CN1772957A - Electrolytic method for high Bi crude aluminum - Google Patents
Electrolytic method for high Bi crude aluminum Download PDFInfo
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- CN1772957A CN1772957A CN 200510032329 CN200510032329A CN1772957A CN 1772957 A CN1772957 A CN 1772957A CN 200510032329 CN200510032329 CN 200510032329 CN 200510032329 A CN200510032329 A CN 200510032329A CN 1772957 A CN1772957 A CN 1772957A
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Abstract
The present invention relates to an electrolytic method of high-bismuth lead matte whose bismuth content is below 1.0%. Its technical scheme is characterized by that its lead anode is made up by mixing high-bismuth lead matte and lead matte whose bismuth content is less than 0.5% according to a certain ratio and making them undergo a moulding process. The composition of said lead anode includes (by weight ratio): Pb greater than 98%, As, less than 0.3%, Sb + As: 0.7-1.1%, Bi, less than 1.0% and Ag, less than 0.25%. The prepared electrolyte contains the following components: lead 80-120 g/l, free silicofluoric acid 60-110 g/l, bismuth less than or equal to 0.002 g/l, copper less than or equal to 0.002 g/l and silver less than or equal to 0.001 g/l. The electrolytic condition is as follows: eletrolyte temperature is 45-50 deg.C, electrolyte circulating speed is 22-30 L/min. bath, current density is greater than or equal to 190 A/sq.m, bath voltage is controlled at 0.3-0.6V and electrolytic time is 48 hr.
Description
Technical field:
The present invention relates to a kind of plumbous smelting process, particularly a kind of method of handling bismuth-containing at the high Bi crude aluminum below 1.0%.
Background technology:
Flourish along with domestic coloured industry, the output of coloured product is soaring year by year, the particularly develop rapidly of Chinese Automobile Industry ' and production domesticization, the consumption and the output of domestic lead improve year by year, day being becoming tight of lead ore resource, the grade of lead ore constantly descends.As foreign matter content in the lead bullion of plumbous refinery feedstock particularly bi content improve thereupon, reach about 1.0%.The general plumbous production method that adopts of domestic production factory is traditional baking with agglomeration-retailoring of blast furnace-electrorefining Production Flow Chart.This method is as adopting high current density electrolysis, can enhance productivity, but to bismuth-containing in the lead anode, gold, silver, copper, arsenic, impurity such as antimony especially bismuth have strict demand, generally should be controlled at below 0.3%, because bismuth, gold, silver, copper, arsenic, antimony etc. are not discharge dissolving in electrolytic process, almost all enter in the lead anode slurry attached to the lead anode surface, lead anode slurry is that fine particle is suspended in easily to carry secretly in the electrolytic solution and sneaks into negative electrode, current density is higher, lead ion transmission speed in the electrolytic solution is accelerated, driving electrolytic solution increases from the speed of lead anode to cathode flow, make easier the carrying secretly of the lead anode slurry particle that is suspended in the electrolytic solution enter negative electrode and separate out lead, lead anode slurry is not come off attached to the lead anode surface.The current density that is adopted is higher, and foreign matter content should be lower in the anode.At the electrolysis process of the lead anode of high bi content, external producer such as day Benshen ridge and Canadian A Luoyi factory adopt lower current density (＜140A/m always
2) and the control anode in As, Sb, Bi ratio production method, this method production efficiency is not high, and adopts the producer of high current density electrolysis such as Japan to broadcast special tired your factory (trnil) of mill factory and Canada, the bismuth-containing amount all must be controlled at below 0.5% in its anode.Domestic enterprise has only strain smelting one family to carry out high current density electrolysis production, and its anode bismuth-containing amount is controlled at below 0.3%.Is Henan, Henan light gold plumbous? once attempted adopting 240A/m
2High current density electrolysis, bi content is up to standard in the lead abandons because of guaranteeing to separate out, and still adopts 170～180A/m
2Middle current density production.Therefore, how using the bismuth-containing amount to reach 0.1% high Bi crude aluminum and make raw material and produce the qualified lead of separating out with traditional plumbous electrolyzer, and improve the bismuth rate of recovery in the anode sludge and the production efficiency of complete assembly, is to need the problems further inquired into.
