CN101705372A - Process for extracting tin from wet lead with high tin content - Google Patents
Process for extracting tin from wet lead with high tin content Download PDFInfo
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- CN101705372A CN101705372A CN200910227075A CN200910227075A CN101705372A CN 101705372 A CN101705372 A CN 101705372A CN 200910227075 A CN200910227075 A CN 200910227075A CN 200910227075 A CN200910227075 A CN 200910227075A CN 101705372 A CN101705372 A CN 101705372A
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- tin
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- plumbous liquid
- slag
- lead
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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
Abstract
The invention relates to a process for extracting tin from wet lead with high tin content. The process comprises the following steps: removing parts of impurities of copper, arsenic, stibium, and the like according to the traditional technological means in an initial fire refining process, raising temperature to 700 to 800 DEG C, adding alkaline oxidizers of sodium nitrate, sodium hydroxide, and the like to oxide tin for slagging, and stirring for a long time to make materials fully react. The invention adopts a high temperature alkali method to oxidize tin , separate tin from lead and recover tin in a mode of tin oxide slag. The effect that tin content of an anode plate is below 0.06 % is achieved, the average direct yield of tin content of tin slag is 96.58 %, and the tin content in wet tin is basically extracted from the tin slag completely.
Description
Technical field
The present invention relates to a kind of process for extracting tin from wet lead with high tin content.The high tin lead bullion of indication of the present invention is by smelting the lead bullion of institute's output with the symbiotic lead ore of tin ore, and its stanniferous weight percent is up to 1~4%.
Background technology
The lead bullion purification is called plumbous refining for lead bullion, its process is removed foreign metal exactly, China generally uses electrolytic process as plumbous purified technical process, its flow process can be sketched and be: the preliminary refining of pyrogenic process, promptly common title market pot slag making removal of impurities → positive plate → electrorefining → separate out lead → final refining promptly claims electric lead pan slag making removal of impurities → electricity lead usually.In plumbous electrolytic process, the electropotential of the foreign metal tin in the lead bullion is-0.136V, and plumbous electropotential is-0.127V, both are very approaching, therefore, metallic tin can also can be separated out at negative electrode at anode dissolution, therefore can have a strong impact on and separate out plumbous quality, thereby influence the plumbous quality of the finished product electricity.Under the normal circumstances, the lead bullion stanniferous is≤0.8%, and the lead refinery can the preliminary refining of pyrogenic process before electrolysis be oxidized into scum silica frost with the prior art oxidation style and removes.The method of so-called prior art detin is that oxidation refining method is in the lead bullion market pot, is warming up to 600 ℃ of excess molten earlier, drags for oxidation scum for the first time, removes fire again and is cooled to 340 ℃ of liquate copper removals.Continue then to heat up, under 450 ℃ temperature, since tin to the avidity of oxygen greater than the avidity of lead to oxygen, therefore the scum silica frost of electricity consumption lead pan is that the oxidation lead skim is made oxygenant, by mechanical stirring it is joined in the plumbous liquid, the oxygen in the plumbous oxide is captured generation by the tin in the plumbous liquid and is insoluble to plumbous stannic oxide, floats on plumbous liquid surface, be the shoddye shape and dragged for, as shown in the formula:
2PbO+Sn=2Pb+SnO
2
This moment, preliminary refined product positive plate stanniferous can drop to below 0.25%, more easily removed in subsequently electrorefining and final refining, can guarantee that electric lead reaches the requirement of first grade quality standard; The index of the plumbous quality standard of alleged first grade is: Pb content mass percent is more than 99.994%, and Sn content mass percent is below 0.001%.
But aforesaid method is handled up to 1~4% high tin lead bullion for stanniferous, and its positive plate separates out that plumbous stanniferous is assorted can be reached more than 0.6%, and will have a strong impact on electric plumbous requisite quality this moment.
With the closely-related patented technology of the present invention be that state's invention patent publication No. CN87104574A disclosed a kind of " new technique of fire refining method for bullion lead " is through liquate with add the sulphur copper removal with lead bullion in 30 days March in 1988, in kier, add sodium hydroxide again, feeding pressurized air and oxygen compression air mixed by 4: 1 after airduct is blown into melt with oxygen under 600 to 630 ℃ of temperature, and pressure is 3~4 kilograms per centimeter
2Generate corresponding about salt with sodium hydroxide behind arsenic in the lead bullion, antimony, the tin oxidation of impurities and remove the first grade quality standard requirement that this method does not reach electricity lead to high tin lead bullion processing equally.
