CN103757439A - Method for recovering antimony and lead from antimony-lead-containing complex sulfide ore - Google Patents
Method for recovering antimony and lead from antimony-lead-containing complex sulfide ore Download PDFInfo
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- CN103757439A CN103757439A CN201410026152.9A CN201410026152A CN103757439A CN 103757439 A CN103757439 A CN 103757439A CN 201410026152 A CN201410026152 A CN 201410026152A CN 103757439 A CN103757439 A CN 103757439A
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Abstract
The invention discloses a method for recovering antimony and lead from antimony-lead-containing complex sulfide ores, belonging to the technical field of hydrometallurgy, and comprising the following steps: pulping the antimony-lead-containing complex sulfide ore to obtain ore pulp, separating metallic antimony from the ore pulp in a hydrochloric acid-ammonium chloride medium by an ore pulp electrolysis method, and performing solid-liquid separation on the leached ore pulp to obtain leachate and leaching residues; replacing the metallic silver in the leaching solution by using the metallic antimony to obtain metallic silver and an antimony-containing solution; dissolving and leaching the leaching slag by adopting a calcium chloride solution, and carrying out solid-liquid separation to obtain sulfur slag and a lead-containing solution; and replacing the metallic lead in the lead-containing solution by using metallic iron to obtain the metallic lead and the iron-containing solution. The invention provides a process for comprehensively recovering antimony and lead from antimony and lead-containing complex sulfide ores, which is a method for realizing clean and efficient comprehensive utilization of antimony and lead-containing complex sulfide ores.
Description
Technical field
The present invention relates to a kind of method that reclaims antimony, lead from antimonial lead complicated sulfuration mine, belong to technical field of wet metallurgy.
Background technology
In the recovery process of compound antimony ore, antimony conventionally forms the compound ore deposit with complicated mineral structure together with the association such as lead, silver, arsenic.And for compound antimony concentrate, aspect hydrometallurgical process, main technique has sodium sulphite leaching-diaphragm electrodeposition method, new chloride-hydrolysis, villaumite chlorination-low-temperature pyrolysis method and chlorine gas selecting lixiviation process.
The common advantage of above-mentioned technique is to have eliminated SO
2pollution problem to environment, antimony, plumbous thoroughly separated.Yet sodium sulphite leaching-diaphragm electrodeposition method is in electrolytic deposition process, due to Na
2s hyperplasia and Na
2sO
4, sodium polysulphide, Sulfothiorine etc. accumulation, need have special liquid waste disposal process, and current efficiency is low, power consumption and alkaline consumption are high; New chloride-hydrolysis exists institute's stibium trioxide that produces higher containing arsenic, does not reach zero level requirement, the shortcoming that product stability is poor, the stibium trioxide that produces placement just flavescence of for some time, therefore be difficult to sale; Villaumite chlorination-low-temperature pyrolysis method and the seriously corroded of chlorine gas selecting lixiviation process to equipment, and do not have and similarly put into practice factory, still need and carry out pilot-plant test checking.
Summary of the invention
Stibium trioxide that the present invention is for the power consumption that solves the antimony in the compound antimony concentrate of existing hydrometallurgic recovery, plumbous method and exist and alkaline consumption is higher, reclaim is higher containing arsenic, product stability is poor, the problem to the seriously corroded of equipment, and then has proposed a kind of antimony, plumbous method of reclaiming from antimonial lead complicated sulfuration mine.For this reason, the present invention proposes following technical scheme:
A method that reclaims antimony, lead from antimonial lead complicated sulfuration mine, comprising:
Described antimonial lead complicated sulfuration mine pulp is processed and obtained ore pulp, more described ore pulp is isolated to metallic antimony by slurry electrolysis in hydrochloric acid-ammonium chloride medium, then will leach ore pulp and obtain leach liquor and leached mud by solid-liquid separation;
Adopt described metallic antimony that the argent in described leach liquor is displaced, obtain argent and contain antimony solution;
Adopt calcium chloride solution to dissolve to leach described leached mud and by obtaining sulphur slag after solid-liquid separation and containing lead solution;
Adopt metallic iron to displace containing the metallic lead in lead solution described, obtain metallic lead and iron-containing liquor.