Summary of the invention:
The object of the present invention is to provide the electrolytic method of a kind of high Bi crude aluminum, it can use the bismuth-containing amount to reach 1.0% high Bi crude aluminum to go out the qualified lead of separating out as raw material production, improve the rate of recovery of bismuth and the production efficiency of complete assembly.
Technical scheme of the present invention is: a kind of method of electrolysis high Bi crude aluminum, comprise steps such as lead anode casting mold, electrolyte quota, electrolysis, anode washing, lead anode is to arrange in pairs or groups in the casting mold process less than 0.5% lead bullion less than 1.0% high Bi crude aluminum and bi content with the bismuth-containing amount to mix and make, and lead anode consists of the following weight ratio: Pb＞98%, As＜0.3%, Sb+As:0.7～1.1%, Bi＜1.0%, Ag＜0.25%;
Leaded 80～120g/l in the electrolytic solution of being prepared contains free silica fluoric acid 60～110g/l, bismuth≤0.002g/l, copper≤0.002g/l, silver≤0.001g/l;
Electrolytic condition is: current density 〉=190A/m
2, electrolyte temperature be 45～50 ℃, circulation of elecrolyte speed 22～30L/min groove, groove pressure-controlled at 0.3～0.6V, electrolysis time 48 hours;
As to further improvement of the present invention, described anode washing divides secondary to carry out, anode washing is for the first time scrubbed anode surface behind the anode electrolysis one-period, obtain the anode sludge, anode is back to the electrolysis of carrying out second period in the electrolyzer, carry out the anode washing second time again, get the anode scrap plate and the anode sludge.
As to further improvement of the present invention, described anode scrap plate is as the raw material of anode casting mold, and as the raw material that reclaims rare precious metal, washing time is 30～60 minutes to the described anode sludge after stirring, washing, press filtration, and washing lotion contains the free silica fluoric acid less than 60g/l.
As to further improvement of the present invention, press filtration is with 621 type nylon cloth bags in the described anode washing step.
As to further improvement of the present invention, described anode sludge wash water send in the clarifying tank clarification after 24 hours as the washing lotion of preparation electrolytic solution, bi content is less than 0.05g/l in the washing lotion.
As to further improvement of the present invention, described negative electrode is separated out lead and is met Pb99.995 standard-required among the GB/T469-1995, and the overwhelming majority is cast electric plumbous product, and small part is made cathode sheets and returned electrolysis.
Beneficial effect:
The bismuth-containing amount of the lead anode that the present invention can not direct pouring becomes reaches 0.1% high Bi crude aluminum and bismuth-containing and mixes less than 0.5% lead bullion, make bi content reduction in the lead anode that is cast into, prepare suitable electrolytic solution again, explore suitable electrolytic condition, realized under traditional electrolysis processing unit condition, carrying out the high current density electrolysis high Bi crude aluminum, separating out of output is plumbous up-to-standard, has the following advantages:
1, improved production efficiency.High current density electrolysis in, the electrolytic production efficiency height of low current density;
2, improved and comprised the recovery utilization rate of bismuth at interior valuable metal.The anode sludge of scrubbing gained is recycled, valuable metal is enriched in the filter residue, can further reclaim.
3, remarkable in economical benefits.Use the present invention result more than a year to show through the contriver: it is more than 99% that bismuth-containing＜0.0028% of high Bi crude aluminum institute output qualified separated out plumbous rate, produce 90000 tons of plumbous factories of separating out lead per year and can reclaim bismuth more than 200 tons more, the plumbous chemical ingredients of separating out of institute's output is checked through Hunan Province non-ferrous metal quality supervision and test granting station, the following % of its result: silver: 0.0016, bismuth: 0.0022, copper: 0.0004, arsenic: 0.001, antimony: 0.002, tin: 0.001, reach the requirement of the Pb99.995 standard among the GB/T469-1995.