Summary of the invention
Task of the present invention promptly is at prior art big to the assorted difficulty of high tin lead bullion detin, a kind of process for extracting tin from wet lead with high tin content is provided, it tin in the high tin lead bullion can be enriched to stanniferous more than 40% as plumbous purified byproduct stannic oxide scum silica frost, make it not only finish plumbous refining removal of impurities and reach the requirement of first grade quality standard, and the valency that has that produces tin metal reclaims, and kills two birds with one stone.
The present invention is achieved in that
A kind of process for extracting tin from wet lead with high tin content is when handling high tin lead bullion, adopts the high temperature alkaline process that the tin oxidation is separated with lead and reclaims with the form of oxidation scruff, has obtained the effect of positive plate stanniferous below 0.06%; This method is to remove impurity such as part copper, arsenic, antimony in the preliminary fire refining process earlier by the prior art means, be warming up to 700~800 ℃ again, add alkaline oxidisers such as SODIUMNITRATE, sodium hydroxide to the tin oxidative slagging, be equipped with long-time stirring medicament is fully reacted, as shown in the formula:
5Sn+6NaOH+4NaNO
3=5Na
2SnO
3+N
2↑+3H
2O
In addition, also to add industrial sodium-chlor in the process,,, reduce NaNO so can reduce the fusing point and the viscosity of slag though its react with has not improved the receptivity of NaOH to impurity salt
3Consumption.
Concrete steps are as follows:
1. prepare burden: choose the lead bullion raw material of high tin lead bullion raw material and stanniferous weight≤0.8% respectively, both mix and match become the pot material of stanniferous weight about 1.5%;
2. dress pot fusing: the pot material that will the match market pot of packing into, heat temperature raising to 560~580 ℃, the melting tank material becomes plumbous liquid; Described market pot is meant that capacity can be installed in 20~25 tons of pot material, and pot mouthful diameter is 2 meters a cauldron;
3. press slag, drag for copper ashes: continue the plumbous liquid heating in the market pot when plumbous liquid temp is raised to 600~650 ℃, is begun to press slag; Pressing slag is to apply downward pressure to floating over the lip-deep scum silica frost of plumbous liquid, and scum silica frost is immersed in the plumbous liquid again; Press slag to require evenly, the scum silica frost on the whole cooker face all will be pressed onto and be immersed in entirely in the plumbous liquid; Subsequently, hang in stirrer with weight handling equipment and stir, add husk or wood sawdust slag making with spades while stirring pressing the plumbous liquid behind the slag in the market pot; Behind the stir about 0.5h, the scum silica frost that floats over plumbous liquid surface is a copper ashes, and the add-on of described husk or wood sawdust is by pot material 1~1.5kg per ton; Manually the spades with the band small opening drags for the copper ashes on clean plumbous liquid surface;
4. make scruff: after having dragged for copper ashes, at plumbous liquid surface coverage one deck industry sodium-chlor, industry sodium-chlor consumption is decided on the lead bullion stanniferous, the lead bullion of stanniferous 1% adds 50kg industry sodium-chlor by pot material per ton and gets, the lead bullion of stanniferous 2% adds 75kg industry sodium-chlor by pot material per ton to be got, and the lead bullion of stanniferous more than 3% adds 100kg industry sodium-chlor by pot material per ton and get; Continuation is to plumbous liquid heat temperature raising 4~6h, and when plumbous liquid variable color was capsanthin, be equivalent to plumbous liquid temp and be raised to 700~800 ℃ this moment; Hang in after stirrer stirs 0.5h by lifting machine, get the adding SODIUMNITRATE by pot material 35kg per ton earlier with spades; Get adding sodium hydroxide by pot material 15kg per ton more afterwards; Continue to stir 4~7h; Before playing pot, expect to get to add 35kg SODIUMNITRATE and 8kg sodium hydroxide by pot per ton once more, continue to play pot behind the stir about 20min;
5. drag for scruff: after playing pot, hang out stirrer, pull scruff out with spades with holes; The clean plumbous liquid of drop of should trying one's best when dragging for slag drags for clean scruff simultaneously, allows the plumbous liquid that drags for behind the clean scruff be cooled to about 450 ℃, insulation, casting, the chloride plate of refining removal of impurities; The scruff of pulling out, to grain diameter 2mm, tin metal is reclaimed in pack with crusher in crushing.
