CN101864522B - Clean metallurgical method for low-temperature molten salt of lead - Google Patents
Clean metallurgical method for low-temperature molten salt of lead Download PDFInfo
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- CN101864522B CN101864522B CN2010102109640A CN201010210964A CN101864522B CN 101864522 B CN101864522 B CN 101864522B CN 2010102109640 A CN2010102109640 A CN 2010102109640A CN 201010210964 A CN201010210964 A CN 201010210964A CN 101864522 B CN101864522 B CN 101864522B
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Abstract
The invention discloses a clean metallurgical method for low-temperature molten salt of lead. Lead sulfide concentrate, secondary lead raw material or secondary material of lead is smelted in low-temperature inertial molten salt and rough lead is refined in one step; and a metal oxide is used as a sulfur fixing agent, wherein the smelted product comprises liquid metal lead and solid sulfur-fixing metal sulfide and the solid sulfur-fixing metal sulfide and solid unreacted material are together called solid matter; the majority of the inertial molten salt is separated from the solid matter to return the smelting process in hot state; a small part of the inertial molten salt adhered by the solid matter is processed by a wet method for recycling; the solid matter after the molten salt is removed by soaking is subjected to ore dressing to recover associated metal and the sulfur-fixing metal sulfide; the sulfide is baked for desulfurization; the smoke is used for making acid; and the oxide is calcined and returned to the smelting process and used as the sulfur fixing agent. The method greatly reduces the metallurgical temperature of the lead, produces the rough lead in one step, realizes the recovery of the sulfur and the utilization of the sulfide energy source, has simple flow and low cost, greatly improves the yield of the vertical force and completely eliminates the lead steam produced during the metallurgical process and the pollution caused by the SO2 smoke to the environment.
Description
Technical field
The present invention relates to a kind of clean metallurgical method for low-temperature molten salt of lead, belong to the Non-ferrous Metallurgy field.
Background technology
The tradition lead smelting technology mainly is sinter machine sintering-retailoring of blast furnace or bottom convertor melting technology; All be under 1250-1350 ℃ high temperature, to carry out; Not only power consumption is high, and insoluble environmental problem below existing: the plumbous mist of (1) plumbous smelting process generation great quantity of Pb steam and disperse causes the severe contamination at factory's surrounding area air, soil and water source; (2) high-temperature process that produce copper dross slag in smelting process, contains zinc furnace cinder etc. also produces a large amount of lead dusts and low concentration SO
2Smoke pollution, the processing of lead matte and the recovery of copper are still unsolved at present difficult problems; (3) traditional lead smelting technology can not or the complicated lead ore of intractable, secondary lead raw material and secondary lead material.
Summary of the invention
The object of the present invention is to provide a kind of clean metallurgical method for low-temperature molten salt of lead.This method significantly reduces plumbous smelting temperature, a step output lead bullion, and realize the recovery and the utilization of the sulfide energy of sulphur, in the simplification flow process, reduce cost, significantly improve vertical yield in, thoroughly eliminate high temperature lead dust and low concentration SO
2Flue gas is to the pollution of ecotope, and can handle complicated lead ores such as plumbous zinc ore, lead bronze ore deposit and plumbous nickel cobalt ore, secondary lead raw materials such as scrap lead acid battery clay, secondary lead materials such as sulfuric acid lead skim, lead fume dirt, lead matte.