4, alleviated because of using high Bi crude aluminum to go out the qualified plumbous product and the contradiction of leady raw materials shortage, made existing plumbous electrolyzer can adapt to the production requirement of different leady raw materialses as raw material production.
Embodiment:
Embodiment 1: the composition that high Bi crude aluminum is made into behind the lead anode is that following weight is than (%): Pb:98.25, As:0.20, As+Sb:0.85, Bi:0.59, Ag:0.23, Cu:0.05, main component in the electrolytic solution is: Pb120g/l, free silica fluoric acid 110g/l, Bi0.001g/l, Ag0.001g/l, Cu0.0017g/l, electrolytic current density 220A/m
2, electrolyzer is pressed and to be 0.42v, cathode efficiency is 98.94%, after the electrolysis output separate out plumbous bismuth-containing 0.00091%, silver: 0.0002%, copper: 0.0005%, arsenic: 0.001%, antimony: 0.002%, tin: 0.001%.In free silica fluoric acid concentration is under 60 minutes the situation of 40g/l agitator treating, and the anode sludge wash water of output clarification detects wherein after 24 hours that bismuth-containing is 0.041g/l, meets the requirement of allocating in the electrolytic solution.
Embodiment 2: the composition that high Bi crude aluminum is made into behind the lead anode is that following weight is than (%): Pb:98.20, As:0.17, As+Sb:0.70, Bi:0.90, Ag:0.15, Cu:0.04, main component in the electrolytic solution is: Pb80g/l, free silica fluoric acid 90g/l, Bi0.0015g/l, Ag0.0010g/l, Cu0.0012g/l, electrolytic current density 196A/m
2, electrolyzer is pressed and to be 0.38v, cathode efficiency is 98.58%, after the electrolysis output separate out plumbous bismuth-containing 0.0012%, silver: 0.0001%, copper: 0.0003%, arsenic: 0.002%, antimony: 0.002%, tin: 0.001%.In free silica fluoric acid concentration is under 30 minutes the situation of 60g/l agitator treating, and the anode sludge wash water of output clarification detects wherein after 24 hours that bismuth-containing is 0.020g/l, meets the requirement of allocating in the electrolytic solution.
Embodiment 3: the composition that high Bi crude aluminum is made into behind the lead anode is that following weight is than (%): Pb:98.21, As:0.23, As+Sb:1.10, Bi:0.50, Ag:0.15, main component in the Cu:0.03 electrolytic solution is: Pb90g/l, free silica fluoric acid: 85g/l, Bi:0.0018g/l, Ag:0.0007g/l, Cu:0.0015g/l, electrolytic current density 196A/m
2, electrolyzer is pressed and to be 0.50v, cathode efficiency is 98.77%, after the electrolysis output separate out plumbous bismuth-containing 0.0025%, silver: copper 0.0001%: arsenic 0.0003%: antimony 0.002%: 0.003%,, tin: 0.002%.In free silica fluoric acid concentration is under 40 minutes the situation of 30g/l agitator treating, and the anode sludge wash water of output clarification detects wherein after 24 hours that bismuth-containing is 0.011g/l, meets the requirement of allocating in the electrolytic solution.
The present invention is including but not limited to the foregoing description; as long as adopted high Bi crude aluminum and bismuth-containing to mix to reduce in the lead anode bi content and to prepare suitable electrolytic solution and carry out electrolytic method, promptly belonged to protection scope of the present invention at suitable electrolytic condition less than 0.5% lead bullion.
