CN102534660B - Method for electrolytically refining crude lead - Google Patents

Method for electrolytically refining crude lead Download PDF

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CN102534660B
CN102534660B CN201210010362.XA CN201210010362A CN102534660B CN 102534660 B CN102534660 B CN 102534660B CN 201210010362 A CN201210010362 A CN 201210010362A CN 102534660 B CN102534660 B CN 102534660B
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lead
sodium hydroxide
electrolytic solution
refining
electrolyte
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CN102534660A (en
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刘伟
杨天足
周琼华
张杜超
刘伟锋
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Henan University of Science and Technology
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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
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Abstract

The invention discloses a method for electrolytically refining crude lead. The method comprises the following steps of: adding sodium hydroxide and tartaric acid into water in turn, and stirring to dissolve at normal temperature to obtain a mixed solution; adding lead oxide powder into the mixed solution, dissolving and filtering to obtain filtrate, namely electrolyte; and adding the prepared electrolyte into an electrolytic cell, and switching on direct current for electrolysis by taking a stainless steel plate or a pure lead plate as a cathode and crude lead to be refined as an anode. By the method, smoke and middle slag generated in pyro-refining are avoided, the direct recovery rate of lead and comprehensive recovery rate of valued metals in the refining process are improved, volatile smoke or acid mist cannot be generated, and a defect that electrolyte in a silicofluoric acid system pollutes environment is overcome; meanwhile, the sodium hydroxide and the tartaric acid are added into the electrolyte, so that the sodium hydroxide and the tartaric acid can form a complex with the lead oxide, the concentration of lead ions in the electrolyte is greatly increased and the electrolysis efficiency is improved.

Description

A kind of method of performing electrolytic refining on lead bullion
Technical field
The present invention relates to plumbous purification refining field, a kind of method of performing electrolytic refining on lead bullion specifically.
Background technology
In order to remove detrimental impurity in lead bullion and to reclaim precious metal, must carry out refining to it, the method for the refining of lead bullion is divided two kinds of pyrogenic process and electrolytic process.The master operation of fire refining process is: 1. copper removal: first liquate or condensation copper removal, then add sulphur deep copper removal; 2. add caustic soda except tellurium; 3. with oxidation style or alkali-chloride improving arsenic removal, antimony, tin; 4. zincification reclaims gold and silver; 5. dezincify; 6. add calcium magnesium except bismuth; 7. final refining ingot casting obtains lead bullion.The slag of each operation output processes respectively to reclaim wherein valuable element.Pyrorefining lead bullion produces quite a large amount of leaded (and other metal) flue dust, various middle slag and sulfur dioxide gas, and contaminate environment is serious, and plumbous direct yield and comprehensive recovery is lower simultaneously.
Compared with pyrogenic process, the waste gas that electrolytic process produces is few, and energy consumption is low, and therefore superior product quality is widely used in the refining of lead bullion.The method that current industrial lead bullion electrorefining extensively adopts is Bai Zifa, and lead bullion is cast positive plate, is processed into starting sheet with negative electrode lead, is containing PbSiF 6with free H 2siF 6in solution, carry out electrolysis.Bai Zifa is widely used in the plumbous smeltery of the states such as China, Canada, Italy, Japan, Peru, Russia at present.But there are some shortcomings in Bai Zifa, as H 2siF 6volatile, job site can produce a large amount of acid mists, and the smell is awful, PbSiF 6preparation process in can emit HF and SiF 4gas, to human body and environmental hazard very large volumes such as (, heavy non-ferrous metal smelting design manual: plumbous zinc bismuth volume, Beijing: metallurgical industry press, 1995, P88-106, P119-146) Beijing Nonferrous Metallurgy Design Research Institute.Other acid system of once studying has muriate, nitrate, borate salt system etc., but only limits to plumbous electrodeposition, there is not yet the report that is applied to the refining of lead bullion, and acid electrolyte is volatile, pollutes generally larger.
