CN103334018A - Method for extracting antimony and bismuth from lead anode mud - Google Patents
Method for extracting antimony and bismuth from lead anode mud Download PDFInfo
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- CN103334018A CN103334018A CN2013102421759A CN201310242175A CN103334018A CN 103334018 A CN103334018 A CN 103334018A CN 2013102421759 A CN2013102421759 A CN 2013102421759A CN 201310242175 A CN201310242175 A CN 201310242175A CN 103334018 A CN103334018 A CN 103334018A
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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
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Abstract
The invention discloses a method for extracting antimony and bismuth from lead anode mud. The method is characterized in that the antimony and bismuth are extracted through leaching, hydrolysis and replacement by adopting a wet processing, and purposes of comprehensive utilization of resources and improvement of the recovery rate of antimony and bismuth are realized. According to the method, the device configuration is simple, the operation is stable and is convenient to control, the comprehensive utilization of resources is high, and the recovery rate of antimony and bismuth is improved.
Description
Technical field:
The present invention relates to nonferrous smelting resource comprehensive recovery and utilization technology field, is a kind for the treatment of process of extracting antimony, bismuth from lead anode slurry concretely, and this method can effectively reclaim antimony, the bismuth in the lead anode slurry.
Background technology:
The production technique of extracting antimony, bismuth from lead anode slurry commonly used at present is: leach lead anode slurry with iron trichloride in hydrochloric acid soln, the amount that adds iron trichloride is 1:0.72-0.76 for material iron ratio, (0.74 is equivalent to 140g/LFe3+), concentration of hydrochloric acid is 0.5mol/L; Carry out wet method according to this condition antianode mud and leach, reclaim the antimony bismuth, leach the leaching yield of back antimony bismuth with this technology and have only about 70% the too low requirement that does not reach production of the rate of recovery.
Summary of the invention:
The objective of the invention is to overcome the problem that above-mentioned prior art exists, and provide a kind of acid wet method from lead anode slurry, to extract the treatment process of antimony, bismuth, mainly solve the low problem of leaching yield of existing method antimony bismuth.
Technical scheme of the present invention is: a kind for the treatment of process of extracting antimony, bismuth from lead anode slurry, its special character are that it comprises following processing step:
The a oxidation acid leaching: configuration hydrochloric acid 5mol/L, press solvent and solute weight ratio 4-6:1, add hydrochloric acid, the anode sludge, press the part by weight adding iron trichloride of lead anode slurry and iron trichloride 3-5:1 again in this solution, agitation leach 2-3h under 65-75 ℃ of condition; Reaction formula:
Sb
2O
3+HCl=?SbCl
3+H
2O
Sb
2S
3+6FeCl
3=2SbCl
3+6FeCl
2+3S
Sb+3FeCl
3=?SbCl
3+3FeCl
2
Bi
2S
3+6FeCl
3=2BiCl
3+6FeCl
2+3S
Bi
2O
3+6HCl=2BiCl
3+2H
2O
Bi+3FeCl
3=BiCl
3+3FeCl
2；
The b solid-liquid separation: material carries out liquid-solid separation, and leached mud is sent into traditional thermal process and extracted precious metals such as gold and silver, and leach liquor is used for next step processing;
Antimony is carried in the c hydrolysis: add the water of 5-6 times of volume in the leach liquor, the antimony ion generation hydrolysis in the liquid produces the antimony oxychloride precipitation; Carry out solid-liquid separation after reaction finishes, obtain liquid after antimony oxychloride and the hydrolysis; Reaction formula:
SbCl3+H2O=SbOCl+2HCl
4SbOCl+5H2O=Sb4O5Cl2+2HCl；
Iron replacement of d: add hydrochloric acid and water to antimony oxychloride, make its whole dissolvings, in lysate, add iron replacement again, under 40-50 ℃ of condition, stir 2-2.5h; After the replacement completion, carry out liquid-solid separation, obtain the sponge antimony product and contain antimony solution;
E secondary iron replacement: to containing antimony solution adding excess iron powder remaining antimony is cemented out, what solid-liquid separation obtained contains the antimony iron powder as the once iron powder reuse of displacement, and parting liquid processing up to standard effluxes; Reaction formula:
Fe+?SbCl3=?FeCl3+Sb；
Bismuth is carried in the f hydrolysis: add soda ash in the liquid after the hydrolysis that produces to step c, the adjusting pH value is 2.5-3.0; Bismuth ion hydrolysis in the liquid obtains chlorine oxygen bismuth precipitation, and reaction finishes the back solid-liquid separation, obtains chlorine oxygen bismuth and neutralization back liquid, and the processing up to standard of neutralization back liquid effluxes; Reaction formula:
BiCl3+H2O=BiOCl+2HCl
4BiOCl+5H2O=Bi4O5Cl2+2HCl；
Iron replacement of g: add hydrochloric acid and water to chlorine oxygen bismuth, make its whole dissolvings, in lysate, add iron replacement, under 40-50 ℃ of condition, stir 2-2.5h; Replacement(metathesis)reaction is carried out liquid-solid separation after finishing, and obtains sponge bismuth product and the solution that contains a small amount of bismuth;
H secondary iron replacement: add excess iron powder to the solution that contains a small amount of bismuth remaining bismuth is cemented out, the bismuth-containing iron powder that solid-liquid separation obtains is recycled as the iron powder of once displacement, and liquid processing up to standard effluxes; Reaction formula:
Fe+?BiCl
3=?BiCl
3+Sb。
Compared with the prior art a kind for the treatment of process of extracting antimony, bismuth from lead anode slurry of the present invention has outstanding substantive distinguishing features and marked improvement: change the usage quantity of iron(ic) chloride and the concentration of hydrochloric acid when 1, leaching, improve the leaching yield of antimony bismuth, the rate of recovery of antimony, bismuth is brought up to about 93% by original about 70%; 2, the processing unit configuration is simple, and stable operation is convenient to control; 3, comprehensive utilization of resources rate height, gold and silver, antimony, bismuth have all obtained recycling; 4, cost recovery is low, has very high economic worth.
Embodiment:
In order to understand better and to implement, describe the present invention in detail below in conjunction with embodiment; Illustrated embodiment only is used for explaining the present invention, is not for limiting scope of the present invention
Embodiment 1: lead anode slurry is example with what contain following element, its constituent content such as table 1:
Table 1
| Title | Gold | Title | Silver |
| Content (g/t) | 611.7 | Content (%) | 7.39 |
| Title | Plumbous | Title | Tellurium |
| Content (%) | 19.64 | Content (%) | 0.43 |
| Title | Selenium | Title | Bismuth |
| Content (%) | 0.02 | Content (%) | 11.1 |
| Title | Antimony | Title | Copper |
| Content (%) | 35.26 | Content (%) | 1.11 |
| Title | Arsenic | Title | Platinum |
| Content (%) | 7.19 | Content (g/t) | 3.49 |
| Title | Palladium | ? | ? |
| Content (g/t)) | 12.36 | ? | ? |
Take following processing step:
Step 1(leaches reaction): reactor is cleaned out, off-response still bottom valve, configuration hydrochloric acid 5mol/L, at first in reactor, add hydrochloric acid 3000L, by configuration solvent and solute weight ratio 5:1, add anode sludge 600kg(dry weight), add iron trichloride 150kg then, open and stir, be warming up to 70 ℃, leach 2h; Reaction formula:
Sb
2O
3+HCl=?SbCl
3+H
2O
Sb
2S
3+6FeCl
3=2SbCl
3+6FeCl
2+3S
Sb+3FeCl
3=?SbCl
3+3FeCl
2
Bi
2S
3+6FeCl
3=2BiCl
3+6FeCl
2+3S
Bi
2O
3+6HCl=2BiCl
3+2H
2O
Bi+3FeCl
3=BiCl
3+3FeCl
2；
Step 2(solid-liquid separation): the material in the reactor is squeezed in the pressure filter, carried out liquid-solid separation, leached mud is sent into pyrogenic process and is extracted gold and silver, and leach liquor 2900L squeezes into and is used for next step processing in the storage tank;
Step 3(hydrolysis reaction): leach liquor is squeezed in the reactor, the water that adds 5.5 times of volumes is 15950L altogether, the reaction that is hydrolyzed of the antimony ion in the liquid, and the generation antimony oxychloride precipitates 295 kg, after finishing, reaction carries out press filtration, liquid 20000L after generation antimony oxychloride 295kg and the hydrolysis; Reaction formula:
SbCl3+H2O=SbOCl+2HCl
4SbOCl+5H2O=Sb4O5Cl2+2HCl；
