CN102102154A - Low-temperature fused salt clean smelting method for tin - Google Patents
Low-temperature fused salt clean smelting method for tin Download PDFInfo
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- CN102102154A CN102102154A CN 201010600469 CN201010600469A CN102102154A CN 102102154 A CN102102154 A CN 102102154A CN 201010600469 CN201010600469 CN 201010600469 CN 201010600469 A CN201010600469 A CN 201010600469A CN 102102154 A CN102102154 A CN 102102154A
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Abstract
一种锡的低温熔盐清洁冶金方法，将锡精矿或含锡物料于钠熔盐中进行低温还原熔炼，一步炼制粗锡。熔炼产物还包括未反应固态物，如脉石成分以及生成的固态产物。反应结束后，大部分惰性熔盐与固态物分离后以热态返回熔炼过程，被固态物粘结的少部分惰性熔盐经湿法处理再生回用。浸除熔盐后的固态物则可进一步处理回收有价金属。本发明大幅降低锡冶炼温度，一步产出粗锡，解决了锡-铁分离难题，流程简短、成本降低、锡直收率大幅提高，是一种低碳、清洁、高效的锡冶炼新方法。The invention relates to a low-temperature molten salt clean metallurgical method for tin. The tin concentrate or tin-containing material is subjected to low-temperature reduction smelting in sodium molten salt to refine crude tin in one step. Smelting products also include unreacted solids, such as gangue components, and resulting solid products. After the reaction, most of the inert molten salt is separated from the solid matter and returns to the smelting process in a hot state, and a small part of the inert molten salt bonded by the solid matter is regenerated and reused by wet treatment. The solid matter after leaching molten salt can be further processed to recover valuable metals. The invention greatly reduces the tin smelting temperature, produces crude tin in one step, solves the problem of tin-iron separation, has a simple process, reduces costs, and greatly improves the direct yield of tin. It is a new low-carbon, clean and efficient tin smelting method.
Description
[technical field]
The present invention relates to a kind of clean metallurgical method for low-temperature molten salt of tin, belong to the Non-ferrous Metallurgy field.
[background technology]
The tin concentrate can be divided into three types by tin grade height: higher-grade concentrate (Sn＞60%); Medium tin ore (Sn:30～60%); Low-grade concentrate (Sn＜30%).Existing tin smelting process is divided pyrogenic process and wet method; The wet method tin-making process comprises that SnO2 is reduced to metallic tin-acidleach-electrodeposition method, SnO2 and is reduced to metallic tin-acidleach-aluminium bits substitution method, SnO2 and is reduced to SnO and is stabilized in the vitreum-acidleach-electrodeposition method and sodium sulphite+sodium hydroxide solution high pressure leaching-electrodeposition method etc., above-mentioned wet method tin-making process exists all that investment is big, cost is high, especially produce a large amount of waste residues and waste water, shortcomings such as harm environment.At present do not see that the wet method tin-making process has the report of large-scale production.Existing tin is smelted the main pyrogenic process tin-making process that adopts, and according to the height of tin concentrate stanniferous grade, adopt three kinds of smelting technologyes respectively: (1) handles the low higher-grade tin concentrate of iron content, with traditional " two sections smelting processes "; (2) handle that iron content is higher, the tin concentrate of the medium grade of stanniferous, with " retailoring-sulfiding volatilization method "; (3) handle low-grade medium tin ore, with " sulfiding volatilization-reducing smelting process ".
There is two large problems in the pyrometallurgical smelting process of tin:
(1) the smelting temperature height, energy consumption is big, environmental pollution is serious.From thermodynamics, reduction SnO
2Not difficult, under 800～1000 ℃ temperature, CO content is 20% o'clock in the balance gas phase, SnO
2Promptly be reduced into metallic tin, iron is still with Fe
3O
4Or FeO exists.But in order to make melting slag, actual tin metallurgy temperature is 1150～1400 ℃.For keeping high temperature like this, must consume a large amount of fat coals or heavy oil; Under this high temperature, all be reduced with Cu, Pb, Bi, As, Sb and the Ag etc. of tin association and enter thick tin, As and Pb be volatilization in a large number also, causes the severe contamination at plant area's ambient air, soil and water source.
