CN101914693B - Clean metallurgical method for low-temperature molten salt of antimony - Google Patents
Clean metallurgical method for low-temperature molten salt of antimony Download PDFInfo
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- CN101914693B CN101914693B CN2010102690427A CN201010269042A CN101914693B CN 101914693 B CN101914693 B CN 101914693B CN 2010102690427 A CN2010102690427 A CN 2010102690427A CN 201010269042 A CN201010269042 A CN 201010269042A CN 101914693 B CN101914693 B CN 101914693B
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- antimony
- fused salt
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Abstract
The invention discloses a clean metallurgical method for low-temperature molten salt of antimony, and belongs to the metallurgical field of non-ferrous metals. The method is characterized by comprising the following steps of: performing reductive sulfur-fixing melting on antimony concentrate and oxide of metal with higher sulfur affinity compared with the antimony in low-temperature inert molten salt to generate liquid metal antimony and sulfur-fixed metal sulfide, and forming molten salt slag by using the sulfur-fixed metal sulfide and non-reacted substances as solid substances; and separating most inert molten salt from the solid substances and then thermally returning the most inert molten salt to the melting process, regenerating NaHCO3 for recycling by using the molten salt slag through a 'water leaching-carbonated precipitation' process, reclaiming the sulfur-fixed metal sulfide concentrate for selling from the leached residue by ore dressing, or performing roasting desulfuration on the leached residue for heat energy utilization and smoke acid making, and returning oxide roasting sand serving as a sulfur-fixing agent to the melting process. The method greatly reduces the antimony melting temperature, produces the crude antimony at one step, realizes reclamation of sulfur and energy utilization of sulfide, thoroughly eliminates environmental pollution of low-concentration SO2 smoke at the same time of simplifying the flow, reducing the cost and greatly improving the direct yield of the antimony, and has the advantages of low carbon, cleanness and high efficiency.
Description
Technical field
The present invention relates to a kind of clean metallurgical method for low-temperature molten salt of antimony, belong to the Non-ferrous Metallurgy field.
Background technology
Current, the smelting technology that from stibnite concentrate, extracts Antimony Metal 99.65& 99.96 is main with " blast furnace volatile smelting-reverberatory furnace retailoring ".This technology is as the alternative techniques of deposition melting; Earlier stibnite concentrate is pressed group or granulation, add blast furnace with coke and flux again, under the operation system in " low column, the thin bed of material, high coke yield, hot-top ", carry out volatile smelting; Make ANTIMONY SULPHIDE volatilization oxidation; Thereby separate with other impurity with gangue, the weisspiessglanz of generation gets into the condensation dust collecting system with flue gas and collects, again through reverberatory furnace retailoring output needle antimony.This technology is strong to adaptability to raw material, and processing power is big, but high, the defectives such as energy consumption is big, dust collecting system is huge, trivial operations of the burnt rate of ubiquity.Especially produce low concentration SO in blast furnace volatile smelting operation
2Flue gas, serious pollution of ecological environment is a still unsolved technical barrier so far.For avoiding the antimony pyrometallurgical smelting process environments to pollute drawback, once adopted parlkaline wet method stibium smelting technology both at home and abroad, but fail to apply because of production cost is high; " chlorination leaching-electrodeposition method " and " slurry electrolysis " are also because of problems such as quick-fried antimony, equipment corrosion, wastewater treatments, and industrialization prospect is dull; Realized that two more than ten years of industrialization " new chloride-hydrolysis " can produce high-purity weisspiessglanz, still adopted at present, but greatly also be difficult to extensive popularization because of wastewater discharge by minority producer.Be the existing stibium smelting technology of thoroughly reform, the present invention combines solid sulphur melting of the reduction of sulphide ores and low-temperature molten salt metallurgy, proposes a kind of low-carbon (LC), cleaning, the low-temperature molten salt clean metallurgical novel process of antimony efficiently.
Summary of the invention
The object of the invention is to provide a kind of clean metallurgical method for low-temperature molten salt of antimony; Significantly reduce the antimony smelting temperature; One step output needle antimony; And realize recovery and the sulfide energy utilization of sulphur, in the simplification flow process, reduce cost, significantly improve the antimony direct yield in, thoroughly eliminate low concentration SO in traditional antimony pyrometallurgical smelting flow process
2Flue gas is to the pollution of ecotope.