Iron replacement of step 4(): (295kg altogether) adds adding 100L hydrochloric acid in the reactor with antimony oxychloride, add water 900L, it is anti-molten to carry out antimony oxychloride hydrochloric acid, adds iron powder (155kg altogether) after the dissolving and carries out reduction reaction, open to stir and be warming up to 40 ℃, reaction 2h; Carry out liquid-solid separation after the replacement completion, obtain sponge antimony product (203.8kg altogether) and contain antimony solution;
Step 5(secondary iron replacement): contain antimony solution and add excess iron powder (altogether 25kg) more remaining antimony is cemented out, liquid processing up to standard effluxes; Reaction formula:
Fe+?SbCl3=?FeCl3+Sb；
Bismuth is carried in step 6(hydrolysis): liquid after the hydrolysis of step 3 is squeezed in the reactor, add soda ash 15kg, bismuth ion in the adjusting pH value 2.5. liquid is hydrolyzed to react and produces chlorine oxygen bismuth precipitation (totally 85 kg), after reaction finishes, carry out press filtration with pressure filter, obtain chlorine oxygen bismuth 85kg and neutralization back liquid, the processing up to standard of neutralization back liquid effluxes; Reaction formula:
BiCl3+H2O=BiOCl+2HCl
4BiOCl+5H2O=Bi4O5Cl2+2HCl；
Iron replacement of step 7(): (85kg altogether) adds adding 100L hydrochloric acid in the reactor with chlorine oxygen bismuth, add water 900L and make its whole dissolvings, add iron powder (50kg altogether) after the dissolving and carry out reduction reaction, open to stir and be warming up to 40 ℃, reaction 2h, reaction is carried out liquid-solid separation after finishing, and filter residue is exactly sponge bismuth product (totally 65.6 kg) and bismuth-containing solution;
Step 8 (secondary iron replacement): bismuth-containing solution adds excess iron powder (5kg altogether) more remaining bismuth is cemented out, and liquid processing up to standard effluxes; Reaction formula:
Fe+?BiCl
3=?BiCl
3+Sb。
Above-described embodiment and former technical process metal recovery rate are to such as table 2:
Table 2
| Title | The rate of recovery % of bismuth | The rate of recovery % of antimony |
| Former technology | 71.21 | 70.21 |
| Embodiment | 97.48 | 97.19 |
Embodiment 2, step 1, and configuration hydrochloric acid 5mol/L press solvent and solute weight ratio 4:1, adds hydrochloric acid, the anode sludge, presses the part by weight adding iron trichloride of lead anode slurry and iron trichloride 3:1 again in this solution, agitation leach 3h under 65 ℃ of conditions;
Step 2, material carries out liquid-solid separation, and leached mud is sent into traditional thermal process and is extracted precious metals such as gold and silver, and leach liquor is used for next step processing;
Step 3 adds the water of 5 times of volumes in the leach liquor, and the antimony ion generation hydrolysis in the liquid produces the antimony oxychloride precipitation; Carry out solid-liquid separation after reaction finishes, obtain liquid after antimony oxychloride and the hydrolysis;
Step 4 adds hydrochloric acid and water to antimony oxychloride, makes its whole dissolvings, adds iron replacement again in lysate, stirring reaction 2.5h under 45 ℃ of conditions; After the replacement completion, carry out liquid-solid separation, obtain the sponge antimony product and contain antimony solution;
Step 5 cements out remaining antimony to containing antimony solution adding excess iron powder, and what solid-liquid separation obtained contains the antimony iron powder as the once iron powder reuse of displacement, and parting liquid processing up to standard effluxes;
Step 6 adds soda ash in the liquid after the hydrolysis that produces to step 3, and regulating pH value is 2.5; Bismuth ion hydrolysis in the liquid obtains chlorine oxygen bismuth precipitation, and reaction finishes the back solid-liquid separation, obtains chlorine oxygen bismuth and neutralization back liquid, and the processing up to standard of neutralization back liquid effluxes;
Step 7 adds hydrochloric acid and water to chlorine oxygen bismuth, makes its whole dissolvings, adds iron replacement in lysate, stirs 2.5h under 40 ℃ of conditions; Replacement(metathesis)reaction is carried out liquid-solid separation after finishing, and obtains sponge bismuth product and the solution that contains a small amount of bismuth;
Step 8 adds excess iron powder to the solution that contains a small amount of bismuth remaining bismuth is cemented out, and the bismuth-containing iron powder that solid-liquid separation obtains is recycled as the iron powder of once displacement, and liquid processing up to standard effluxes.