(2) tin iron separation difficulty, long flow path, production cost height.Because the oxide compound of tin and iron and the thermodynamic property of their silicate are approaching, iron and tin easily form alloy, enter thick tin and hardhead so a large amount of iron and tin reduce together, and SnO causes slag stanniferous height also in a large number with the FeO slag making, tin-iron separation difficulty.Especially in recent years along with head grade reduces year by year, the iron level in the tin ore is more and more higher, and at present, the circulation of iron in the tin smelting process become the heavy burden of two sections sn smelting methods.
[summary of the invention]
The object of the present invention is to provide a kind of low-carbon (LC), cleaning, tin metallurgy method efficiently---low-temperature molten salt cleaning tin metallurgical method.This method significantly reduces the tin smelting temperature, avoids the pollution of heavy metal to environment; One step was produced thick tin, significantly improved tin and smelted direct yield, thoroughly solved tin-iron and separated a difficult problem, simplified the tin metallurgy flow process, reduced production costs.
Technical scheme of the present invention is: tin concentrate or stanniferous material under 700～950 ℃ temperature, are carried out retailoring in the inertia fused salt, step refining obtains thick tin; Adopt fine coal or coke powder to make reductive agent in the retailoring process; Fused salt after melting finishes through with after the solids slag separates with hot form Returning smelting process.
Described inertia fused salt is the combination of one or both or three in yellow soda ash, sodium-chlor, the sodium hydroxide, and sodium hydrate content is 1%～10% in the combination fused salt.
Inertia fused salt consumption is tin concentrate or stanniferous weight of material 1～6 times, and fine coal or coke powder consumption are 5～20% of tin concentrate or stanniferous weight of material.
For the tin concentrate or the stanniferous material of sulfur-bearing, the oxide compound of the avidity of the sulphur metal stronger than tin is made sulphur-fixing agent by adding.The consumption of sulphur-fixing agent is 0.8～1.5 times with the theoretical molar amount of the tin concentrate of sulfur-bearing or the reaction of the metallic sulfide in the stanniferous material.
After melting finishes, adopt clarification or filtering mode to separate the inertia fused salt.
Described clarification separates the inertia fused salt and is meant 700～950 ℃ of temperature, and top clarification fused salt slowly comes down in torrents; Described filtering separation inertia fused salt is meant 700～950 ℃ of temperature, filters fused salt with-200 purpose stainless (steel) wires.
Going back the agglutinating fused salt on the solids slag needs through the wet processing regeneration, soaks except that the solids behind the fused salt and further handles the recovery valuable element.
The fused salt that also is bonded with on the described solids slag then need pass through wet processing, and the solids slag that is about to be bonded with fused salt is in 10～100 ℃ of following water loggings of temperature, and infusion solid volume mass ratio is 1～8: 1, obtains leached mud and leach liquor; Water washing leached mud 3～5 times to pH=7～8, thereby obtains soaking solids except that behind the fused salt.Leach liquor then can also can be back to melting place by continuing to be settled out sodium bicarbonate, and its deposition condition is: temperature 10-95 ℃, the CO2 volumetric usage is 1.05-2 a times of theoretical amount, and reaction end pH value is 3～8.
Method of the present invention is carried out retailoring with tin concentrate or stanniferous material in low temperature inertia fused salt, the thick tin of step refining.In the fusion process, as flux, fine coal or coke powder are made reductive agent, if tin concentrate or stanniferous material sulfur-bearing are then used the oxide compound of the avidity of the sulphur metal stronger than tin is made sulphur-fixing agent with the lower sodium salt of one or more fusing points.After melting finished, most of fused salt separated the back with hot Returning smelting process with solids,, was soaked except that the solids behind the fused salt and further handled the recovery valuable element through the wet processing regeneration by solids agglutinating small part fused salt.