Technology of the present invention can be finished the removal of impurities of the high tin refining of lead bullion, tin in the high tin lead bullion can be enriched to stanniferous more than 40% as plumbous purified byproduct stannic oxide scum silica frost; The chloride plate of obtaining reaches the requirement of first grade quality standard, and the scruff final product quality of gained is better, main chemical compositions: Sn 〉=40%, Pb≤25%, Ag≤200g/t.Technology direct yield height of the present invention, workable, the average direct yield of scruff stanniferous is 96.58%, and the tin content in the lead bullion is all proposed from scruff basically.
Embodiment
Below in conjunction with the present invention is described in detail in conjunction with specific embodiments.
A kind of process for extracting tin from wet lead with high tin content, concrete steps are as follows:
1. prepare burden: choose the lead bullion raw material of high tin lead bullion raw material and stanniferous weight≤0.8% respectively, should mix into about 1.5% going into a pot lead bullion stanniferous as far as possible, scruff quality that extract this moment and quantity are all comparatively desirable.The lead bullion stanniferous is≤0.8%;
2. dress pot fusing
A. adorn the strike number amount: this detin market pot is the pot of Φ 2m25t, and lead bullion dress strike number amount is 20~25t.
B. fusing: behind the dress pot, heat temperature raising to 560~580 ℃, the melting tank material becomes plumbous liquid; This operation needs 2~3h approximately.
3. press slag, drag for copper ashes
A. press slag: continue the plumbous liquid heating in the market pot when plumbous liquid temp is raised to 600~650 ℃, is begun to press slag, press slag to require evenly, the scum silica frost on the whole cooker face all will be pressed onto and be immersed in entirely in the plumbous liquid;
B. stir: hang in stirrer with weight handling equipment and stir, add husk or wood sawdust slag making with spades while stirring pressing the plumbous liquid behind the slag in the market pot; The add-on of described husk or wood sawdust is by pot material 1~1.5kg per ton;
C. drag for slag: behind the stir about 0.5h, the scum silica frost that floats over plumbous liquid surface is a copper ashes, and behind the stir about 0.5h, manually the spades with the band small opening drags for the copper ashes on clean plumbous liquid surface;
4. make scruff
A. heat up, processing industry sodium-chlor: after having dragged for copper ashes, increasing firepower to temperature rises to 700~800 ℃ (are that capsanthin is advisable with plumbous liquid variable color), adds industrial sodium-chlor 50~100kg (50kg/ bag) covering surfaces simultaneously.Industry sodium-chlor consumption is decided on the lead bullion stanniferous, and generalized case is: stanniferous 1% adds 50kg, and stanniferous 2% adds 75kg, and stanniferous adds 100kg more than 3%.This operation needs 4~6h approximately.
B. stir, oxidizer: after treating that plumbous liquid reddens, hang in stirrer and stir, open cooling water chiller case.Behind the stir about 0.5h, add 2/3 an about 35kg SODIUMNITRATE of wrapping, add 2/3 about 15kg sodium hydroxide of a bag afterwards again with spades.The high-temperature stirring time is about 4~7h, and time length depends on that plumbous liquid brightness and scruff outward appearance are grass green, Φ 10mm left and right sides particle is good.Playing the bag surplus that pot precontract 20min adds SODIUMNITRATE and sodium hydroxide, continue to play pot behind the stir about 20min.Total add-on of SODIUMNITRATE and sodium hydroxide is a bag when lead bullion stanniferous 1.5% left and right sides.Wherein the SODIUMNITRATE 50kg/ of above-mentioned indication wraps, sodium hydroxide 25kg/ bag.
5. drag for scruff: after playing pot, treat that scruff reaches requirement, hang out stirrer, pull scruff out with spades with holes; The clean plumbous liquid of drop of should trying one's best when dragging for slag drags for clean scruff simultaneously, allows the plumbous liquid that drags for behind the clean scruff be cooled to about 450 ℃, insulation, casting, the chloride plate of refining removal of impurities; The scruff of pulling out, to grain diameter 2mm, tin metal is reclaimed in pack with crusher in crushing.
Present embodiment is about 10~16h whole man-hours, does not comprise the lead bullion dress pot time.