For realizing above-mentioned target; The present invention adopts the oxide compound of a kind of and the sulphur avidity metal more much bigger than antimony to make sulphur-fixing agent, and fine coal or coke powder are reductive agent, and itself and antimony concentrate are reduced solid sulphur melting in low temperature inertia fused salt; One step refining needle antimony and the solid sulfur metal sulfide of output; The latter and unreacted reactant form the fused salt slag as solids, and most of inertia fused salt separates the hot Returning smelting process in back with solids, and the fused salt slag is then through " water logging-carbonating deposition " process regeneration NaHCO
3Reuse, leached mud reclaims solid sulfur metal sulfide concentrate through ore dressing and sells, or its desulfurization with roasting technique is carried out heat energy utilization and flue gas acid preparing, and the oxide compound calcining then returns antimony melting operation and makes sulphur-fixing agent, and the processing condition of correlated process are:
(1) the solid sulphur fusion process of reduction: 1. temperature is 800～950 ℃; 2. time 1～5h; 3. secondary zinc oxide or zinc-oxide calcine, cupric oxide material or cupric oxide calcining are as sulphur-fixing agent, and its quality consumption is 1～1.5 times of theoretical value; 4. the inertia fused salt is the fused salt mixt of yellow soda ash fused salt or yellow soda ash and small amounts of sodium hydroxide; The sodium hydroxide mass content is less than 10% in the fused salt mixt; Inertia fused salt quality consumption is 2～6 times of solids amount, and wherein solids comprises solid sulfur metal sulfide and unreacted reactant; 5. reductive agent such as fine coal or coke powder quality consumption is 4～10% of an antimony concentrate amount;
(2) leave standstill fining process and separate inertia fused salt process: 1. temperature is 800～950 ℃; 2. time 0.5～5h; 3. the slow hectare clarification of falling top fused salt;
(3) solids fused salt pulp water soaks process: 1. temperature is 50～100 ℃; 2. time 0.5～6h; 3. liquid-solid volume mass is than being (1～8): 1, and hot wash leached mud 3～5 times, wash water endpoint pH 7～8;
(4) infusion deposition regeneration sodium hydrogencarbonate process: 1. temperature is 10～95 ℃; 2. time 0.5～10h; 3. CO
2Volumetric usage is 1.05～2 times of theoretical amount; 4. reaction end pH value 3～8.
Adopt the antimony clean metallurgical method for low-temperature molten salt of technique scheme, its ultimate principle is:
In the low temperature inertia fused salt that with yellow soda ash is main body, the Sb in the antimony concentrate
2S
3, the reduction desulfurization reaction takes place in PbS and ZnO or CuO under 650～950 ℃ of temperature and reducing atmosphere:
2Sb
2S
3+6ZnO+3C＝4Sb+6ZnS+3CO
2 (1)
2Sb
2S
3+6CuO+3C＝4Sb+6CuS+3CO
2 (2)
2PbS+2ZnO+C＝2Pb+2ZnS+CO
2 (3)
2PbS+2CuO+C＝2Pb+2CuS+CO
2 (4)
Weisspiessglanz in the antimony concentrate then carries out reduction reaction:
2Sb
2O
3+3C＝4Sb+3CO
2 (5)
Sb
2O
4+2C＝2Sb+2CO
2 (6)
2Sb
2O
5+5C＝4Sb+5CO
2 (7)
The melting initial stage, the sodium hydrogencarbonate generation decomposition reaction that regeneration is returned:
2NaHCO
3＝Na
2CO
3+H
2O+CO
2 (8)
In the immersion liquid of solids fused salt pulp water, feed CO
2The reaction of gas precipitation regeneration sodium hydrogencarbonate is following:
NaOH+CO
2＝NaHCO
3 (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, its ZnS that generates with melting, CuS form the fused salt slag 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; Significantly reduce the antimony smelting temperature, a step is produced needle antimony, and realizes the recovery of sulphur and the energy utilization of sulfide; When simplifying flow process, reducing cost, significantly improve the antimony direct yield, thoroughly eliminate low concentration SO in traditional antimony pyrometallurgical smelting process
2Flue gas is to the pollution of ecotope, has low-carbon (LC), cleaning, advantage such as efficient, and technical progress and the energy-saving and emission-reduction that promote China's antimony metallurgy industry are significant.