The objective of the invention is to realize in the following manner:
A kind of clean metallurgical method for low-temperature molten salt of lead may further comprise the steps:
1) make sulphur-fixing agent with MOX, lead-containing material concentrate of lead sulfide ore or complicated lead ore or secondary lead raw material or secondary lead material are carried out solid sulfur reduction melting in low temperature inertia fused salt, step refining lead bullion, and obtain the mixture of inertia fused salt and solids; Lead bullion is emitted and natural separation by siphon in the bottom of the mixture of inertia fused salt and solids;
The described MOX of making sulphur-fixing agent is secondary zinc oxide or zinc-oxide calcine, or cupric oxide material or cupric oxide calcining;
Described inertia fused salt is the fused salt mixt of yellow soda ash fused salt or yellow soda ash and sodium hydroxide, and the sodium hydroxide mass content is not higher than 10% in the fused salt mixt;
Described solid sulfur reduction melting condition is: 1. temperature is 800～950 ℃; 2. time 1～5h; 3. admittedly sulfur metal oxide compound consumption is 1～1.5 times of theoretical amount; 4. make reductive agent with fine coal or coke powder, the reductive agent consumption is the 5-20% of lead-containing material quality, and 5. inertia fused salt consumption is 1.5～4 times of all reactant quality;
2) then the inertia fused salt is separated the back with the hot fusion process that returns step 1) with solids, the isolated solids fused salt of water logging slag;
3) to step 2) the water logging slag carry out ore dressing, obtain solid sulfur metal sulfide product and associated metal concentrate, perhaps further will consolidate sulfur metal sulfide desulfurization with roasting technique, flue gas acid preparing, the oxide compound calcining that obtains returns the fusion process of step 1) and makes sulphur-fixing agent; To step 2) infusion in feed the carbonic acid gas precipitate sodium bicarbonate, the sodium hydrogencarbonate that obtains returns the fusion process of step 1), and mother liquor returns step 2) the water logging process.
Described complicated lead ore is plumbous zinc ore, lead bronze ore deposit and plumbous nickel cobalt ore; Described secondary lead raw material is a scrap lead acid battery clay; Described secondary lead material is sulfuric acid lead skim, lead fume dirt and lead matte.
Described step 2) adopt fining process to separate inertia fused salt and solids in, actual conditions is: 1. temperature is 800～950 ℃, and 2. 3. time 0.5～5h slowly gushes top clarification fused salt just.
Described step 2) solids fused salt pulp water soaks process condition and is in: 1. temperature is 50～100 ℃, 2. time 0.5～6h, and 3. liquid-solid volume mass ratio is 1～8: 1ml/g, water washing leached mud 3～5 times is to PH=7～8.
The condition of precipitate sodium bicarbonate process is in the described step 3): 1. temperature 10-95 ℃, 2. the time is 0.5-10h, 3. CO
2Volumetric usage is 1.05-2 a times of theoretical amount, 4. reacts to pH=3～8.
Technological process principle of the present invention
In the low temperature inertia fused salt that with yellow soda ash is main body, lead sulfide in lead ore concentrate or complicated lead ore or the secondary lead and lead sulfate and reductive agent and ZnO or CuO produce solid sulfur reduction reaction under 650～950 ℃ of temperature:
2PbS+2ZnO+C＝2Pb+2ZnS+CO
2 (1)
2PbS+2CuO+C＝2Pb+2CuS+CO
2 (2)
PbSO
4+ZnO+2.5C＝Pb+ZnS+2.5CO
2 (3)
PbSO
4+CuO+2.5C＝Pb+CuS+2.5CO
2 (4)
Plumbous oxide produces reduction reaction:
PbO+CO＝Pb+CO
2 (5)
PbO
2+C＝Pb+CO
2 (6)
FeS
2Also change into FeO and ZnS:
FeS
2+2ZnO＝FeO+2ZnS (7)
At the melting initial stage, the sodium hydrogencarbonate after returning decomposes:
2NaHCO
3＝Na
2CO
3+H
2O+CO
2 (8)
In infusion, feed the carbonic acid gas precipitate sodium bicarbonate:
2NaOH+CO
2＝NaHCO
3+H
2O (9)
Na
2CO
3+CO
2+H
2O＝2NaHCO
3 (10)
SiO in the furnace charge
2, Al
2O
3, CaCO
3, MgCO
3, FeO, CuS etc. are nonreactant, do not participate in reaction, they form the fused salt slag with the ZnS CuS that melting generates as solids.
In sum; The present invention is through a low-temperature molten salt metallurgical method that relates to the gas, liquid, solid three-phase equilibrium; This method is made sulphur-fixing agent with the oxide compound that a kind of avidity with sulphur compares the much bigger metal of lead; The all recyclable utilization of the sulphur and the sulfide energy is carried out in realization melting, solid sulphur and alkali regeneration synchronously.This method can significantly reduce plumbous smelting temperature, and a step is produced lead bullion, when simplifying flow process, reducing cost, significantly improve vertical yield, thoroughly eliminates the lead steam and the low concentration SO that produce in the high-temperature smelting process
2Flue gas has advantages such as low-carbon (LC), cleaning, efficient and suitable dealing with complicated lead ore and secondary lead resource to the pollution of ecotope, and technical progress and the energy-saving and emission-reduction that promote lead smelting in China industry are significant.
