition system and are precipitated in cathode into 99.9% tough cathode.
(4) P204 extract-is stripped electrowinning zinc
The lime stone of raffinate obtained by step (3) adjusts pH to 3.5~4.0, and the dioxygen water depth that 0.5% volume ratio is added removes Iron.Except the impurity elements such as micro copper, the cadmium of zinc powder purified solution are added in liquid after iron, liquid is with 40%+60%P204 kerosene through 4 after purification Solution of zinc sulfate is obtained after stage countercurrent extraction, 3 grades of washings, 3 grades of back extraction, solution of zinc sulfate send electrowinning zinc to prepare zinc ingot metal.
The wet treatment method of copper, zinc, the oxygen leaching condition are as follows: reaction temperature in a kind of above-mentioned recycling bismuth chats 170~180 DEG C, 1.4~1.6Mpa of stagnation pressure, reaction 4h, 6~8:1 of liquid-solid ratio, 60~80g/L of leaching agent initial acidity, lignin Sulfoacid calcium additive amount is the 0.5~1% of raw material.
The wet treatment method of copper, zinc in a kind of above-mentioned recycling bismuth chats, leachate terminal controlling pH 20~ 30g/L, iron concentration are lower than 1g/L.
The wet treatment method of copper, zinc in a kind of above-mentioned recycling bismuth chats, N902 extract copper section organic phase: feed liquid be 1~ 1.5:1;Washing section: water phase is 10~15:1;Stripping section organic phase: anti-copper acid is 4~5:1.
The wet treatment method of copper, zinc in a kind of above-mentioned recycling bismuth chats, P204 extract zinc section organic phase: feed liquid be 2~ 3:1;Washing section: water phase is 15~20:1;Stripping section organic phase: anti-copper acid is 6~8:1.
Leaded 10% or so, bismuth 30% or so in oxygen leaching slag;Copper, Zn content are below 1%;Iron content 10~15%.Leaching The equal sulphate form of middle lead, bismuth of slagging tap exists, and palpus high-temperature roasting desulfurization is at oxide, bismuth oxide and bismuth concentrate mixed smelting shape At thick bismuth.
The invention has the benefit that 1. use the metals such as copper, zinc in sulfuric acid oxygen leaching bismuth chats, realize soluble The separation of zinc sulfate, the lead sulfate of copper sulphate and slightly solubility, bismuth sulfate had both avoided interference of the elements such as copper, zinc to recycling bismuth, Synthetical recovery complex multi-metal mineral are achieved the purpose that again;2. oxygen leaching is handled, the process flow of bismuth chats is short, and raw material adapts to Property it is strong, recovery rate of valuable metals is high, and solution is small except impurity load, and material consumption is few, high degree of automation, and production process does not generate Waste water, discarded and waste residue, are free of contamination cleaning procedures;3. the present invention can be obtained by recycling in bismuth chats for the purpose of copper, zinc To the final products of tough cathode and zinc ingot metal, oxygen leaching slag lead, bismuth respectively obtain enrichment, and leached mud can return to pyrogenic process refining bismuth system System.
Detailed description of the invention
Fig. 1 bismuth chats oxygen leaching flow chart of the present invention;
Fig. 2 copper zinc lixiviating solution extraction procedure figure of the present invention.
Specific embodiment
The present invention can be with the invention will be further described by the following examples, however the scope of the present invention is not It is limited to following embodiments.
Embodiment 1: it is operated by technique shown in Fig. 1-2.
It is realized by following 4 steps and technique process: (1) ball milling;(2) oxygen presses acidleach copper, zinc;(3) N902 Extraction-back extraction electro deposited copper;(4) P204 extract-is stripped electrowinning zinc.
By bismuth-containing 18.63%, copper 7.59%, lead 7.72%, zinc 17.64% bismuth chats 100t through wet ball mill ball milling, point Grade machine classification, ceramic filter filtering obtain the bismuth chats powder that -160 mesh account for 98%.