As seen from the above technical solution provided by the invention, the invention provides a kind of from antimonial lead complicated sulfuration mine the comprehensive technique that reclaims antimony lead, be to realize that antimonial lead complicated sulfuration mine resource is clean, the way of high-efficiency comprehensive utilization.
Embodiment
The schematic flow sheet that reclaims antimony, plumbous method from antimonial lead complicated sulfuration mine that Fig. 1 provides for the specific embodiment of the present invention.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein, only for description and interpretation the present invention, is not intended to limit the present invention.
The specific embodiment of the present invention provides a kind of method that reclaims antimony, lead from antimonial lead complicated sulfuration mine, as shown in Figure 1, its principle is: adopt slurry electrolysis to process antimonial lead complicated sulfuration mine, at hydrochloric acid---separated and produce metallic antimony plate in ammonium chloride medium, leaded leaching residue is again by leaching, iron powder replacement separate sulfur simple substance and lead, after leaching agent regeneration, part is returned to leaching, after the form output of part with hydrochloric acid, returns to in-pulp electrolysis operation.
Concrete, the method that reclaims antimony, lead from antimonial lead complicated sulfuration mine that this embodiment provides comprises:
Step 1, antimony lead ore pulpization is processed: by cyclone classification after the ball milling of antimonial lead ore deposit, a certain amount of water slurry is allocated in the ore deposit that reaches qualified particle diameter into, enters step 2;
Step 2, the separated antimony of slurry electrolysis: step 1 ore pulp is used in hydrochloric acid-ammonium chloride medium to the separated antimony of slurry electrolysis, antimony is with the form output of metallic antimony plate, and leaching pulp liquid-solid isolation obtains leach liquor and leached mud enters respectively step 3 and step 4;
Step 3, separation by displacement silver: displacement silver the in-pulp electrolysis leach liquor that the metallic antimony obtaining by step 2 produces from step 2, silver, with the form output of metal, returns to step 2 in-pulp electrolysis operation containing antimony solution;
Step 4, separated and dissolved lead: use the calcium chloride solution of predetermined concentration to dissolve the leached mud that leaches step 2 generation, lead enters liquid phase, after liquid-solid separation, the lead solution that contains of acquisition enters step 5, and slag is the main form output with sulphur slag;
Step 5, separation by displacement is plumbous: with metallic iron, from step 4, obtain containing the mid-separation of lead of changing of lead solution, lead is with the form output of spongy lead, the iron-containing liquor of acquisition enters step 6;
Step 6, regeneration and recycle: with the iron in lime precipitation separating step 6 liquid, iron is with the form output of scum, the calcium chloride solution obtaining partly returns to step 4 and dissolves splicer's order, part need to be returned to step 2 in-pulp electrolysis operation by adding the mode of sulfuric acid to be converted into hydrochloric acid according to technique, and output calcium sulfate.
Wherein, the antimonial lead complicated sulfuration mine in step 1 is the complicated sulfuration mine containing antimony associate lead, and after ball milling, cyclone classification, the particle diameter in qualified ore deposit is less than 74 μ m and accounts for the mass percent of measuring in whole ore deposits and is not less than 70%.Metallic antimony in step 3 divides with antimony or the form of antimony sheet adds described infusion solution, add-on is theoretical amount 0.9～1.1 times, temperature of reaction is 20～90 ℃, the reaction times is 0.5～2h.The concentration of the calcium chloride solution in step 4 is 100～400g/L, leaching process pH1～3, and the temperature of leaching is 20～90 ℃, the time of leaching is 1～5h, liquid-solid ratio 3:1～10:1.Metallic iron in step 5 is iron filings, iron powder or iron plate, and consumption is 0.9～1.1 times of theoretical amount, and the temperature of reaction of described replacement process is 20～90 ℃, and the reaction times is 0.5～2h.Lime in step 6 adds described iron-containing liquor with the form of lime powder or milk of lime, and add-on is 1.1～1.3 times of theoretical amount, and temperature of reaction is room temperature, and the reaction times is 0.5～2h.The calcium chloride solution of step 6 returns to step 4, and to dissolve the ratio of splicer's order be 70～100%, for the calcium chloride solution ratio of the hydrochloric acid of regenerating, is 0～30%.In step 6, the concentration of sulfuric acid is 60～98%, add-on is theoretical amount 0.9～1.0 times.