Description of drawings
Fig. 1 is a schematic flow sheet of the present invention.
Embodiment
Following examples are intended to further specify the present invention, and unrestricted the present invention.
Embodiment 1
The chemical constitution of concentrate of lead sulfide ore is (%): Pb70.12, Fe6.08, S15.04, Zn2.84, Cu0.40, SiO
20.79., the chemical constitution of fine coal is (%): C 82.33, S 3.01, SiO
26.66, CaO 0.83, Al
2O
34.81.Take by weighing 100g concentrate of lead sulfide ore, 10.0 fine coal, 200g technical grade yellow soda ash respectively and contain the secondary zinc oxide 35.07g uniform mixing of Zn78.33%; The plumbago crucible of packing into; Then in resistance furnace at 900 ℃ of following melting 2h; Output contains the lead bullion 67.34g of Pb 98.40%, and plumbous direct yield reaches 94.5%; Obtain the solids slag 111.7g of fusion yellow soda ash 162.5g and bonding small portion yellow soda ash behind the hot fused salt clarification separate solid thing, leach 3h at normal temperatures, must do leached mud 71.3, contain Zn 42.51%, S21.01%, sulfur-fixing rate 99.61% with the 300mL tap water; Filtrate volume is 340mL, contains Na
2CO
3180g/L at room temperature feeds CO
2, eutectoid goes out NaHCO
365g gets mother liquor 330ml. and contains NaHCO
356g/L.
Embodiment 2
With the scrap battery clay is raw material, and composition is: Pb74.15%, and S 7.85%, and coke powder contains C 82%, ash content 10% as reductive agent.Take by weighing 100g clay, 15g coke powder respectively and contain the cupric oxide cigarette ash 31.79g of Cu49.03%, add the fusion yellow soda ash 162.5g that embodiment 1 returns, uniform mixing, the plumbago crucible of packing into covers the NaHCO that embodiment 1 returns again
365g.Then in resistance furnace at 870 ℃ of following melting 1.5h, output contains the lead bullion 72.13g of Pb 97.66%, plumbous direct yield reaches 95.00%; Obtain the solids slag 71.2g of fusion yellow soda ash 146g and bonding small portion yellow soda ash behind the hot fused salt clarification separate solid thing; Leach under the condition of normal temperature, time 2h with the 300mL tap water, must do leached mud 54.2g, contain Cu28.76%; S14.48%, sulfur-fixing rate 99.99%; Filtrate volume is 360mL, contains Na
2CO
3165g/L at room temperature feeds CO
2, eutectoid goes out NaHCO
358.63g, get mother liquor 350ml. and contain NaHCO
354.3g/L.
Embodiment 3
With the lead bronze concentrate is raw material, and its composition (%) is: Pb40.85, Cu18.17, Zn8.87, S20.16%, SiO
23.27, Fe5.66, the fine coal of embodiment 1 is made reductive agent, and the cupric oxide cigarette ash of embodiment 2 is made sulphur-fixing agent.Take by weighing 500g lead bronze concentrate, 40g fine coal respectively and contain the cupric oxide cigarette ash 127.76g of Cu49.03%, add yellow soda ash 852g, uniform mixing, the plumbago crucible of packing into covers NaHCO again
3325g.Then in resistance furnace at 860 ℃ of following melting 1.0h, output contains the lead bullion 194.96g of Pb 98.06%, plumbous direct yield reaches 93.60%; Obtain the solids slag 591.56g of fusion yellow soda ash 750g and bonding small portion yellow soda ash behind the hot fused salt clarification separate solid thing; Leach under the condition of normal temperature, time 2.5h with the 1500mL tap water, washing must be done leached mud 284.5g; Contain Cu53.95%; Zn15.59%, S34.80%, sulfur-fixing rate 98.12%; Filtrate volume is 1760mL, contains Na
2CO
3174.5g/L, at room temperature feed CO
2, eutectoid goes out NaHCO
3398.65g, get mother liquor 1650ml. and contain NaHCO
354.3g/L.
