CN105734270A - Additive for reinforcing reduction roasting of tin-containing materials to recover tin and method for separating and recovering tin from tin-containing materials - Google Patents
Additive for reinforcing reduction roasting of tin-containing materials to recover tin and method for separating and recovering tin from tin-containing materials Download PDFInfo
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- CN105734270A CN105734270A CN201610143175.7A CN201610143175A CN105734270A CN 105734270 A CN105734270 A CN 105734270A CN 201610143175 A CN201610143175 A CN 201610143175A CN 105734270 A CN105734270 A CN 105734270A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B25/00—Obtaining tin
- C22B25/02—Obtaining tin by dry processes
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses an additive for reinforcing reduction roasting of tin-containing materials to recover tin and a method for separating and recovering the tin from the tin-containing materials. The additive comprises main components such as fluorite, borax, sodium humate and the like. The method for applying the additive to reinforcement of reduction roasting of the tin-containing materials to recover the tin comprises steps as follows: the tin-containing materials are ground, crushed and then mixed with the additive for agglomeration; obtained agglomerates are dried and then placed in a reducing atmosphere for high-temperature roasting, and volatile tin fluorides are recovered. According to the method, through use of the additive, the reduction roasting temperature can be effectively reduced, the separation and recovery rate of the tin can be increased, and the method is applicable to treatment of various tin-containing materials difficult to treat, is particularly applicable to treatment of tin-containing tailings, iron-tin ores, tin smelting slag and the like which have iron-tin minerals closely disseminated and associated and are difficult to separate through conventional mineral separation means, is simple in technology and low in cost, and meets industrial production.
Description
Technical field
The present invention relates to a kind of additive for strengthening stanniferous material reduction roasting separation and recovery stannum and the method separating and recovering stannum from stanniferous material, belong to tin mineral processing technique field,
Background technology
China's Tin Resources rich reserves, but mostly be and bury lode tin mineral deposit deep, that distribution is overlapping, thus mining and the difficulty sorted and cost are high.The domestic tin ore deposit more than 90% is based on lode tin ore deposit, and association, symbiotic fungi kind complexity, and comprehensive utilization difficulty is big.Along with the alluvial tin resource exhaustion that domestic high-quality is easily selected, the payable grade of cassiterite declines year by year, and current domestic alluvial tin payable grade is reduced to 0.009%～0.03%, and the payable grade in lode tin ore deposit is about 0.2%.
Owing to cassiterite and gangue mineral disseminated grain size are thin, symbiosis/association situation is complicated, especially part stannum is present among the mineral lattices such as magnetic iron ore, brownmillerite garnet, hornblend, Actinolitum with lattice replacement form, adopt existing beneficiation combined method method (ore grinding-gravity treatment-magnetic separation-flotation) to part is difficult containing tin resource, be difficulty with the efficiently separating of stannum, reclaim.Current stannum is smelted and is generally required that Tin concentrate grade is not less than 35%, constantly throws tail in ore dressing process, and cassiterite comprehensive recovery is relatively low, and when with lode tin ore deposit for raw material, this problem is more prominent.
Iron mineral is the element that in the earth's crust, content is only second to oxygen, silicon, aluminum, and ferrum element character is active, and in almost all of nonferrous metallurgical process, the existence of ferrum all can have negative impact；Ore dressing and the smelting process of cassiterite are also had very disadvantageous effect by iron mineral.First, in ore dressing process, iron mineral can constantly dissociate Fe in the solution3+, form the Fe (OH) of lotus positive electricity2 +、Fe(OH)2+It is adsorbed on cassiterite surface, also can weaken the effect of medicament and cassiterite surface while consuming floating agent, cause the reduction of the tin-lead soldering response rate.And in stannum smelting process, the iron oxides content increase in Tin concentrate can consume the interpolation of reducing agent in smelting process, metallic tin and the extremely strong again affinity of metallic iron, cause the generation of stannum ferroalloy hardhead, cause a large amount of losses of stannum simultaneously；On the other hand in blast furnace iron-making process, stannum is a kind of harmful element, and the stannum in iron mine can be eventually entered into molten iron by synchronizing to be reduced into metallic tin, increases the fragility of steel, therefore generally requires that the Theil indices in iron-smelting furnace charge is lower than 0.08%.In summary, single ore-dressing technique, it is difficult to realizing the effective recycling to tin element, stannum ferrum inferior separating effect, is the main cause causing stanniferous comprehensive resource utilization rate low.