Oxygen leaching copper, zinc: with liquid (H after the zinc electrolysis after dilution2SO4180~200g/L, Zn2+50~60g/L) and ball The pulp of bismuth chats powder, preimpregnation after mill, preimpregnated slurry are pumped into 100m by diaphragm pump3In horizontal reacting kettle, reacting 4h, slurry flow 20m are reacted under conditions of 170~180 DEG C of temperature, 1.4~1.6Mpa of stagnation pressure3/h;Copper ion is dense in leachate Spend 8~10g/L, 35~40g/L of zinc ion concentration, iron ion 0.78g/L, bismuth ion 0.2g/L.
Leachate 20~30g/l of spent acid, adjusting acidity to pH with agstone is 1.5~2.0, adjusts sour process agstone First pulp of being sure to is pumped into neutralization chamber again.The neutralizer that pH is 1.5~2.0 is 20%N902+80% kerosene through 3 grades with content of material Counter-current extraction copper, extraction N902 organic phase and material flow ratio are 1~1.5:1, and extraction gained extraction copper extraction raffinate cupric is lower than 0.2g/L; Extraction back loading N902 organic phase washs organic phase with 2 stage countercurrent of wash water, and washing process loads N902 organic phase and aqueous phase stream ratio For 10~15:1, wash water lime precipitation wherein copper, zinc ion after washing, liquid is returned for washing repeatedly load N902 after precipitating Organic phase;Back loading N902 organic phase is washed using copper in 2 grades of back extraction organic phases of the poor copper liquid of electrodeposition, load N902 organic phase with it is poor Copper liquid flowing ratio is 8~10:1, obtains copper-bath after back extraction, copper-bath enter copper electrodeposition system cathode be precipitated at 99.9% tough cathode.
Extract copper extraction raffinate 12~15g/L containing acid, adjusts pH to 4.0~4.5 with lime stone, and add 0.5% hydrogen peroxide oxidation and remove Iron to iron ion is lower than 0.001g/L.Except liquid removes the impurity elements such as copper, cadmium micro in solution, zinc powder dosage with zinc powder after iron For copper, 1.0~1.2 times of cadmium content.
Liquid pH is 4.0~4.5 after purification, demodulates pH to 2.0~2.5 with sulfuric acid.It is 40%P204+60% coal with content of material Liquid after oily extracting and purifying, through 4 stage countercurrent extracting zincs, liquid flowing ratio is 2~3:1 after extracting P204 organic phase and purification, is born after extraction Carry P204 organic phase and organic phase washed using 3 stage countercurrent of wash water, washing process load P204 organic phase and wash water stream ratio be 15~ 20:1, washing back loading P204 organic phase load P204 organic phase using zinc in 3 stage countercurrent of electrodeposition zincky waste liquor back extraction organic phase It is 8~10:1 with zincky waste liquor stream ratio, zinc sulfate strip liquor is obtained after back extraction.Solution of zinc sulfate oil in oil expeller absorbent solution Point, Zinc electrolysis system electrowinning zinc is sent, zinc ingot metal is made in zinc metal sheet founding.
Further, extraction zinc extraction raffinate supplying sulfuric acid returns to oxygen leaching process.
The metals such as copper, zinc in this method oxygen leaching bismuth chats, realize copper, zinc and lead, bismuth separation, both avoided copper, Interference of the elements such as zinc to recycling bismuth, and achieved the purpose that synthetical recovery complex multi-metal mineral;2. oxygen leaching handles bismuth Chats process flow is short, and adaptability to raw material is strong, and recovery rate of valuable metals is high, and solution is small except impurity load, and material consumption is few, automatically Change degree is high, and it is free of contamination cleaning procedure that production process, which does not generate waste water, discarded and waste residue,.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and Improvement is both fallen in the range of claimed invention.The present invention claims protection scope by appended claims and its Equivalent defines.