Embodiment 4
With the lead and zinc concentrate is raw material, and its composition (%) is: Pb38.65, Cu0.27, Zn28.87, S22.11%, SiO
25.27, Fe3.26, the fine coal of embodiment 1 is made reductive agent, and the secondary zinc oxide of embodiment 1 is made sulphur-fixing agent.Take by weighing 200g lead and zinc concentrate, 20g fine coal respectively and contain the secondary zinc oxide 40.88g of Zn78.33%, add yellow soda ash 340g, uniform mixing, the plumbago crucible of packing into covers NaHCO again
3130g.Then in resistance furnace at 880 ℃ of following melting 1.5h, output contains the lead bullion 73.96g of Pb98.45%, plumbous direct yield is 94.20%; Obtain the solids slag 283.2g of fusion yellow soda ash 310g and bonding small portion yellow soda ash behind the hot fused salt clarification separate solid thing; Leach under the condition of normal temperature, time 1.5h with the 700mL tap water, washing must be done leached mud 171.2g; Contain Zn52.43%; Cu0.32%, S25.83%, sulfur-fixing rate 99.98%; Filtrate volume is 744mL, contains Na
2CO
3150.57g/L, at room temperature feed CO
2, eutectoid goes out NaHCO
3137.23g, get mother liquor 720ml. and contain NaHCO
356.0g/L.
Embodiment 5
With composition (%) is Pb25.56, Fe6.61, S13.10, Co0.60, Cu2.46, Ni0.37, SiO
223.08 the flotation of lead nickel cobalt concentrate in Australia ore deposit be raw material, the fine coal of embodiment 1 is made reductive agent, the cupric oxide cigarette ash of embodiment 2 is made sulphur-fixing agent.Take by weighing the plumbous nickel cobalt concentrate of 500g, 25g fine coal respectively and contain the cupric oxide cigarette ash 156.64g of Cu49.03%, add yellow soda ash 1000g, uniform mixing, the plumbago crucible of packing into covers NaHCO again
3317g.Then in resistance furnace at 880 ℃ of following melting 1.5h, output contains the lead bullion 112.25g of Pb 98.00%, plumbous direct yield reaches 86.07%; Obtain the solids slag 651.68g of fusion yellow soda ash 850g and bonding small portion yellow soda ash behind the hot fused salt clarification separate solid thing, under the condition of normal temperature, time 2.0h, leach washing with the 1950mL tap water; Must do leached mud 301.68g, contain Cu29.53%, Pb5.78%; Fe10.96%, S21.70%, CoO.99%; Ni0.61%, SiO
238.25%, sulfur-fixing rate 99.94%; Filtrate volume is 2060mL, contains Na
2CO
3169.9g/L, at room temperature feed CO
2, eutectoid goes out NaHCO
3442.41g, get mother liquor 2020ml. and contain NaHCO
355.6g/L.Find Cu, Ni, Co sulfide and SiO
2No chemical transformation, with solid-state entering smelting slag, owing to lead sulfide and pyritous melting reaction have destroyed the raw ore structure, free copper, nickel, cobalt sulphide ores, thus help reclaiming.
Embodiment 6
With the sulfuric acid lead skim is raw material, and its composition (%) is: Pb45.37, Cu0.24, Zn6.21, Fe4.51, S11.02%, SiO
23.35, CaO1.83, the fine coal of embodiment 1 is made reductive agent, and the secondary zinc oxide that contains Zn70.30% and Pb12.07% is made sulphur-fixing agent.Take by weighing 200g sulfuric acid lead skim, 30g fine coal and secondary zinc oxide 40.75g respectively, add yellow soda ash 320g, uniform mixing, the plumbago crucible of packing into covers NaHCO again
3110g.Then in resistance furnace at 860 ℃ of following melting 2.5h, output contains the lead bullion 92.15g of Pb97.45%, plumbous direct yield is 93.88%; Obtain the solids slag 159.55g of fusion yellow soda ash 315g and bonding small portion yellow soda ash behind the hot fused salt clarification separate solid thing; Leach under the condition of normal temperature, time 2h with the 600mL tap water; Wash dried leached mud 85.15g, contain Zn48.23%, Cu0.56%; S25.59%, sulfur-fixing rate 98.87%; Filtrate volume is 624mL, contains Na
2CO
3119.24g/L, at room temperature feed CO
2, eutectoid goes out NaHCO
384.77g, get mother liquor 605ml. and contain NaHCO
354.8g/L.