Summary of the invention
The present invention be solve prior art in the time of lead bullion electrorefining to environment and the very large problem of harm, a kind of method of performing electrolytic refining on lead bullion is provided, the method, by containing the electrorefining that carries out lead bullion in tartaric basic solution, can alleviate the environmental pollution of electrolytic process and the harm to human body.
The present invention solves the problems of the technologies described above the technical scheme of employing to be: a kind of method of performing electrolytic refining on lead bullion, sodium hydroxide, tartrate are added to the water successively, stirring and dissolving makes mixing solutions at normal temperatures, and the add-on of tartrate and sodium hydroxide is in every liter of mixing solutions, to add 100 ~ 160g tartrate, 80 ~ 160g sodium hydroxide; Then in mixing solutions, adding lead oxide powder, is stirring and dissolving under 40 ~ 98 ℃, the condition of stirring velocity 200 ~ 400r/min in temperature, and time 1 ~ 6h, then filters, and gained filtrate is electrolytic solution; The granularity of described lead oxide powder is less than 200 orders, and in the electrolytic solution preparing, plumbum ion concentration is 80 ~ 130g/L;
The electrolytic solution making is added in electrolyzer, adopt stainless steel plate or pure stereotype as negative electrode, employing treats that the lead bullion of refining makes anode, pass into direct current and carry out electrolysis, concrete electrolytic process parameter is: 40 ~ 60 ℃ of electrolyte temperatures, the circulation of elecrolyte cycle is 45 ~ 120min, and circulation of elecrolyte mode is bottom in and top out, cathode current density 100 ~ 160A/m 2, bath voltage 0.25 ~ 1.0V, anodic current density 100 ~ 160A/m 2, with interpole gap 80 ~ 130mm;
In electrolytic process, rise to 1.0V when bath voltage, while there is anode passivation, take out positive plate and scrub or double teeming positive plate, scrub or double teeming after positive plate return to participation electrolysis;
According to the steam output of electrolytic solution, timing is to make up water in electrolytic solution, to maintain plumbum ion concentration 80 ~ 130g/L in electrolytic solution, sodium hydroxide 80 ~ 160 g/L and tartaric acid concentration 100 ~ 160 g/L;
The dirt settling of collecting on negative electrode is the lead obtaining after refining.
In the present invention, described tartrate, sodium hydroxide and plumbous oxide are analytical pure or technical grade reagent.
The present invention can carry out in the time of the dirt settling of collecting on negative electrode in the time scrubbing anode.
In the present invention, in the time of preparation electrolytic solution, add sodium hydroxide and tartaric reason to be: sodium hydroxide and tartrate can form a kind of structure that is similar to title complex with plumbous oxide, can greatly increase the concentration of lead ion in electrolytic solution, the electrolytic solution of alkalescence is also more stable in the time of electrolysis simultaneously, can not produce environment and the harmful gas of human body.
In the present invention, in electrolytic process, the anode of being poured into a mould by lead bullion, under the effect of electric current, lead constantly enters into electrolytic solution and forms title complex, and then title complex obtains electron reduction for plumbous at negative electrode; Anode constantly dissolves, and final anode is remaining is the anode sludge of anode scrap and precious metal composition.
The present invention is applicable to the lead bullion of plumbous smelting process output, and its main component scope is: Pb 96% ~ 99%, Sb 0.5% ~ 3%, Cu 0.05% ~ 3%, As 0.005% ~ 1.5%, Sn 0.02% ~ 1%, Bi 0.1% ~ 1%, Ag 0.1% ~ 3%; Also be suitable for processing lead antimony alloy, lead bismuth alloy etc.