The method that reclaims antimony, lead from antimonial lead complicated sulfuration mine that this embodiment provides has following features:
(1) one step output metallic antimony, silver is with the form output of silver powder, and lead is with the form output of spongy lead, and sulphur is with the form output of elemental sulfur, and valuable element comprehensive utilization ratio is high.
(2) technique has realized regeneration and the recycle of part hydrochloric acid, has made up in prior art the unbalanced deficiency of whole system after hydrochloric acid consumption.
(3) whole technique all completes under condition of normal pressure, and reagent consumption is few, and equipment is simple and invest littlely, is easy to realize suitability for industrialized production, has a extensive future.
The surface modifying method of the metallic pigment that the present invention proposed below by specific embodiment elaborates.
Embodiment 1:
Raw ore after broken wet-milling particle diameter is less than 74 μ m and accounts for 80% antimony lead ore deposit ore pulp, in chlorination of hydrochloric acid ammonium system, carry out the separated output metallic antimony of in-pulp electrolysis, ore pulp carries out liquid-solid separation; The antimony powder that adds 0.9 times of theoretical amount in liquid, temperature of reaction is 90 ℃, the reaction times is 1h, displacement output argent, liquid returns to in-pulp electrolysis operation; Slag adopts the calcium chloride solution that concentration is 300g/L to dissolve leaching, leaching process pH～2.0, and extraction temperature is 40 ℃, and the time is 3h, and liquid-solid ratio is 5:1, carries out liquid-solid separation after having leached, output sulphur slag, liquid enters lower step operation; The iron replacement output spongy lead that adds 1.0 times of theoretical amount in liquid, temperature of reaction is 60 ℃, and the reaction times is 2h, has reacted rear liquid-solid separation, and liquid enters lower step operation; Using lime dry powder as neutralizing agent, the iron of step in solution in precipitation, add-on is theoretical amount 1.1 times, the reaction times is 1h; The calcium chloride solution 90% of regeneration returns to in-pulp electrolysis operation, adds vitriol oil regeneration output hydrochloric acid and the calcium sulfate of concentration 98% in 10% calcium chloride solution, and hydrochloric acid returns to in-pulp electrolysis operation.
Embodiment 2:
Raw ore after broken wet-milling particle diameter is less than 74 μ m and accounts for 70% antimony lead ore deposit ore pulp, in chlorination of hydrochloric acid ammonium system, carry out the separated output metallic antimony of in-pulp electrolysis, ore pulp carries out liquid-solid separation; The antimony powder that adds 1.1 times of theoretical amount in liquid, temperature of reaction is 20 ℃, the reaction times is 2h, displacement output argent, liquid returns to in-pulp electrolysis operation; Slag adopts the calcium chloride solution that concentration is 400g/L to dissolve leaching, leaching process pH～3.0, and extraction temperature is 90 ℃, and the time is 1h, and liquid-solid ratio is 3:1, carries out liquid-solid separation after having leached, output sulphur slag, liquid enters lower step operation; The iron replacement output spongy lead that adds 1.1 times of theoretical amount in liquid, temperature of reaction is 20 ℃, and the reaction times is 1.5h, has reacted rear liquid-solid separation, and liquid enters lower step operation; Using lime dry powder as neutralizing agent, the iron of step in solution in precipitation, add-on is theoretical amount 1.3 times, the reaction times is 0.5h; The calcium chloride solution of regeneration all returns to in-pulp electrolysis operation.