Embodiment 7
With lead fume dirt is raw material, and its composition (%) is: Pb46.64, Cu trace, Zn4.5, Fe0.56, S4.30%, SiO
20.73, CaO0.61, the fine coal of embodiment 1 is made reductive agent, embodiment 2 secondary zinc oxide make sulphur-fixing agent.Take by weighing 200g lead fume dirt, 15g fine coal and secondary zinc oxide 12.21g respectively, add yellow soda ash 250g, uniform mixing, the plumbago crucible of packing into covers NaHCO again
3100g.Then in resistance furnace at 850 ℃ of following melting 1.5h, output contains the lead bullion 92.17g of Pb98.36%, plumbous direct yield is 95.68%; Obtain the solids slag 169.43g of fusion yellow soda ash 274g and bonding small portion yellow soda ash behind the hot fused salt clarification separate solid thing; Leach under the condition of normal temperature, time 1.5h with the 400mL tap water; Washing must be done leached mud 30.33g, contains Zn57.97%; S28.36%, the nearly a hundred per cent of sulfur-fixing rate; Filtrate volume is 414mL, contains Na
2CO
394.43g/L, at room temperature feed CO
2, eutectoid goes out NaHCO
339.53g, get mother liquor 405ml. and contain NaHCO
355.4g/L.
Embodiment 8
With the lead matte is raw material, and its composition (%) is: Pb26.20, Cu15.17, Zn8.20, S23.04%, SiO
21.27, Fe17.66, the fine coal of embodiment 1 is made reductive agent, and the cupric oxide cigarette ash of embodiment 2 is made sulphur-fixing agent.Take by weighing 200g lead matte, 20g fine coal respectively and contain the cupric oxide cigarette ash 92.23g of Cu49.03%, add yellow soda ash 405g, uniform mixing, the plumbago crucible of packing into covers NaHCO again
3215g.Then in resistance furnace at 900 ℃ of following melting 2.0h, output contains the lead bullion 47.74g of Pb 97.24%, plumbous direct yield reaches 88.60%; Obtain the solids slag 254.95g of fusion yellow soda ash 450g and bonding small portion yellow soda ash behind the hot fused salt clarification separate solid thing; Leach under the condition of normal temperature, time 3.0h with the 800mL tap water, washing must be done leached mud 164.3g; Contain Cu45.99%; Zn9.98%, S27.85%, sulfur-fixing rate 99.30%; Filtrate volume is 840mL, contains Na
2CO
3107.92g/L, at room temperature feed CO
2, eutectoid goes out NaHCO
397.86g, get mother liquor 818ml. and contain NaHCO
356g/L.
Claims (5)
1. the clean metallurgical method for low-temperature molten salt of a lead is characterized in that, may further comprise the steps:
1) make sulphur-fixing agent with MOX, lead-containing material concentrate of lead sulfide ore or complicated lead ore or secondary lead raw material or secondary lead material are carried out solid sulfur reduction melting in low temperature inertia fused salt, step refining lead bullion, and obtain the mixture of inertia fused salt and solids; Lead bullion is emitted and natural separation by siphon in the bottom of the mixture of inertia fused salt and solids;
The described MOX of making sulphur-fixing agent is secondary zinc oxide or zinc-oxide calcine, or cupric oxide material or cupric oxide calcining;
Described inertia fused salt is the fused salt mixt of yellow soda ash fused salt or yellow soda ash and sodium hydroxide, and the sodium hydroxide mass content is not higher than 10% in the fused salt mixt;
Described solid sulfur reduction melting condition is: 1. temperature is 800～950 ℃; 2. time 1～5h; 3. admittedly sulfur metal oxide compound consumption is 1～1.5 times of theoretical amount; 4. make reductive agent with fine coal or coke powder, the reductive agent consumption is the 5-20% of lead-containing material quality, and 5. inertia fused salt consumption is 1.5～4 times of all reactant quality;
2) then the inertia fused salt is separated the back with the hot fusion process that returns step 1) with solids, the isolated solids fused salt of water logging slag;
3) to step 2) the water logging slag carry out ore dressing, obtain solid sulfur metal sulfide product and associated metal concentrate, perhaps further will consolidate sulfur metal sulfide desulfurization with roasting technique, flue gas acid preparing, the oxide compound calcining that obtains returns the fusion process of step 1) and makes sulphur-fixing agent; To step 2) infusion in feed the carbonic acid gas precipitate sodium bicarbonate, the sodium hydrogencarbonate that obtains returns the fusion process of step 1) and mother liquor returns step 2) the water logging process.