Claims (5)

1. the wet treatment method of copper, zinc in a kind of recycling bismuth chats, which is characterized in that this method comprises the following steps:
Ball milling: bismuth chats obtains the ore pulp that bismuth chats particle is -160 mesh through ball milling, spiral classifier, and it is dense that ore pulp is pumped into subsider Contracting, underflow are pumped into ceramic filter with underflow pump and are separated by solid-liquid separation, and obtain the powder that water content is 18%~20% or so;
Oxygen leaching: powder and zinc electrolyte pulp after ball milling, while the lignin sulfonic acid that mass fraction is 0.5%~1% is added Calcium is pumped into pre- leaching tanks preimpregnation and is warming up to 80~85 DEG C after being sufficiently mixed, slurry is pumped into horizontal reacting by diaphragm pump after heating In kettle, while pressure leaching is carried out for oxygen rich gas is counter into reaction kettle, slurry flashed down is discharged after leaching, through plate compression Machine is separated by solid-liquid separation, and send pyrogenic process process after leached mud washing;
N902 extraction-electrodeposition recycles copper: leachate adjusts pH to 1.5~2.0 with agstone, uses 20%+80%N902 after filtering Kerosene extracts through 3 stage countercurrents, 2 grades of washings, 2 grades of back extraction obtain copper-baths, copper-bath feeding copper electrodeposition system electrodeposition At 99.9% tough cathode;
P204 extraction-electrowinning zinc: extraction copper extraction raffinate adjusts pH to 3.5~4.0, and the hydrogen peroxide neutralization for being added 0.5% removes iron, except after iron Liquid be added zinc powder carry out purified solution, after purification liquid extract with 40%+60%P204 kerosene through 4 stage countercurrents, 3 grades washing, 3 grades be stripped After obtain solution of zinc sulfate, solution of zinc sulfate oil in oil expeller absorbent solution is sent into Zinc electrolysis system and prepares zinc ingot metal.
2. the wet treatment method of copper, zinc in a kind of recycling bismuth chats according to claim 1, which is characterized in that described Oxygen leaching condition are as follows: 170~180 DEG C of reaction temperature, 1.4~1.6Mpa of stagnation pressure, reaction 4h, 6~8:1 of liquid-solid ratio, leaching agent 60~80g/L of initial acidity, 0.5~1% that calcium lignosulfonate additive amount is raw material.
3. the wet treatment method of copper, zinc in a kind of recycling bismuth chats according to claim 2, which is characterized in that leach Liquid terminal controlling pH is lower than 1g/L in 20~30g/L, iron concentration.
4. the wet treatment method of copper, zinc in a kind of recycling bismuth chats according to claim 1, which is characterized in that N902 Extract copper section organic phase: feed liquid is 1~1.5:1;Washing section: water phase is 10~15:1;Stripping section organic phase: anti-copper acid is 4~5: 1。
5. the wet treatment method of copper, zinc in a kind of recycling bismuth chats according to claim 1, which is characterized in that P204 Extract zinc section organic phase: feed liquid is 2~3:1;Washing section: water phase is 15~20:1;Stripping section organic phase: anti-copper acid is 6~8:1.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110396608A (en) * 2019-08-02 2019-11-01 中南大学 A kind of methane sulfonic acid system bismuth sulfide concentrate oxygen leaching method
CN111647748A (en) * 2020-05-08 2020-09-11 成都中建材光电材料有限公司 Method for separating and purifying crude cuprous telluride slag

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011135991A1 (en) * 2010-04-27 2011-11-03 国立大学法人茨城大学 Valuable metal recovery method
CN102851693A (en) * 2012-08-29 2013-01-02 江西自立资源再生有限公司 Technology for recovering production of electrolytic copper and zinc from smelting ash
CN109554539A (en) * 2018-12-26 2019-04-02 湖南柿竹园有色金属有限责任公司 A kind of method of bismuth and copper and iron in pressurized acid leaching separation of Bismuth concentrate

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011135991A1 (en) * 2010-04-27 2011-11-03 国立大学法人茨城大学 Valuable metal recovery method
CN102851693A (en) * 2012-08-29 2013-01-02 江西自立资源再生有限公司 Technology for recovering production of electrolytic copper and zinc from smelting ash
CN109554539A (en) * 2018-12-26 2019-04-02 湖南柿竹园有色金属有限责任公司 A kind of method of bismuth and copper and iron in pressurized acid leaching separation of Bismuth concentrate

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110396608A (en) * 2019-08-02 2019-11-01 中南大学 A kind of methane sulfonic acid system bismuth sulfide concentrate oxygen leaching method
CN110396608B (en) * 2019-08-02 2021-06-18 中南大学 Oxygen pressure leaching method for bismuth sulfide concentrate in methanesulfonic acid system
CN111647748A (en) * 2020-05-08 2020-09-11 成都中建材光电材料有限公司 Method for separating and purifying crude cuprous telluride slag

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