Embodiment 3, step 1, and configuration hydrochloric acid 5mol/L press solvent and solute weight ratio 6:1, adds hydrochloric acid, the anode sludge, presses the part by weight adding iron trichloride of lead anode slurry and iron trichloride 5:1 again in this solution, agitation leach 2.5h under 75 ℃ of conditions;
Step 2, material carries out liquid-solid separation, and leached mud is sent into traditional thermal process and is extracted precious metals such as gold and silver, and leach liquor is used for next step processing;
Step 3 adds the water of 5-6 times of volume in the leach liquor, and the antimony ion generation hydrolysis in the liquid produces the antimony oxychloride precipitation; Carry out solid-liquid separation after reaction finishes, obtain liquid after antimony oxychloride and the hydrolysis;
Step 4 adds hydrochloric acid and water to antimony oxychloride, makes its whole dissolvings, adds iron replacement again in lysate, stirs 2h under 50 ℃ of conditions; After the replacement completion, carry out liquid-solid separation, obtain the sponge antimony product and contain antimony solution;
Step 5 cements out remaining antimony to containing antimony solution adding excess iron powder, and what solid-liquid separation obtained contains the antimony iron powder as the once iron powder reuse of displacement, and parting liquid processing up to standard effluxes;
Step 6 adds soda ash in the liquid after the hydrolysis that produces to step 3, and regulating pH value is 3.0; Bismuth ion hydrolysis in the liquid obtains chlorine oxygen bismuth precipitation, and reaction finishes the back solid-liquid separation, obtains chlorine oxygen bismuth and neutralization back liquid, and the processing up to standard of neutralization back liquid effluxes;
Step 7 adds hydrochloric acid and water to chlorine oxygen bismuth, makes its whole dissolvings, adds iron replacement in lysate, stirs 2h under 50 ℃ of conditions; Replacement(metathesis)reaction is carried out liquid-solid separation after finishing, and obtains sponge bismuth product and the solution that contains a small amount of bismuth;
Step 8 adds excess iron powder to the solution that contains a small amount of bismuth remaining bismuth is cemented out, and the bismuth-containing iron powder that solid-liquid separation obtains is recycled as the iron powder of once displacement, and liquid processing up to standard effluxes.
Claims (1)
1. treatment process of extracting antimony, bismuth from lead anode slurry is characterized in that comprising following processing step:
The a oxidation acid leaching: configuration hydrochloric acid 5mol/L, press solvent and solute weight ratio 4-6:1, add hydrochloric acid, the anode sludge, press the part by weight adding iron trichloride of lead anode slurry and iron trichloride 3-5:1 again in this solution, agitation leach 2-3h under 65-75 ℃ of condition; Reaction formula:
Sb
2O
3+HCl=?SbCl
3+H
2O
Sb
2S
3+6FeCl
3=2SbCl
3+6FeCl
2+3S
Sb+3FeCl
3=?SbCl
3+3FeCl
2
Bi
2S
3+6FeCl
3=2BiCl
3+6FeCl
2+3S
Bi
2O
3+6HCl=2BiCl
3+2H
2O
Bi+3FeCl
3=BiCl
3+3FeCl
2；
The b solid-liquid separation: material carries out liquid-solid separation, and leached mud is sent into traditional thermal process and extracted precious metals such as gold and silver, and leach liquor is used for next step processing;
Antimony is carried in the c hydrolysis: add the water of 5-6 times of volume in the leach liquor, the antimony ion generation hydrolysis in the liquid produces the antimony oxychloride precipitation; Carry out solid-liquid separation after reaction finishes, obtain liquid after antimony oxychloride and the hydrolysis; Reaction formula:
SbCl3+H2O=SbOCl+2HCl
4SbOCl+5H2O=Sb4O5Cl2+2HCl；
Iron replacement of d: add hydrochloric acid and water to antimony oxychloride, make its whole dissolvings, in lysate, add iron replacement again, under 40-50 ℃ of condition, stir 2-2.5h; After the replacement completion, carry out liquid-solid separation, obtain the sponge antimony product and contain antimony solution;
E secondary iron replacement: to containing antimony solution adding excess iron powder remaining antimony is cemented out, what solid-liquid separation obtained contains the antimony iron powder as the once iron powder reuse of displacement, and parting liquid processing up to standard effluxes; Reaction formula:
Fe+?SbCl3=?FeCl3+Sb；
Bismuth is carried in the f hydrolysis: add soda ash in the liquid after the hydrolysis that produces to step c, the adjusting pH value is 2.5-3.0; Bismuth ion hydrolysis in the liquid obtains chlorine oxygen bismuth precipitation, and reaction finishes the back solid-liquid separation, obtains chlorine oxygen bismuth and neutralization back liquid, and the processing up to standard of neutralization back liquid effluxes; Reaction formula:
BiCl3+H2O=BiOCl+2HCl
4BiOCl+5H2O=Bi4O5Cl2+2HCl；
Iron replacement of g: add hydrochloric acid and water to chlorine oxygen bismuth, make its whole dissolvings, in lysate, add iron replacement, under 40-50 ℃ of condition, stir 2-2.5h; Replacement(metathesis)reaction is carried out liquid-solid separation after finishing, and obtains sponge bismuth product and the solution that contains a small amount of bismuth;
H secondary iron replacement: add excess iron powder to the solution that contains a small amount of bismuth remaining bismuth is cemented out, the bismuth-containing iron powder that solid-liquid separation obtains is recycled as the iron powder of once displacement, and liquid processing up to standard effluxes; Reaction formula:
Fe+?BiCl
3=?BiCl
3+Sb。
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107190151A (en) * | 2017-06-07 | 2017-09-22 | 六盘水中联工贸实业有限公司 | With the comprehensive recovering process of heavy scum in a kind of zinc hydrometallurgy |
| CN108300873A (en) * | 2018-03-14 | 2018-07-20 | 湖南工业大学 | A kind of clean Au-Sn deposit circulating leaching method |
| CN110358919A (en) * | 2019-07-23 | 2019-10-22 | 郴州市金贵银业股份有限公司 | A kind of method of acid dipping separation antimony lead |
| CN111172408A (en) * | 2020-01-20 | 2020-05-19 | 昆明瀚创科技有限公司 | Equipment for continuously and deeply purifying zinc sulfate solution to remove nickel, cobalt and germanium and control method |
| CN111197119A (en) * | 2020-02-25 | 2020-05-26 | 广州市尚信净化工程有限公司 | Method for recovering valuable metals from bismuth-containing waste residues |
| CN111233036A (en) * | 2020-01-20 | 2020-06-05 | 昆明瀚创科技有限公司 | Made of Sb2O3Direct preparation of Sb with aqueous hydrochloric acid4O5Cl2Method (2) |
| CN111254292A (en) * | 2020-01-20 | 2020-06-09 | 昆明瀚创科技有限公司 | Method for removing nickel, cobalt and germanium by zinc sulfate aqueous solution purification |
| CN115305361A (en) * | 2022-08-26 | 2022-11-08 | 山东恒邦冶炼股份有限公司 | High-purity antimony rod and high-purity antimony white combined preparation process |
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Cited By (11)
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|---|---|---|---|---|
| CN107190151A (en) * | 2017-06-07 | 2017-09-22 | 六盘水中联工贸实业有限公司 | With the comprehensive recovering process of heavy scum in a kind of zinc hydrometallurgy |
| CN108300873A (en) * | 2018-03-14 | 2018-07-20 | 湖南工业大学 | A kind of clean Au-Sn deposit circulating leaching method |
| CN110358919A (en) * | 2019-07-23 | 2019-10-22 | 郴州市金贵银业股份有限公司 | A kind of method of acid dipping separation antimony lead |
| CN111172408A (en) * | 2020-01-20 | 2020-05-19 | 昆明瀚创科技有限公司 | Equipment for continuously and deeply purifying zinc sulfate solution to remove nickel, cobalt and germanium and control method |
| CN111233036A (en) * | 2020-01-20 | 2020-06-05 | 昆明瀚创科技有限公司 | Made of Sb2O3Direct preparation of Sb with aqueous hydrochloric acid4O5Cl2Method (2) |
| CN111254292A (en) * | 2020-01-20 | 2020-06-09 | 昆明瀚创科技有限公司 | Method for removing nickel, cobalt and germanium by zinc sulfate aqueous solution purification |
| WO2021147809A1 (en) * | 2020-01-20 | 2021-07-29 | 昆明瀚创科技有限公司 | Method for preparing sb4o5cl2 directly from sb2o3 and aqueous hydrochloric acid solution |
| CN111233036B (en) * | 2020-01-20 | 2022-07-26 | 昆明瀚创科技有限公司 | Is composed of Sb 2 O 3 Direct preparation of Sb with aqueous hydrochloric acid 4 O 5 Cl 2 Method (2) |
| CN111197119A (en) * | 2020-02-25 | 2020-05-26 | 广州市尚信净化工程有限公司 | Method for recovering valuable metals from bismuth-containing waste residues |
| CN115305361A (en) * | 2022-08-26 | 2022-11-08 | 山东恒邦冶炼股份有限公司 | High-purity antimony rod and high-purity antimony white combined preparation process |
| CN115305361B (en) * | 2022-08-26 | 2023-05-09 | 山东恒邦冶炼股份有限公司 | High-purity antimony rod and high-purity antimony white combined preparation process |
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Application publication date: 20131002 |