Details are as follows for technological process principle of the present invention and technical qualification:
1. technological process principle
The essence of low-temperature molten salt tin metallurgy be melt with a kind of in yellow soda ash, sodium-chlor, the sodium hydroxide or wherein two kinds or three's combination as the melting system, under 700～950 ℃ temperature, melt itself does not participate in reaction, gangue content SiO
2, Al
2O
3, CaCO
3, MgCO
3, Fe
xO
y, CuS do not melt not slag making.Simple substance tin fusing in the melt, tin-oxide then is reduced into metallic tin:
SnO
2(s)+CO＝SnO(s)+CO
2
SnO(s)+CO＝Sn(L)+CO
2
C(s)+CO
2＝2CO
Except zinc, the associated metal oxide compound also is reduced into corresponding metal, and the high price ferric oxide is reduced to iron protoxide:
MeO(s)+CO＝Me(L)+CO
2
Me
2O
3(s)+3CO＝2Me(L)+3CO
2
Fe
2O
3(s)+CO＝2FeO(s)+CO
2
If tin metallurgy raw material sulfur-bearing then produces solid sulphur reduction reaction:
MeS(s)+ZnO(s)+CO＝Me(L)+ZnS(s)+CO
2
MeS(s)+CuO(s)+CO＝Me(L)+CuS(s)+CO
2
Me
2S
3(s)+3ZnO(s)+3CO＝2Me(L)+3ZnS(s)+3CO
2
Me
2S
3(s)+3CuO(s)+3CO＝2Me(L)+3CuS(s)+3CO
2
2. the technical qualification of relevant process
(1) low-temperature reduction fusion process: 1. temperature is 700～950 ℃, 2. time 1～5h, 3. inertia fused salt consumption is tin concentrate or stanniferous weight of material 1～6 times, and 4. fine coal or coke powder consumption are 5～20% of tin concentrate or stanniferous weight of material, and the consumption of sulphur-fixing agent is 0.8～1.5 times of theoretical amount.
(2) separate fused salt and solids slag process: adopt clarification or filtering method separating most inertia fused salt, actual conditions is: 1. temperature is 700～950 ℃, 2. time 0.5～5h, top clarification fused salt or with-200 purpose stainless (steel) wires filtration fused salt 3. slowly comes down in torrents.
(3) the solids pulp water that is bonded with fused salt soaks and obtains leached mud and leach liquor:: the water logging condition is: 1. temperature is 10～100 ℃, 2. time 0.5～6h, 3. liquid-solid volume mass ratio is 1～8: 1, water washing leached mud 3～5 times is to pH=7～8.
(4) leach liquor precipitate sodium bicarbonate condition: 1. temperature 10-95 ℃, 2. the time is 0.5-10h, 3. CO
2Volumetric usage is 1.05-2 a times of theoretical amount, and 4. reaction end pH value is 3～8.
In sum, the present invention is by a low-temperature molten salt metallurgical method that relates to the gas, liquid, solid three-phase equilibrium, and this method significantly reduces the tin smelting temperature, has greatly alleviated the pollution of harmful heavy metal to surrounding enviroment; One step was produced thick tin, significantly improved tin and smelted direct yield, thoroughly solved tin-iron and separated a difficult problem, simplified the tin metallurgy flow process, reduced production costs.Method of the present invention has low-carbon (LC), cleaning, advantage such as efficient, applicable to high, medium and low three types tin essence, technical progress and the energy-saving and emission-reduction that promote China's tin smelter industry is significant.
[description of drawings]
Fig. 1 is a process flow diagram of the present invention.