Embodiment 3:
Raw ore after broken wet-milling particle diameter is less than 74 μ m and accounts for 90% antimony lead ore deposit ore pulp, in chlorination of hydrochloric acid ammonium system, carry out the separated output metallic antimony of in-pulp electrolysis, ore pulp carries out liquid-solid separation; The antimony powder that adds 0.9 times of theoretical amount in liquid, temperature of reaction is 90 ℃, the reaction times is 0.5h, displacement output argent, liquid returns to in-pulp electrolysis operation; Slag adopts the calcium chloride solution that concentration is 100g/L to dissolve leaching, leaching process pH～1.0, and extraction temperature is 20 ℃, and the time is 5h, and liquid-solid ratio is 10:1, carries out liquid-solid separation after having leached, output sulphur slag, liquid enters lower step operation; The iron replacement output spongy lead that adds 0.9 times of theoretical amount in liquid, temperature of reaction is 90 ℃, and the reaction times is 0.5h, has reacted rear liquid-solid separation, and liquid enters lower step operation; Using lime dry powder as neutralizing agent, the iron of step in solution in precipitation, add-on is theoretical amount 1.2 times, the reaction times is 2h; The calcium chloride solution 95% of regeneration returns to in-pulp electrolysis operation, adds vitriol oil regeneration output hydrochloric acid and the calcium sulfate of concentration 60% in 5% calcium chloride solution, and hydrochloric acid returns to in-pulp electrolysis operation
Embodiment 4:
Raw ore after broken wet-milling particle diameter is less than 74 μ m and accounts for 100% antimony lead ore deposit ore pulp, in chlorination of hydrochloric acid ammonium system, carry out the separated output metallic antimony of in-pulp electrolysis, ore pulp carries out liquid-solid separation; The antimony powder that adds 0.9 times of theoretical amount in liquid, temperature of reaction is 60 ℃, the reaction times is 1.5h, displacement output argent, liquid returns to in-pulp electrolysis operation; Slag adopts the calcium chloride solution that concentration is 250g/L to dissolve leaching, leaching process pH～1.5, and extraction temperature is 50 ℃, and the time is 2h, and liquid-solid ratio is 7:1, carries out liquid-solid separation after having leached, output sulphur slag, liquid enters lower step operation; The iron replacement output spongy lead that adds 1.0 times of theoretical amount in liquid, temperature of reaction is 30 ℃, and the reaction times is 2h, has reacted rear liquid-solid separation, and liquid enters lower step operation; Using lime dry powder as neutralizing agent, the iron of step in solution in precipitation, add-on is theoretical amount 1.1 times, the reaction times is 1h; The calcium chloride solution of regeneration all returns to in-pulp electrolysis operation.
Embodiment 5:
Raw ore after broken wet-milling particle diameter is less than 74 μ m and accounts for 850% antimony lead ore deposit ore pulp, in chlorination of hydrochloric acid ammonium system, carry out the separated output metallic antimony of in-pulp electrolysis, ore pulp carries out liquid-solid separation; The antimony powder that adds 1.0 times of theoretical amount in liquid, temperature of reaction is 70 ℃, the reaction times is 2h, displacement output argent, liquid returns to in-pulp electrolysis operation; Slag adopts the calcium chloride solution that concentration is 350g/L to dissolve leaching, leaching process pH～2.5, and extraction temperature is 80 ℃, and the time is 1.5h, and liquid-solid ratio is 4:1, carries out liquid-solid separation after having leached, output sulphur slag, liquid enters lower step operation; The iron replacement output spongy lead that adds 1.0 times of theoretical amount in liquid, temperature of reaction is 50 ℃, and the reaction times is 1h, has reacted rear liquid-solid separation, and liquid enters lower step operation; Using lime dry powder as neutralizing agent, the iron of step in solution in precipitation, add-on is theoretical amount 1.2 times, the reaction times is 2h; The calcium chloride solution 70% of regeneration returns to in-pulp electrolysis operation, adds vitriol oil regeneration output hydrochloric acid and the calcium sulfate of concentration 98% in 30% calcium chloride solution, and hydrochloric acid returns to in-pulp electrolysis operation.
The above; it is only preferably embodiment of the present invention; but protection scope of the present invention is not limited to this; anyly be familiar with those skilled in the art in the technical scope that the embodiment of the present invention discloses; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (10)
1. a method that reclaims antimony, lead from antimonial lead complicated sulfuration mine, is characterized in that, comprising:
Described antimonial lead complicated sulfuration mine pulp is processed and obtained ore pulp, more described ore pulp is isolated to metallic antimony by slurry electrolysis in hydrochloric acid-ammonium chloride medium, then will leach ore pulp and obtain leach liquor and leached mud by solid-liquid separation;
Adopt described metallic antimony that the argent in described leach liquor is displaced, obtain argent and contain antimony solution;
Adopt calcium chloride solution to dissolve to leach described leached mud and by obtaining sulphur slag after solid-liquid separation and containing lead solution;
Adopt metallic iron to displace containing the metallic lead in lead solution described, obtain metallic lead and iron-containing liquor.