Description of drawings
Fig. 1 is the low-temperature molten salt clean metallurgical technological principle schematic flow sheet of antimony.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described further.
Embodiment 1
Referring to Fig. 1, the chemical constitution of stibnite concentrate is (%): Sb 63.91, Fe 0.94, S 24.91, Cu 0.43, Pb 0.43, Cd 0.0038, As 0.10, SiO
25.28, Al
2O
32.38, CaO 1.21, MgO 1.95, 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 stibnite concentrate, 9.48g fine coal, 297.02g technical grade yellow soda ash respectively and contain the secondary zinc oxide 64.4g uniform mixing of Zn 78.33%, compound is packed into behind the plumbago crucible, again at its surface coverage 74.26g technical grade yellow soda ash.Plumbago crucible is pushed in the resistance furnace, and at 900 ℃ of following melting 2h, output contains the needle antimony 63.6g of Sb 99.02%, and the direct yield of antimony reaches 98.54%; Under 900 ℃, leave standstill clarification and separate inertia fused salt and solids; The slow hectare clarification of falling top fused salt behind the 1h; Obtain the solids slag 155.93g of fusion yellow soda ash 301.5g and bonding small portion yellow soda ash; The latter adopts the 300mL tap water to leach 3h, hot wash leached mud 5 times, wash water endpoint pH 8 down at 85 ℃; The dried leached mud 85.39g of gained contains Zn 59.98%, S 29.12%, the nearly a hundred per cent of sulfur-fixing rate; Filtrate volume is 340mL, contains Na
2CO
3205.2g/L, under 85 ℃, feed CO to it
2Gas, reaction times 8h, CO
2Volumetric usage is 1.05 times of theoretical amount, reaction end pH value 8, and eutectoid goes out NaHCO
392.10g, mother liquor volume 330mL, wherein NaHCO
3Content is 56g/L.
Embodiment 2:
The chemical constitution of stibnite concentrate is identical with embodiment 1, and coke powder (containing C 82%, ash content 10%) is made reductive agent.Take by weighing 100g stibnite concentrate, 8g coke respectively and contain the cupric oxide calcining 68.19g uniform mixing of Cu 49.03%, compound is packed into behind the plumbago crucible, adds the fusion yellow soda ash 301.5g that embodiment 1 returns, and covers the NaHCO that embodiment 1 returns again
392.1g with technical grade yellow soda ash 22g.Plumbago crucible is pushed in the resistance furnace, and at 870 ℃ of following melting 3h, output contains the needle antimony 64.25g of Sb 98.78%, and the direct yield of antimony reaches 99.31%; Under 800 ℃, leave standstill clarification and separate inertia fused salt and solids, the slow hectare clarification of falling top fused salt behind the 5h, the solids slag 175.43g of acquisition fusion yellow soda ash 296.5g and bonding small portion yellow soda ash; The latter adopts the 400mL tap water to leach 2h down at 90 ℃; Hot wash leached mud 3 times, wash water endpoint pH 7 must be done leached mud 105.25g; Contain Cu 32.16%, S 16.19%, the nearly a hundred per cent of sulfur-fixing rate; Filtrate volume is 460mL, contains Na
2CO
3185g/L feeds CO to it under 90 ℃
2Gas, reaction times 5h, CO
2Volumetric usage is 2 times of theoretical amount, reaction end pH value 7, and eutectoid goes out NaHCO
3109.63g, mother liquor volume 450mL, NaHCO
3Content is 56.1g/L.