2. the clean metallurgical method for low-temperature molten salt of a kind of lead according to claim 1, it is characterized in that: described complicated lead ore is plumbous zinc ore, lead bronze ore deposit and plumbous nickel cobalt ore; Described secondary lead raw material is a scrap lead acid battery clay; Described secondary lead material is sulfuric acid lead skim, lead fume dirt and lead matte.
3. the clean metallurgical method for low-temperature molten salt of a kind of lead according to claim 1; It is characterized in that: adopt fining process to separate inertia fused salt and solids described step 2); Actual conditions is: 1. temperature is 800～950 ℃, 2. time 0.5～5h, and top clarification fused salt 3. slowly comes down in torrents.
4. the clean metallurgical method for low-temperature molten salt of a kind of lead according to claim 1; It is characterized in that: solids fused salt pulp water soaks process condition and is described step 2): 1. temperature is 50～100 ℃; 2. time 0.5～6h; 3. liquid-solid volume mass ratio is 1～8: 1ml/g, water washing leached mud 3～5 times is to PH=7～8.
5. the clean metallurgical method for low-temperature molten salt of a kind of lead according to claim 1, it is characterized in that: the condition of precipitate sodium bicarbonate process is in the described step 3): 1. temperature 10-95 ℃, 2. the time is 0.5-10h, 3. CO
2Volumetric usage is 1.05-2 a times of theoretical amount, 4. reacts to pH=3～8.
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|---|---|---|---|
| CN2010102109640A CN101864522B (en) | 2010-06-28 | 2010-06-28 | Clean metallurgical method for low-temperature molten salt of lead |
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|---|---|---|---|
| CN2010102109640A CN101864522B (en) | 2010-06-28 | 2010-06-28 | Clean metallurgical method for low-temperature molten salt of lead |
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| CN101864522B true CN101864522B (en) | 2012-07-25 |
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| CN103266226B (en) * | 2013-04-27 | 2014-08-20 | 中南大学 | Method for extracting silver from silver-containing zinc concentrate and improving quality of zinc concentrate |
| CN103320614B (en) * | 2013-07-10 | 2015-11-18 | 郴州市金贵银业股份有限公司 | A kind of lead matte pyrogenic attack technique |
| CN104451161A (en) * | 2014-12-04 | 2015-03-25 | 中南大学 | Method for low-temperature smelting of regenerated lead |
| CN104862483A (en) * | 2015-05-13 | 2015-08-26 | 杨华锋 | Method for disposing secondary lead materials by high oxygen-enriched side-blown bath smelting combination acid-making system |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1003654B (en) * | 1984-02-07 | 1989-03-22 | 波利顿股份公司 | Method for producing metallic lead by direct lead-smelting |
| CN1124297A (en) * | 1994-12-08 | 1996-06-12 | 景治熙 | Technique for producing metal by directly smelting sulphide ore |
| CN101724753A (en) * | 2009-12-28 | 2010-06-09 | 中南大学 | Low-temperature alkaline lead-smelting method |
-
2010
- 2010-06-28 CN CN2010102109640A patent/CN101864522B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1003654B (en) * | 1984-02-07 | 1989-03-22 | 波利顿股份公司 | Method for producing metallic lead by direct lead-smelting |
| CN1124297A (en) * | 1994-12-08 | 1996-06-12 | 景治熙 | Technique for producing metal by directly smelting sulphide ore |
| CN101724753A (en) * | 2009-12-28 | 2010-06-09 | 中南大学 | Low-temperature alkaline lead-smelting method |
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