[embodiment]
Following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1
The chemical constitution of tin concentrate A is (%): Sn 69.1%, and As 0.01%, and S 0.34%, and Fe 1.12%, Cu0.07%, and Pb 0.035%, SiO
22.17%.Take by weighing 100g tin concentrate, 32g fine coal, 310g technical grade yellow soda ash and 10g technical grade caustic soda uniform mixing respectively, the compound plumbago crucible of packing into.Plumbago crucible is pushed in the resistance furnace, at 850 ℃ of following melting 2.5h, the thick tin 68.4g of output stanniferous 98.86%, the direct yield of tin reaches 99.0%; Obtain the solids slag 35.6g of fusion sodium salt 287g and bonding small portion sodium salt behind the hot fused salt clarification separate solid thing, leach under the condition of 75 ℃ of temperature, time 3h with the 200mL tap water, must do leached mud 19.7g, filtrate and washing lotion volume are 220mL, at room temperature feed CO
2, eutectoid goes out NaHCO
318.6g.
Embodiment 2
The chemical constitution of tin concentrate B is (%): Sn 41.0%, and As 1.6%, and S 1.3%, and Fe 22.3%, and Cu 0.13%, and Pb 4.5%, Bi0.11%, and CaO 0.30%, SiO
24.12%.Take by weighing 100g tin concentrate B, 26g fine coal, 3.6g zinc oxide respectively, 300g technical grade sodium-chlor and 15g technical grade caustic soda uniform mixing, the compound plumbago crucible of packing into.Plumbago crucible is pushed in the resistance furnace, at 900 ℃ of following melting 2h, the thick tin 44.5g of output stanniferous 90%, the direct yield of tin reaches 98.0%; Obtain the solids slag 80g of fusion sodium salt 280g and bonding small portion sodium salt behind the hot fused salt clarification separate solid thing, leach under the condition of 80 ℃ of temperature, time 3h with the 400mL tap water, must do leached mud 47.5g, filtrate and washing lotion volume are 620mL, at room temperature feed CO
2, eutectoid goes out NaHCO
328.2g.
Embodiment 3
With a kind of hydroxide scruff of handling the tin anode mud output is raw material, and tin content is 60%, also contains a spot of lead, antimony and sodium-chlor in addition; Make reductive agent with the coke powder that contains C 82%, ash content 10%.Take by weighing 1000g scruff, 250g coke powder and 1000g industrial sodium carbonate uniform mixing respectively, compound is packed into behind the plumbago crucible, and the fusion yellow soda ash 694g that embodiment 1 and embodiment 2 are returned and the NaHCO3 of recovery 40g altogether cover the material surface.Then plumbago crucible is pushed in the resistance furnace, at 800 ℃ of following melting 3h, output contains the thick tin 612.4g of Sn 96.5%, and the direct yield of tin reaches 98.5%; Hot fused salt obtains the solids slag 212g of fusion sodium salt 1510.6g and bonding small portion sodium salt after-200 purpose stainless (steel) wire filtering separation solids, leach under the condition of 80 ℃ of temperature, time 2.5h with the 1000mL tap water, must do leached mud 102.5g; Filter gained filtrate and at room temperature feed CO
2, eutectoid goes out NaHCO
378.6g.
Claims (11)
1. the clean metallurgical method for low-temperature molten salt of a tin is characterized in that, tin concentrate or stanniferous material under 700～950 ℃ temperature, are carried out retailoring in the inertia fused salt, and step refining obtains thick tin; Adopt fine coal or coke powder to make reductive agent in the retailoring process; Fused salt after melting finishes through with after the solids slag separates with hot form Returning smelting process.
2. method according to claim 1 is characterized in that, described inertia fused salt is the combination of one or both or three in yellow soda ash, sodium-chlor, the sodium hydroxide, and sodium hydrate content is 1%～10% in the combination fused salt.
3. method according to claim 1 and 2 is characterized in that, for the tin concentrate or the stanniferous material of sulfur-bearing, by adding the oxide compound of the avidity of the sulphur metal stronger than tin is made sulphur-fixing agent.