Claims (6)
1, a kind of method of electrolysis high Bi crude aluminum, comprise steps such as lead anode casting mold, electrolyte quota, electrolysis, anode washing, it is characterized in that: lead anode is to arrange in pairs or groups less than 0.5% lead bullion with high Bi crude aluminum and bi content to mix and make in the casting mold process, and lead anode consists of the following weight ratio: plumbous＞98%, arsenic＜0.3%, arsenic+antimony: 0.7～1.1%, bismuth＜1.0%, silver＜0.25%;
Leaded 80～120g/l in the electrolytic solution of being prepared contains free silica fluoric acid 60～110g/l, bismuth≤0.002g/l, copper≤0.002g/l, silver≤0.001g/l;
Electrolytic condition is: current density 〉=190A/m
2, electrolyte temperature be 45～50 ℃, circulation of elecrolyte speed 22～30L/min groove, groove pressure-controlled at 0.3～0.6V, electrolysis time 48 hours.
2, the method for electrolysis high Bi crude aluminum according to claim 1, it is characterized in that: described anode washing divides secondary to carry out, anode washing is for the first time scrubbed anode surface behind the anode electrolysis one-period, obtain the anode sludge, anode is back to the electrolysis of carrying out second period in the electrolyzer, carry out the anode washing second time again, get the anode scrap plate and the anode sludge.
3, the method for electrolysis high Bi crude aluminum according to claim 2, it is characterized in that: described anode scrap plate is as the raw material of anode casting mold, the raw material of rare precious metal is reclaimed in the conduct after stirring, washing, press filtration of the described anode sludge, washing time is 30～60 minutes, and washing lotion contains the free silica fluoric acid less than 60g/l.
4, the method for electrolysis high Bi crude aluminum according to claim 3 is characterized in that: press filtration is with 621 type nylon cloth bags in the described anode washing step.
5, the method for electrolysis high Bi crude aluminum according to claim 3 is characterized in that: described anode sludge wash water is sent into the washing lotion of clarification conduct preparation electrolytic solution after 24 hours in the clarifying tank, and bi content is less than 0.05g/l in the washing lotion.
6, the method for electrolysis high Bi crude aluminum according to claim 1 is characterized in that: described negative electrode is separated out lead and is met Pb99.995 standard-required among the GB/T469-1995, and the overwhelming majority is cast electric plumbous product, and small part is made cathode sheets and returned electrolysis.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100323297A CN100545318C (en) | 2005-11-01 | 2005-11-01 | A kind of electrolysis process of high Bi crude aluminum |
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| CNB2005100323297A CN100545318C (en) | 2005-11-01 | 2005-11-01 | A kind of electrolysis process of high Bi crude aluminum |
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| CN1772957A true CN1772957A (en) | 2006-05-17 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101974765A (en) * | 2010-08-31 | 2011-02-16 | 云南锡业集团（控股）有限责任公司 | Comprehensive method for separating stibium from materials containing stibium, tin and lead |
| WO2011063577A1 (en) * | 2009-11-24 | 2011-06-03 | 江西稀有金属钨业控股集团有限公司 | Method of washing anode slime from lead-bismuth alloy electrolysis |
| CN103290429A (en) * | 2013-06-17 | 2013-09-11 | 湖南省桂阳银星有色冶炼有限公司 | Method for electrolyzing high-content low-grade lead bullion |
| CN103938228A (en) * | 2014-03-26 | 2014-07-23 | 湖南水口山有色金属集团有限公司 | Purifying method for removing impurities metal ions in lead electrolyte and anode slime washing water |