Fuming volatility process is the process that can efficiently separate from various stanniferous materials at present and reclaim stannum, mainly includes sulfiding volatilization, chloridizing volatilization and weak reduction volatilization method.Its cardinal principle is to utilize SnO, SnS and SnCl2Difference in vaporization at high temperature character, in a heated condition by the combined effect of reducing agent and additive, by the SnO in stanniferous material2It is reduced into SnO, SnS or SnCl2Volatilize in a gaseous form, then in dirt receipts system and carry out reclaim stannum.But, vulcanize and chloridizing volatilization technique sintering temperature high (requiring more than the high temperature of 1000 DEG C), and roasting process have harmful gas SO2Produce with HCl etc., cause seriously more serious secondary pollution and equipment corrosion.And the weak reduction volatilization a kind of method that to be separation efficiency high, cost recovery low, eco-friendly separates and recovers stannum from stanniferous material.But the technique of reduction roasting separation and recovery stannum still suffers from present, the problems such as sintering temperature height, roasting time length, therefore a kind of additive strengthening stanniferous material reduction roasting separation and recovery stannum and method are developed, to the comprehensive utilization realizing difficult stanniferous material, accelerate that extensive utilization the containing tin resource is had highly important realistic meaning.
Summary of the invention
For the defect that the technique of existing stanniferous material recycle stannum exists, it is an object of the invention to be in that provide one can strengthen stanniferous material reduction roasting, can effectively destroy the stone-like pulse in stanniferous material and tin mineral lattice etc., make stannum efficiently volatilize the additive reclaimed.
Another object of the present invention is to be in that to provide a kind of method adopting the compound additive such as calcium fluoride, Borax to reclaim stannum by weak reduction volatilization method high efficiency separation, and the method production cost simple to operate is low, environmental friendliness, meets industrialization production requirements.
In order to realize above-mentioned technical purpose, the invention provides a kind of additive reclaiming stannum for strengthening stanniferous material reduction roasting, this additive includes the component of following weight portion: 50 parts～60 parts of fluorite；Borax 20 parts～30 parts；Sodium humate 20 parts～30 parts.
The additive of the present invention mainly includes fluorite, Borax and sodium humate component.Fluorite and Borax component primarily serve the effect destroyed containing tin mineral and gangue mineral lattice in reduction process；And containing organic groups such as a large amount of-C=O ,-COOH ,-OH in sodium humate, roasting process produces CO and H2Isoreactivity gas, these active gasess are conducive to the activation of tin-oxide, have promoted that calcium fluoride and tin-oxide react, have formed SnF2And SnF4Two kinds of low melting points (respectively 215 DEG C and 705 DEG C), significantly improve the volatilization efficiency of stannum.By the combined effect of each component in additive, strengthen stanniferous material reduction roasting effect, be conducive to improving the response rate of stannum.Meanwhile, compound additive can significantly reduce the temperature of reduction roasting, reduces the effect of energy consumption.
Preferred scheme, the additive reclaiming stannum for strengthening stanniferous material reduction roasting is made up of the component of following weight portion:
53 parts～57 parts of fluorite；Borax 23 parts～27 parts；Sodium humate 22 parts～24 parts.
Present invention also offers a kind of described additive method for strengthening stanniferous material reduction roasting separation and recovery stannum, the method is after being ground by stanniferous material, with described additive mixing agglomeration；Gained agglomerate, through dried, is placed in reducing atmosphere, in 600 DEG C～850 DEG C roasting temperatures, reclaims the stannum fluoride of volatilization；Described reducing atmosphere is by CO and CO2Composition, the concentration of volume percent of CO is 10%～30%.