Beneficial effect: the present invention and traditional plumbous refinery practice comparison, have following advantage: 1, the present invention has avoided various flue dust, the middle slag that pyrorefining produces, and has improved the direct yield of refining process lead and the comprehensive recovery of various valuable metals;
2, alkaline organic electrolysis system is environmentally friendly, can not produce volatilization flue dust or acid mist, has overcome the shortcoming of silicofluoric acid system electrolyte contamination environment;
3, in electrolytic solution, add sodium hydroxide and tartrate to form title complex with plumbous oxide, greatly increased the concentration of lead ion in electrolytic solution, improved electrolytic efficiency.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment 1
Lead content in lead bullion is 98.30%, and major impurity composition is tin 0.0008%, antimony 0.8281%, bismuth 0.1363%, arsenic 0.5127%, copper 0.0795%, zinc 0.0006%, silver 0.1406%, iron 0.0013%.Tartrate, sodium hydroxide and plumbous oxide are analytical pure.
Take lead bullion 500 g, in retort furnace, 600 ℃ of fusing 15 min that heat take out, and are cast into positive plate in graphite jig, are of a size of 10cm × 10cm.
Take 200 g plumbous oxide, 180 g sodium hydroxide, 180 g tartrate add in 1.5 L water, and 70 ℃ of magnetic agitation 4 h filter, and obtain electrolytic solution, and wherein plumbum ion concentration is 110g/L.Control 55 ℃ of electrolysis temperatures, current density 140 A/m 2, pole span 4 cm, polar plate area 9.7 cm × 9.9 cm, circulation of elecrolyte speed 30 mL/min, when bath voltage is increased to 1.0V, take out positive plate, scrub to put into electrolyzer after the anode sludge and continue electrolysis, and electrolysis time amounts to 24h.Average cell voltage 0.32V, current efficiency 98.93%, negative electrode energy consumption 83.69 kWh/t Pb.The constituent content of negative electrode lead and the anode sludge is respectively in table 1 and table 2.
The foreign matter content (× 10 of table 1 negative electrode lead -6%)
Element Sn Sb Bi As Cu Zn Fe Ag Ni Cd Summation
Negative electrode lead ＜8.9 ＜8.9 2880 15.8 573 ＜8.9 310 ＜8.9 ＜8.9 ＜8.9 ＜3832.2
GB (≤) 500 800 4000 500 1000 400 500 800 - - 6000
The constituent content (%) of table 2 anode sludge
Element Sn Sb Bi As Cu Zn Fe Ag Ni Cd
The anode sludge - 12.28 10.84 33.83 7.188 - 0.464 10.66 0.109 -
As can be seen from Table 1, the foreign matter content in negative electrode lead is very low, and the purity of negative electrode lead is higher, higher than 99.99617%, has reached the standard of Pb99.994 lead pig in GB/T 469-2005.As can be seen from Table 2, the enrichment of element such as silver, bismuth, antimony is in the anode sludge.
Embodiment 2
Plumbous content in lead bullion is 98.10%, and major impurity composition is tin 0.0008%, antimony 0.9106%, bismuth 0.1959%, arsenic 0.5451%, copper 0.0933%, zinc 0.0006%, silver 0.1521%, iron 0.0015%.Tartrate, sodium hydroxide and plumbous oxide are analytical pure.
Take lead bullion 500g, in retort furnace, heat to 650 ℃ of fusing 15min, take out, in graphite jig, be cast into positive plate, be of a size of 10cm × 10cm.
Get 180 g plumbous oxide, 210 g sodium hydroxide, 210 g tartrate add in 1.5 L distilled water, and 80 ℃ of magnetic agitation 4 h, obtain electrolytic solution after filtration, and wherein plumbum ion concentration is 100g/L.Control 45 ℃ of electrolysis temperatures, current density 160 A/m2, pole span 4 cm, polar plate area 9.7 cm × 9.9 cm, electrolytic solution volume 1.5 L, circulation of elecrolyte speed 30 mL/min.When bath voltage is increased to 1.0V, take out positive plate, scrub and put into electrolyzer after the anode sludge and continue electrolysis, electrolysis time amounts to 25h.Average cell voltage 0.39V, current efficiency 98.77%, negative electrode energy consumption 102.16 kWh/t Pb.The constituent content of negative electrode lead and the anode sludge is respectively in table 3 and table 4.