Embodiment 3:
With the jamesonite is raw material, and its chemical ingredients is (%): Sb 26.36, Pb 31.33, Zn 3.92, Fe 8.69, Cu 0.12, S 22.10, As 0.58, SiO
21.56, CaO 1.44, Al
2O
30.34 coal dust is a reductive agent, its chemical ingredients is identical with embodiment 1, and zinc-oxide calcine is a sulphur-fixing agent, and its chemical ingredients is (%): Zn 52.87, Cu 3.58, Pb 0.35, Sb 0.68.Take by weighing 100g jamesonite concentrate, 80.63g zinc-oxide calcine, 10g coal dust and 306g technical grade sodium hydrogencarbonate and 25.66g technical grade sodium hydroxide respectively; The plumbago crucible of packing into behind the uniform mixing; Then in resistance furnace in 820 ℃ of following melting 4h; Output magnolium 56.87g contains Sb46.58%, Pb 51.42%, and antimony, plumbous direct yield are respectively 98.45% and 92.50%; Under 850 ℃, leave standstill clarification and separate fused salt and solids; The slow hectare clarification of falling top fused salt behind the 3h; Obtain the solids slag 145.1g of fusion yellow soda ash 286.25g and bonding small portion yellow soda ash; The latter adopts the 300mL tap water to leach 3h, hot wash leached mud 4 times, wash water endpoint pH 7.5 down at 80 ℃; Solid carbon dioxide soaks the heavy 91.35g of slag, contains Zn 50.96%, Cu 3.44%, S 24.52%, the nearly a hundred per cent of sulfur-fixing rate; Filtrate volume is 360mL, contains Na
2CO
3153.6g/L, under 80 ℃, feed CO to it
2Gas, reaction times 3h, CO
2Volumetric usage is 2 times of theoretical amount, reaction end pH value 6, and eutectoid goes out NaHCO
368.43g, mother liquor volume 340mL, NaHCO
3Content is 56.5g/L.
Embodiment 4:
With the jamesonite is raw material, and its chemical ingredients is identical with embodiment 3, and coal dust is a reductive agent, and its chemical ingredients is identical with embodiment 1.Take by weighing 100g stibnite concentrate, 10g fine coal, 218.36g technical grade yellow soda ash respectively and contain the cupric oxide material 101.18g uniform mixing of Cu 35.68%, compound is packed into behind the plumbago crucible, again at its surface coverage 54.59g technical grade yellow soda ash.Plumbago crucible is pushed in the resistance furnace, and at 950 ℃ of following melting 1.5h, output magnolium 56.65g contains Sb 45.86%, Pb 52.72%, and antimony, plumbous direct yield are respectively 98.56% and 95.33%; Under 950 ℃, leave standstill clarification and separate inertia fused salt and solids; The slow hectare clarification of falling top fused salt behind the 2h; Obtain the solids slag 117.37g of fusion yellow soda ash 232.01g and bonding small portion yellow soda ash; The latter adopts the 300mL tap water to leach 1h, hot wash leached mud 5 times, wash water endpoint pH 7 down at 100 ℃; The dried leached mud 76.43g of gained contains Cu 46.99%, Zn 5.10%, S 28.91%, the nearly a hundred per cent of sulfur-fixing rate; Filtrate volume is 370mL, contains Na
2CO
3109.55g/L, under 95 ℃, feed CO to it
2Gas, reaction times 1h, CO
2Volumetric usage is 1.05 times of theoretical amount, reaction end pH value 8, and eutectoid goes out NaHCO
361.68g, mother liquor volume 350mL, wherein NaHCO
3Content is 36.72g/L.
Claims (2)
1. the clean metallurgical method for low-temperature molten salt of an antimony; Adopt and a kind ofly make sulphur-fixing agent with the sulphur avidity MOX more much bigger than antimony, fine coal or coke powder are reductive agent, and itself and antimony concentrate are reduced solid sulphur melting in low temperature inertia fused salt; One step refining needle antimony and the solid sulfur metal sulfide of output; The latter and unreacted reactant form the fused salt slag as solids, and most of inertia fused salt separates the hot Returning smelting process in back with solids, and the fused salt slag is then through the reuse of " water logging-carbonating deposition " process regeneration sodium hydrogencarbonate; Leached mud reclaims solid sulfur metal sulfide concentrate through ore dressing and sells; Or its desulfurization with roasting technique carried out heat energy utilization and flue gas acid preparing, oxide compound calcining then Returning smelting is made sulphur-fixing agent, it is characterized in that:
A, the solid sulphur melting condition of reduction are: 1. temperature is 800～950 ℃; 2. time 1～5h; 3. admittedly sulfur metal oxide mass consumption is 1～1.5 times of theoretical amount, is secondary zinc oxide, zinc-oxide calcine, cupric oxide material or cupric oxide calcining as the MOX of sulphur-fixing agent; 4. inertia fused salt quality consumption is 2～6 times of solids amount; Solids then comprises solid sulfur metal sulfide and unreacted reactant; Described inertia fused salt is the fused salt mixt of yellow soda ash fused salt or yellow soda ash and small amounts of sodium hydroxide, and the sodium hydroxide mass content is less than 10% in the described fused salt mixt; 5. fine coal or coke powder reductive agent quality consumption are 4～10% of antimony concentrate amount;
B, employing fining process separating most inertia fused salt and solids, actual conditions is: 1. temperature is 800～950 ℃; 2. time 0.5～5h; 3. slowly topple over top clarification fused salt;
C, solids fused salt pulp water soak process condition and be: 1. temperature is 50～100 ℃; 2. time 0.5～6h; 3. liquid-solid volume mass ratio is 1～8: 1, hot wash leached mud 3～5 times, wash water endpoint pH 7～8.