In technical scheme, the stanniferous material of employing mainly includes containing tailing, difficult tin-iron mine, stanniferous metallurgical slag etc., and stannum is mainly with micro fine particle (SnO2) embedding cloth in gangue mineral, also have part Sn4+Replacing form with lattice and be present in the mineral such as magnetic iron ore, andradite, this part tinbase does not originally have washability.And in the technical scheme of the present patent application, mainly through the compound additive that interpolation is made up of fluorite, Borax and sodium humate etc., fluorite and Borax can effectively destroy gangue mineral and tin mineral lattice, under reducing atmosphere simultaneously, as under carbon monoxide and hydrogen (comprising carbon monoxide and the hydrogen of release under sodium humate high temperature) isoreactivity gas catalysis, promote that calcium fluoride and stannum oxide react and generate volatile stannous fluoride and stannic fluoride etc., make stannum effectively be volatilized recovery.
Preferred scheme, in described additive, calcium fluoride is (5～15) with the mol ratio of stannum in stanniferous material: 1；More preferably mol ratio is (8～12): 1.
Preferred scheme, in reducing atmosphere, the concentration of volume percent of CO is 12%～18%.
Preferred scheme, sintering temperature is 750～850 DEG C.
More preferably scheme, roasting time is 15～120min；It most preferably is 35～65min.
Preferred scheme, stanniferous material is containing at least one in tailing, difficult tin-iron mine, stanniferous metallurgical slag.
Preferred scheme, stanniferous material and additive are all ground to the mass percentage content of-0.074mm grade more than 80%.
Preferred scheme, in stanniferous material, the volatility of stannum is more than 85%.
Hinge structure, the Advantageous Effects that technical scheme is brought:
(1) compound additive that technical scheme provides is in the reducing roasting process of stanniferous material, synergistic function between each component been significantly enhanced, can effectively destroy the gangue mineral in stanniferous material and tin mineral lattice, and stannum is changed into volatile stannum fluoride under high temperature, making stannum efficiently be volatilized recovery, the volatility of stannum reaches more than 85%.
(2) compound additive that technical scheme adopts can significantly reduce the temperature of stanniferous material reduction roasting, it is achieved energy-conservation, reduce the purpose of production cost.
(3) technical scheme is simple to operate, energy consumption is low, cost is low, it is easy to accomplish industrialized production.
(4) technical scheme is applicable to process all kinds of difficult stanniferous materials, is particularly well-suited to process the embedding cloth symbiosis of tin-iron mine thing tight, and conventional ore dressing means difficulty separate containing tailing, tin-iron mine and stannum metallurgical slag etc..
Detailed description of the invention
Below in conjunction with embodiment the present invention being further explained and illustrate, the protection domain of the claims in the present invention is not limited by the following examples.
Percentage composition described in following example and comparative example is mass percentage content.
Embodiment 1:
Being that-0.074mm accounts for the stanniferous milltailings (TSn0.40%) of 92% with addition of entering additive (additive is according to mass percent 50% fluorite, 30% Borax, 20% sodium humate mixing composition) by granularity, additive addition is according to CaF2The mol ratio of/Sn is 15:1, is joined by described additive in fine grinding material, carries out agglomeration, dried after mix homogeneously, is placed in weakly reducing atmosphere by dry agglomerate and carries out reduction roasting, sintering temperature 600 DEG C, and calcination atmosphere is CO/ (CO+CO2)=10%, roasting time 120min.The Theil indices analyzed in fired slags is 0.03%, and the volatility calculating stannum is 91.1%.
Embodiment 2:
Tin-iron mine (TSn0.71%) is accounted for 83% through broken, ore grinding to granularity-0.074mm ratio, by in fine grinding material with addition of enter additive (additive according to weight/mass percentage composition by 50% fluorite, 20% Borax, 30% sodium humate mixing form), additive addition is according to CaF2The mol ratio of/Sn is 11:1, is joined by described additive in fine grinding material, carries out agglomeration, dried after mix homogeneously, is placed in weakly reducing atmosphere by dry agglomerate and carries out reduction roasting, sintering temperature 725 DEG C, and calcination atmosphere is CO/ (CO+CO2)=30%, roasting time 15min.The Theil indices analyzed in fired slags is 0.08%, and the volatility calculating stannum is 90.2%.