2. method according to claim 1, is characterized in that, described method also comprises:
By the metallic iron in iron-containing liquor described in lime precipitation, and obtain calcium chloride solution;
Described calcium chloride solution is leached to described leached mud or by adding the mode of sulfuric acid to be converted into the hydrochloric acid for described slurry electrolysis for dissolving, and output calcium sulfate.
3. method according to claim 2, is characterized in that, described lime adds described iron-containing liquor with the form of lime powder or milk of lime, and temperature of reaction is room temperature, and the reaction times is 0.5～2h.
4. method according to claim 2, is characterized in that, described calcium chloride solution leaches described leached mud ratio for dissolving is 70～100%, for being converted into the ratio of hydrochloric acid, is 0～30%.
5. method according to claim 2, is characterized in that, the concentration of described sulfuric acid is 60～98%.
6. method according to claim 1, is characterized in that, described antimonial lead complicated sulfuration mine is the complicated sulfuration mine containing antimony associate lead, and after ball milling, cyclone classification, the particle diameter in qualified ore deposit is less than 74 μ m and accounts for the mass percent of measuring in whole ore deposits and is not less than 70%.
7. method according to claim 1, is characterized in that, described metallic antimony divides with antimony or the form of antimony sheet adds described infusion solution, and temperature of reaction is 20～90 ℃, and the reaction times is 0.5～2h.
8. method according to claim 1, is characterized in that, the concentration of described calcium chloride solution is 100～400g/L, leaching process pH1～3.
9. method according to claim 1, is characterized in that, the temperature of described leaching is 20～90 ℃, and the time of leaching is 1～5h, liquid-solid ratio 3:1～10:1.
10. method according to claim 1, is characterized in that, described metallic iron is iron filings, iron powder or iron plate, and the temperature of reaction of described replacement process is 20～90 ℃, and the reaction times is 0.5～2h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106893860A (en) * | 2017-02-24 | 2017-06-27 | 中南大学 | It is a kind of to process the method containing antimony sulphide ore |
| CN106367780B (en) * | 2016-08-31 | 2018-08-28 | 北京矿冶研究总院 | Method for producing antimony by rotational flow electrodeposition of antimony-containing solution |
| CN111020635A (en) * | 2019-12-19 | 2020-04-17 | 新邵辰州锑业有限责任公司 | Novel be arranged in ore pulp electrolysis antimony smelting hydrochloric acid recovery device |
| CN113354164A (en) * | 2021-08-10 | 2021-09-07 | 北京矿冶研究总院 | Comprehensive treatment method of acid wet antimony smelting solution |
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| CN1381612A (en) * | 2002-03-11 | 2002-11-27 | 北京矿冶研究总院 | Method for producing antimony by electrolyzing antimony-containing sulfide mineral pulp |
| CN101555550A (en) * | 2009-05-22 | 2009-10-14 | 北京科技大学 | Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board |
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2014
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| CN1381612A (en) * | 2002-03-11 | 2002-11-27 | 北京矿冶研究总院 | Method for producing antimony by electrolyzing antimony-containing sulfide mineral pulp |
| CN101555550A (en) * | 2009-05-22 | 2009-10-14 | 北京科技大学 | Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106367780B (en) * | 2016-08-31 | 2018-08-28 | 北京矿冶研究总院 | Method for producing antimony by rotational flow electrodeposition of antimony-containing solution |
| CN106893860A (en) * | 2017-02-24 | 2017-06-27 | 中南大学 | It is a kind of to process the method containing antimony sulphide ore |
| CN111020635A (en) * | 2019-12-19 | 2020-04-17 | 新邵辰州锑业有限责任公司 | Novel be arranged in ore pulp electrolysis antimony smelting hydrochloric acid recovery device |
| CN113354164A (en) * | 2021-08-10 | 2021-09-07 | 北京矿冶研究总院 | Comprehensive treatment method of acid wet antimony smelting solution |
| CN113354164B (en) * | 2021-08-10 | 2021-11-02 | 北京矿冶研究总院 | Comprehensive treatment method of acid wet antimony smelting solution |
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