2. the clean metallurgical method for low-temperature molten salt of antimony according to claim 1 is characterized in that: the processing condition of described " water logging-carbonating deposition " process regeneration sodium hydrogencarbonate are: 1. temperature is 10～95 ℃; 2. time 0.5～10h; 3. CO
2Volumetric usage is 1.05～2 times of theoretical amount; 4. reaction end pH value 3～8.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102102154A (en) * | 2010-12-22 | 2011-06-22 | 中南大学 | Low-temperature fused salt clean smelting method for tin |
| CN102534255B (en) * | 2011-12-30 | 2014-01-29 | 中南大学 | Wet-fire combined smelting process for antimony or bismuth |
| CN104975166B (en) * | 2015-06-30 | 2017-11-10 | 中南大学 | A kind of method that sulfide thing mutually reduces conversion beneficiating method processing stibnite concentrate |
| CN105695742B (en) * | 2016-02-24 | 2017-11-10 | 锡矿山闪星锑业有限责任公司 | A kind of smelting process of antimony oxygen low-temperature reduction antimony |
| CN108103315A (en) * | 2017-12-05 | 2018-06-01 | 广西生富锑业科技股份有限公司 | A kind of method that zinc is recycled in the caustic fusion slag from jamesonite |
| CN108425023A (en) * | 2017-12-26 | 2018-08-21 | 中国恩菲工程技术有限公司 | The extraction system of antimony metal |
| CN108118158B (en) * | 2018-02-01 | 2020-04-21 | 长沙有色冶金设计研究院有限公司 | Method for extracting valuable metals from sulfide slag and blast furnace gas ash |
| CN111172563B (en) * | 2020-02-25 | 2020-12-29 | 中南大学 | Method and device for electrolyzing antimony sulfide-containing material by using molten salt |
| CN115821064A (en) * | 2022-12-02 | 2023-03-21 | 昆明理工大学 | Low-temperature reduction method for antimony oxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3944653A (en) * | 1972-08-30 | 1976-03-16 | Occidental Petroleum Corporation | Process for preparing high purity antimony trichloride and antimony oxide from stibnite ores |
| CN101376929A (en) * | 2008-09-27 | 2009-03-04 | 中南大学 | Method for extracting bismuth from bismuth ore concentrate or material containing bismuth |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4333762A (en) * | 1980-03-20 | 1982-06-08 | Asarco Incorporated | Low temperature, non-SO2 polluting, kettle process for the separation of antimony values from material containing sulfo-antimony compounds of copper |
-
2010
- 2010-09-01 CN CN2010102690427A patent/CN101914693B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3944653A (en) * | 1972-08-30 | 1976-03-16 | Occidental Petroleum Corporation | Process for preparing high purity antimony trichloride and antimony oxide from stibnite ores |
| CN101376929A (en) * | 2008-09-27 | 2009-03-04 | 中南大学 | Method for extracting bismuth from bismuth ore concentrate or material containing bismuth |
Non-Patent Citations (2)
| Title |
|---|
| JP昭56-139638A 1981.10.31 |
| 陈永明等.硫化锑精矿还原造硫熔炼一步炼锑.《中国有色金属学报》.2005,第15卷(第8期),第1311-1316页. * |
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