The foreign matter content (× 10 of table 3 negative electrode lead -6%)
Element Sn Sb Bi As Cu Zn Fe Ag Ni Cd Summation
Negative electrode lead ＜9.5 ＜9.5 3100 19.8 540 ＜9.5 335 ＜9.5 ＜9.5 ＜9.5 ＜4042.3
GB (≤) 500 800 4000 500 1000 400 500 800 - - 6000
The constituent content (%) of table 4 anode sludge
Element Sn Sb Bi As Cu Zn Fe Ag Ni Cd
The anode sludge - 14.58 9.431 31.53 6.673 - 0.312 9.85 0.0845 -
As can be seen from Table 3, the purity of negative electrode lead is 99.99596%, has reached the standard of Pb99.994 lead pig in GB/T 469-2005.Can find out by 4, the enrichment of element such as silver, bismuth, antimony are in the anode sludge.
Embodiment 3
Lead content in lead bullion is 98.30%, and major impurity composition is tin 0.0008%, antimony 0.8281%, bismuth 0.1363%, arsenic 0.5127%, copper 0.0795%, zinc 0.0006%, silver 0.1406%, iron 0.0013%.Tartrate, sodium hydroxide and plumbous oxide are analytical pure.
Take lead bullion 500 g, in retort furnace, 600 ℃ of fusing 15 min that heat take out, and are cast into positive plate in graphite jig, are of a size of 10cm × 10cm.
Take 100 g plumbous oxide, 120g sodium hydroxide, 150 g tartrate add in 1.5 L water, and 70 ℃ of magnetic agitation 4 h filter, and obtain electrolytic solution, and wherein plumbum ion concentration is 80g/L.Control 40 ℃ of electrolysis temperatures, current density 100 A/m 2, pole span 4 cm, polar plate area 9.7 cm × 9.9 cm, circulation of elecrolyte speed 8.5 mL/min, when bath voltage is increased to 1.0V, take out positive plate, scrub to put into electrolyzer after the anode sludge and continue electrolysis, and electrolysis time amounts to 24h.Average cell voltage 0.27V, current efficiency 99.15%, negative electrode energy consumption 70.45 kWh/t Pb.The constituent content of negative electrode lead and the anode sludge is respectively in table 5 and table 6.
The foreign matter content (× 10 of table 5 negative electrode lead -6%)
Element Sn Sb Bi As Cu Zn Fe Ag Ni Cd Summation
Negative electrode lead ＜8.9 ＜8.9 1850 12.6 435 ＜8.9 230 ＜8.9 ＜8.9 ＜8.9 ＜2581
GB (≤) 500 800 4000 500 1000 400 500 800 - - 6000
The constituent content (%) of table 6 anode sludge
Element Sn Sb Bi As Cu Zn Fe Ag Ni Cd
The anode sludge - 13.44 10.97 35.27 8.322 - 0.489 10.83 0.112 -
As can be seen from Table 5, the foreign matter content in negative electrode lead is very low, and the purity of negative electrode lead is higher, higher than 99.99741%, has reached the standard of Pb99.994 lead pig in GB/T 469-2005.As can be seen from Table 6, the enrichment of element such as silver, bismuth, antimony is in the anode sludge.
Embodiment 4
Lead content in lead bullion is 98.30%, and major impurity composition is tin 0.0008%, antimony 0.8281%, bismuth 0.1363%, arsenic 0.5127%, copper 0.0795%, zinc 0.0006%, silver 0.1406%, iron 0.0013%.Tartrate, sodium hydroxide and plumbous oxide are analytical pure.
Take lead bullion 500 g, in retort furnace, 600 ℃ of fusing 15 min that heat take out, and are cast into positive plate in graphite jig, are of a size of 10cm × 10cm.