Embodiment 3:
Tin-iron mine (TSn0.71%) is accounted for 83% through broken, ore grinding to granularity-0.074mm ratio, by in fine grinding material with addition of enter additive (additive according to weight/mass percentage composition 60% fluorite, 20% Borax, 20% sodium humate mixing composition), additive addition is according to CaF2The mol ratio of/Sn is 5:1, is joined by described additive in fine grinding material, carries out agglomeration, dried after mix homogeneously, is placed in weakly reducing atmosphere by dry agglomerate and carries out reduction roasting, sintering temperature 750 DEG C, and calcination atmosphere is CO/ (CO+CO2)=19%, roasting time 55min.The Theil indices analyzed in fired slags is 0.07%, and the volatility calculating stannum is 91.7%.
Embodiment 4:
Stannum metallurgical slag (TSn5.49%) is accounted for 97% through broken, ore grinding to granularity-0.074mm ratio, by in fine grinding material with addition of enter additive (additive according to weight/mass percentage composition 53% fluorite, 23% Borax, 24% sodium humate mixing composition), additive addition is according to CaF2The mol ratio of/Sn is 12:1, is joined by described additive in fine grinding material, carries out agglomeration, dried after mix homogeneously, is placed in weakly reducing atmosphere by dry agglomerate and carries out reduction roasting, sintering temperature 750 DEG C, and calcination atmosphere is CO/ (CO+CO2)=12%, roasting time 35min.The Theil indices analyzed in fired slags is 0.17%, and the volatility calculating stannum is 98.2%.
Embodiment 5:
Stannum metallurgical slag (TSn5.49%) is accounted for 97% through broken, ore grinding to granularity-0.074mm ratio, by in fine grinding material with addition of enter additive (additive according to weight/mass percentage composition 55% fluorite, 23% Borax, 22% sodium humate mixing composition), additive addition is according to CaF2The mol ratio of/Sn is 8:1, is joined by described additive in fine grinding material, carries out agglomeration, dried after mix homogeneously, is placed in weakly reducing atmosphere by dry agglomerate and carries out reduction roasting, sintering temperature 850 DEG C, and calcination atmosphere is CO/ (CO+CO2)=18%, roasting time 65min.The Theil indices analyzed in fired slags is 0.26%, and the volatility calculating stannum is 97.3%.
Comparative example 1:(is additive-free)
Stannum metallurgical slag (TSn5.49%) is accounted for 97% through broken, ore grinding to granularity-0.074mm ratio, described fine grinding material will add the bentonite of 1%, carry out agglomeration after mix homogeneously, dried, dry agglomerate is placed in weakly reducing atmosphere and carries out reduction roasting, sintering temperature 850 DEG C, calcination atmosphere is CO/ (CO+CO2)=18%, roasting time 65min.The Theil indices analyzed in fired slags is 5.26%, and the volatility calculating stannum is 5.2%.
Comparative example 2:(adds sulfur as additive)
Stannum metallurgical slag (TSn5.49%) is accounted for 97% through broken, ore grinding to granularity-0.074mm ratio, it is that 8:1 adds sulfur additive and 1% bentonite adhesive by mol ratio according to S/Sn in described fine grinding material, carry out agglomeration after mix homogeneously, dried, dry agglomerate is placed in weakly reducing atmosphere and carries out reduction roasting, sintering temperature 850 DEG C, calcination atmosphere is CO/ (CO+CO2)=18%, roasting time 65min.The Theil indices analyzed in fired slags is 4.51%, and the volatility calculating stannum is 18.9%.
Comparative example 3:(adds calcium chloride as additive)
Stannum metallurgical slag (TSn5.49%) is accounted for 97% through broken, ore grinding to granularity-0.074mm ratio, by described fine grinding material according to CaCl2The mol ratio of/Sn is that 8:1 adds calcium chloride additive and 1% bentonite adhesive, carries out agglomeration, dried after mix homogeneously, is placed in weakly reducing atmosphere by dry agglomerate and carries out reduction roasting, sintering temperature 850 DEG C, and calcination atmosphere is CO/ (CO+CO2)=18%, roasting time 65min.The Theil indices analyzed in fired slags is 4.07%, and the volatility calculating stannum is 25.9%.
From result above, stanniferous material adds appropriate additive, the volatility of stannum in reducing roasting process can be improved significantly, especially for the intractable stanniferous material of ore dressing, the volatility of stannum is up to more than 90%, and result of the test when comparative example does not use additive and uses sulfur and calcium chloride as additive shows that stannum volatility is less than 30%.