4. method according to claim 3 is characterized in that, the consumption of sulphur-fixing agent is 0.8～1.5 times with the tin concentrate of sulfur-bearing or the metallic sulfide reaction theory molar weight in the stanniferous material.
5. according to claim 1 or 2 each described methods, it is characterized in that inertia fused salt consumption is tin concentrate or stanniferous weight of material 1～6 times, fine coal or coke powder consumption are 5～20% of tin concentrate or stanniferous weight of material.
6. claim 1 or 2 described methods is characterized in that: after melting finishes, adopt clarification or filtering mode to separate the inertia fused salt.
7. method according to claim 6 is characterized in that: described clarification separates the inertia fused salt and is meant 700～950 ℃ of temperature, and top clarification fused salt slowly comes down in torrents; Described filtering separation inertia fused salt is meant 700～950 ℃ of temperature, filters fused salt with-200 purpose stainless (steel) wires.
8. method according to claim 1 and 2 is characterized in that, goes back the agglutinating fused salt on the solids slag, needs through the wet processing regeneration, soaks except that the solids behind the fused salt and further handles the recovery valuable element.
9. the clean metallurgical method for low-temperature molten salt of described a kind of tin according to Claim 8, it is characterized in that, described solids slag agglutinating fused salt is to be bonded with the solids slag of fused salt in 10～100 ℃ of following water loggings of temperature through wet processing, infusion solid volume mass ratio is 1～8: 1, obtains leached mud and leach liquor; Water washing leached mud 3～5 times to pH=7～8, thereby obtains soaking solids except that behind the fused salt.
10. method according to claim 9 is characterized in that: leach liquor continues precipitate sodium bicarbonate, and its deposition condition is: temperature 10-95 ℃, and CO
2Volumetric usage is 1.05-2 a times of theoretical amount, and reaction end pH value is 3～8.
11. method according to claim 1 is characterized in that, described stanniferous material is the secondary raw material of tin, comprises tin anode mud, tin flue dust, tin refining slag, useless scolding tin or useless tin alloy.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776386A (en) * | 2012-07-20 | 2012-11-14 | 北京科技大学 | Method for recycling stannic oxide from tin-containing lead slag |
| CN104152717A (en) * | 2014-07-21 | 2014-11-19 | 中南大学 | Composite additive applied to metallic tin preparation process by reducing roasting of cassiterite ore concentrate, and method for preparing metallic tin |
| CN107034365A (en) * | 2017-06-08 | 2017-08-11 | 安徽省金鸿再生资源科技有限公司 | A kind of method of thick tin pyro-refining |
| CN110453080A (en) * | 2019-09-11 | 2019-11-15 | 广东先导稀材股份有限公司 | Method for recovering tin from sponge tin |
| CN111172409A (en) * | 2020-01-19 | 2020-05-19 | 河南豫光金铅股份有限公司 | Recovery smelting process of tin-containing material |
| CN111485117A (en) * | 2020-05-28 | 2020-08-04 | 中南大学 | A kind of method for reducing high lead slag with hydrogen |
| CN114833490A (en) * | 2022-06-02 | 2022-08-02 | 云南锡业集团（控股）有限责任公司研发中心 | Method for improving oxidation resistance of tin raw material or tin-based solder |
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| CN111485117A (en) * | 2020-05-28 | 2020-08-04 | 中南大学 | A kind of method for reducing high lead slag with hydrogen |
| CN114833490A (en) * | 2022-06-02 | 2022-08-02 | 云南锡业集团（控股）有限责任公司研发中心 | Method for improving oxidation resistance of tin raw material or tin-based solder |
| CN114833490B (en) * | 2022-06-02 | 2024-04-05 | 云南锡业集团（控股）有限责任公司研发中心 | Method for improving oxidation resistance of tin raw material or tin-based solder |
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Application publication date: 20110622 |