Take 250 g plumbous oxide, 240 g sodium hydroxide, 240 g tartrate add in 1.5 L water, and 70 ℃ of magnetic agitation 4 h filter, and obtain electrolytic solution, and wherein plumbum ion concentration is 130g/L.Control 55 ℃ of electrolysis temperatures, current density 160 A/m 2, pole span 4 cm, polar plate area 9.7 cm × 9.9 cm, circulation of elecrolyte speed 30 mL/min, when bath voltage is increased to 1.0V, take out positive plate, scrub to put into electrolyzer after the anode sludge and continue electrolysis, and electrolysis time amounts to 24h.Average cell voltage 0.38V, current efficiency 98.27%, negative electrode energy consumption 100.05 kWh/t Pb.The constituent content of negative electrode lead and the anode sludge is respectively in table 7 and table 8.
The foreign matter content (× 10 of table 7 negative electrode lead -6%)
Element Sn Sb Bi As Cu Zn Fe Ag Ni Cd Summation
Negative electrode lead ＜8.9 ＜8.9 3250 17.4 698 ＜8.9 421 ＜8.9 ＜8.9 ＜8.9 ＜4749.8
GB (≤) 500 800 4000 500 1000 400 500 800 - - 6000
The constituent content (%) of table 8 anode sludge
Element Sn Sb Bi As Cu Zn Fe Ag Ni Cd
The anode sludge - 11.13 10.62 31.53 6.205 - 0.375 10.35 0.115 -
As can be seen from Table 7, the foreign matter content in negative electrode lead is very low, and the purity of negative electrode lead is higher, higher than 99.99525%, has reached the standard of Pb99.994 lead pig in GB/T 469-2005.As can be seen from Table 8, the enrichment of element such as silver, bismuth, antimony is in the anode sludge.

Claims (1)

1. the method for a performing electrolytic refining on lead bullion, it is characterized by: sodium hydroxide, tartrate are added to the water successively, stirring and dissolving makes mixing solutions at normal temperatures, and the add-on of tartrate and sodium hydroxide is in every liter of mixing solutions, to add 100 ~ 160g tartrate, 80 ~ 160g sodium hydroxide; Then in mixing solutions, adding lead oxide powder, is stirring and dissolving under 40 ~ 98 ℃, the condition of stirring velocity 200 ~ 400r/min in temperature, and time 1 ~ 6h, then filters, and gained filtrate is electrolytic solution; The granularity of described lead oxide powder is less than 200 orders, and in the electrolytic solution preparing, plumbum ion concentration is 110 ~ 130g/L;
The electrolytic solution making is added in electrolyzer, adopt stainless steel plate or pure stereotype as negative electrode, employing treats that the lead bullion of refining makes anode, pass into direct current and carry out electrolysis, concrete electrolytic process parameter is: 40 ~ 60 ℃ of electrolyte temperatures, the circulation of elecrolyte cycle is 45 ~ 120min, and circulation of elecrolyte mode is bottom in and top out, cathode current density 100 ~ 160A/m 2, bath voltage 0.25 ~ 1.0V, anodic current density 100 ~ 160A/m 2, with interpole gap 80 ~ 130mm;
In electrolytic process, rise to 1.0V when bath voltage, while there is anode passivation, take out positive plate and scrub or double teeming positive plate, scrub or double teeming after positive plate return to participation electrolysis;
According to the steam output of electrolytic solution, timing is to make up water in electrolytic solution, to maintain plumbum ion concentration 110 ~ 130g/L in electrolytic solution, sodium hydroxide 80 ~ 160 g/L and tartaric acid concentration 100 ~ 160 g/L;
The dirt settling of collecting on negative electrode is the lead obtaining after refining.
CN201210010362.XA 2012-01-13 2012-01-13 Method for electrolytically refining crude lead Expired - Fee Related CN102534660B (en)

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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
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