Claims (10)
1. the additive reclaiming stannum for strengthening stanniferous material reduction roasting, it is characterised in that: include the component of following weight portion:
50 parts～60 parts of fluorite；
Borax 20 parts～30 parts；
Sodium humate 20 parts～30 parts.
2. the additive reclaiming stannum for strengthening stanniferous material reduction roasting according to claim 1, it is characterised in that: it is made up of the component of following weight portion:
53 parts～57 parts of fluorite；
Borax 23 parts～27 parts；
Sodium humate 22 parts～24 parts.
3. the method for strengthening stanniferous material reduction roasting separation and recovery stannum of the additive described in claim 1 or 2, it is characterised in that: after stanniferous material is ground, with described additive mixing agglomeration；Gained agglomerate, through dried, is placed in reducing atmosphere, in 600 DEG C～850 DEG C roasting temperatures, reclaims the stannum fluoride of volatilization；Described reducing atmosphere is by CO and CO2Composition, the concentration of volume percent of CO is 10%～30%.
4. the additive according to claim 3 method for strengthening stanniferous material reduction roasting separation and recovery stannum, it is characterised in that: in described additive, calcium fluoride is (5～15) with the mol ratio of stannum in stanniferous material: 1.
5. the additive according to claim 4 method for strengthening stanniferous material reduction roasting separation and recovery stannum, it is characterised in that: in described additive, calcium fluoride is (8～12) with the mol ratio of stannum in stanniferous material: 1.
6. the additive according to claim 3 method for strengthening stanniferous material reduction roasting separation and recovery stannum, it is characterised in that: in described reducing atmosphere, the concentration of volume percent of CO is 12%～18%.
7. the additive according to claim 3 method for strengthening stanniferous material reduction roasting separation and recovery stannum, it is characterised in that: sintering temperature is 750～850 DEG C.
8. the additive according to claim 7 method for strengthening stanniferous material reduction roasting separation and recovery stannum, it is characterised in that: roasting time is 15～120min.
9. the additive according to claim 8 method for strengthening stanniferous material reduction roasting separation and recovery stannum, it is characterised in that: roasting time is 35～65min.
10. the additive according to claim 3 method for strengthening stanniferous material reduction roasting separation and recovery stannum, it is characterised in that: described stanniferous material is containing at least one in tailing, difficult tin-iron mine, stanniferous metallurgical slag；Described stanniferous material and additive are all ground to the mass percentage content of-0.074mm grade more than 80%.
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| CN201610143175.7A CN105734270B (en) | 2016-03-14 | 2016-03-14 | A kind of method for being used to strengthen the additive of stanniferous material reduction roasting recovery tin and separate and recover tin from stanniferous material |
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| CN201610143175.7A CN105734270B (en) | 2016-03-14 | 2016-03-14 | A kind of method for being used to strengthen the additive of stanniferous material reduction roasting recovery tin and separate and recover tin from stanniferous material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107034354A (en) * | 2017-04-28 | 2017-08-11 | 中南大学 | Additive and tin iron tailings calcification baking Separation of Tin iron method for strong permanent magnet ore deposit type tin iron tailings calcification baking |
| CN116676492A (en) * | 2023-04-12 | 2023-09-01 | 高邮市环创资源再生科技有限公司 | Method for preparing regenerated tin by arc furnace smelting |
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| CN102242253A (en) * | 2011-08-10 | 2011-11-16 | 中南大学 | Method for treating poor-tin middling ore and recovering iron-making raw material |
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| CN102242253A (en) * | 2011-08-10 | 2011-11-16 | 中南大学 | Method for treating poor-tin middling ore and recovering iron-making raw material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107034354A (en) * | 2017-04-28 | 2017-08-11 | 中南大学 | Additive and tin iron tailings calcification baking Separation of Tin iron method for strong permanent magnet ore deposit type tin iron tailings calcification baking |
| CN116676492A (en) * | 2023-04-12 | 2023-09-01 | 高邮市环创资源再生科技有限公司 | Method for preparing regenerated tin by arc furnace smelting |
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