Quality product requires:
The scruff chemical ingredients requires: Sn 〉=40%, Pb≤25%, Ag≤200g/t.
The scruff physical specification requires: grass green, and granularity 10 ± 5mm smashes scruff to 2mm with making husky machine again, the woven bag of about 30~40kg/ bag of packing into, dividing about 30t is a collection of neat sign indicating number heap, and carries out mark.
This technology lead bullion is carried process of tin batching inventory
Annotate: this inventory must be adjusted according to the variation of raw materials quality or processing requirement.
Claims (2)
1. process for extracting tin from wet lead with high tin content, it is characterized in that: in the preliminary fire refining process, remove impurity such as part copper, arsenic, antimony earlier by the prior art means, be warming up to 700~800 ℃ again, add alkaline oxidisers such as SODIUMNITRATE, sodium hydroxide to the tin oxidative slagging, be equipped with long-time stirring medicament is fully reacted, as shown in the formula:
5Sn+6NaOH+4NaNO
3=5Na
2SnO
3+N
2↑+3H
2O
Concrete steps are as follows:
1. prepare burden: choose the lead bullion raw material of high tin lead bullion raw material and stanniferous weight≤0.8% respectively, both mix and match become the pot material of stanniferous weight about 1.5%;
2. dress pot fusing: the pot material that will the match market pot of packing into, heat temperature raising to 560~580 ℃, the melting tank material becomes plumbous liquid;
3. press slag, drag for copper ashes: continue the plumbous liquid heating in the market pot when plumbous liquid temp is raised to 600~650 ℃, is begun to press slag; Press slag to require evenly, the scum silica frost on the whole cooker face all will be pressed onto and be immersed in entirely in the plumbous liquid; Subsequently, hang in stirrer with weight handling equipment and stir, add husk or wood sawdust slag making with spades while stirring pressing the plumbous liquid behind the slag in the market pot; Behind the stir about 0.5h, the scum silica frost that floats over plumbous liquid surface is a copper ashes, and the add-on of described husk or wood sawdust is by pot material 1~1.5kg per ton; Manually the spades with the band small opening drags for the copper ashes on clean plumbous liquid surface;
4. make scruff: after having dragged for copper ashes, at plumbous liquid surface coverage one deck industry sodium-chlor, industry sodium-chlor consumption is decided on the lead bullion stanniferous, the lead bullion of stanniferous 1% adds 50kg industry sodium-chlor by pot material per ton and gets, the lead bullion of stanniferous 2% adds 75kg industry sodium-chlor by pot material per ton to be got, and the lead bullion of stanniferous more than 3% adds 100kg industry sodium-chlor by pot material per ton and get; Continuation is to plumbous liquid heat temperature raising 4~6h, and when plumbous liquid variable color was capsanthin, be equivalent to plumbous liquid temp and be raised to 700~800 ℃ this moment; Hang in after stirrer stirs 0.5h by lifting machine, get the adding SODIUMNITRATE by pot material 35kg per ton earlier with spades; Get adding sodium hydroxide by pot material 15kg per ton more afterwards; Continue to stir 4~7h; Before playing pot, expect to get to add 35kg SODIUMNITRATE and 8kg sodium hydroxide by pot per ton once more, continue to play pot behind the stir about 20min;
5. drag for scruff: after playing pot, hang out stirrer, pull scruff out with spades with holes; The clean plumbous liquid of drop of should trying one's best when dragging for slag drags for clean scruff simultaneously, allows the plumbous liquid that drags for behind the clean scruff be cooled to about 450 ℃, insulation, casting, the chloride plate of refining removal of impurities; The scruff of pulling out, to grain diameter 2mm, tin metal is reclaimed in pack with crusher in crushing.
2. process for extracting tin from wet lead with high tin content according to claim 1 is characterized in that: described market pot is meant that capacity can be installed in 20~25 tons of pot material, and pot mouthful diameter is 2 meters a cauldron.
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CN102534249A (en) * | 2012-02-22 | 2012-07-04 | 郴州丰越环保科技有限公司 | Method for refining tin from high-silver crude tin |
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DE507769C (en) * | 1924-12-11 | 1930-09-19 | Henry Harris | Treatment of molten metals and alloys containing at least two different metals for the deposition of one or more of these metals by the use of oxidizing agents |
CN1003310B (en) * | 1987-06-27 | 1989-02-15 | 昆明工学院 | New technique of fire refining method for bullion lead |
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