| CN104947146A (en) * | 2015-06-03 | 2015-09-30 | 郴州市金贵银业股份有限公司 | Method for electrolyzing and recycling valuable metal from high-bismuth lead bullion |
| CN105887138A (en) * | 2016-06-16 | 2016-08-24 | 郴州市金贵银业股份有限公司 | Method for treating lead bullion through electrorefining |
| CN106011931A (en) * | 2016-08-08 | 2016-10-12 | 昆明冶金研究院 | Large-pole plate long-time cycle lead anode two-step electrolytic refining method |
| CN106916954A (en) * | 2017-01-20 | 2017-07-04 | 株洲冶炼集团股份有限公司 | A kind of method washed lead anode slurry and reclaim lead in lead anode slurry |
| CN118028903A (en) * | 2024-04-11 | 2024-05-14 | 矿冶科技集团有限公司 | Method for preparing lead particles by two-stage suspension electrolysis of waste lead plaster |
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| US4026776A (en) * | 1970-12-02 | 1977-05-31 | Mitsui Mining & Smelting Co., Ltd. | Method for producing high purity lead |
| US3960681A (en) * | 1974-02-21 | 1976-06-01 | Mitsui Mining & Smelting Co., Ltd. | Method for producing electrolytic high purity lead using large-sized electrodes |
| CA1126684A (en) * | 1978-04-06 | 1982-06-29 | Robert C. Kerby | Bipolar refining of lead |
| AU4093989A (en) * | 1988-09-06 | 1990-03-15 | Institute Po Tzvetna Metalurgia | Method and apparatus for electric refining of lead |
| JP2002210340A (en) * | 2001-01-22 | 2002-07-30 | Core Medical Kk | Ozone water producer |
| RU2197565C1 (en) * | 2001-07-27 | 2003-01-27 | Северо-Кавказский государственный технологический университет | Process of electrolytic refining of bismuth lead |
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| WO2011063577A1 (en) * | 2009-11-24 | 2011-06-03 | 江西稀有金属钨业控股集团有限公司 | Method of washing anode slime from lead-bismuth alloy electrolysis |
| US9051624B2 (en) | 2009-11-24 | 2015-06-09 | Jiangxi Rare Earth and Rare Metals Tungsten Group Holding Co., Ltd. | Method of washing anode slime from lead-bismuth alloy electrolysis |
| CN101974765A (en) * | 2010-08-31 | 2011-02-16 | 云南锡业集团（控股）有限责任公司 | Comprehensive method for separating stibium from materials containing stibium, tin and lead |
| CN103290429A (en) * | 2013-06-17 | 2013-09-11 | 湖南省桂阳银星有色冶炼有限公司 | Method for electrolyzing high-content low-grade lead bullion |
| CN103938228A (en) * | 2014-03-26 | 2014-07-23 | 湖南水口山有色金属集团有限公司 | Purifying method for removing impurities metal ions in lead electrolyte and anode slime washing water |
| CN103938228B (en) * | 2014-03-26 | 2016-08-10 | 湖南水口山有色金属集团有限公司 | Lead electrolytic solution and the purification method of earth of positive pole wash water foreign metal ion |
| CN104947146A (en) * | 2015-06-03 | 2015-09-30 | 郴州市金贵银业股份有限公司 | Method for electrolyzing and recycling valuable metal from high-bismuth lead bullion |
| CN105887138A (en) * | 2016-06-16 | 2016-08-24 | 郴州市金贵银业股份有限公司 | Method for treating lead bullion through electrorefining |
| CN106011931A (en) * | 2016-08-08 | 2016-10-12 | 昆明冶金研究院 | Large-pole plate long-time cycle lead anode two-step electrolytic refining method |
| CN106916954A (en) * | 2017-01-20 | 2017-07-04 | 株洲冶炼集团股份有限公司 | A kind of method washed lead anode slurry and reclaim lead in lead anode slurry |
| CN106916954B (en) * | 2017-01-20 | 2019-03-29 | 株洲冶炼集团股份有限公司 | A method of washing lead anode slurry simultaneously recycles lead in lead anode slurry |
| CN118028903A (en) * | 2024-04-11 | 2024-05-14 | 矿冶科技集团有限公司 | Method for preparing lead particles by two-stage suspension electrolysis of waste lead plaster |
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| CN100545318C (en) | 2009-09-30 |
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