CN104711637B - Method for recovering metal lead from solid lead oxide - Google Patents
Method for recovering metal lead from solid lead oxide Download PDFInfo
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- CN104711637B CN104711637B CN201310670718.7A CN201310670718A CN104711637B CN 104711637 B CN104711637 B CN 104711637B CN 201310670718 A CN201310670718 A CN 201310670718A CN 104711637 B CN104711637 B CN 104711637B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/18—Electrolytic production, recovery or refining of metals by electrolysis of solutions of lead
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
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Abstract
The invention relates to a method for recovering metal lead from solid lead oxide. The method is characterized by comprising the following steps: (1) subjecting vulcanized lead concentrate to chlorination leaching, and crystallizing the leachate to obtain solid lead chloride; (2) carrying out first conversion on the solid lead chloride by using calcium oxide to generate basic lead chloride PbOHCl, and then carrying out second conversion between PbOHCl and a sodium hydroxide solution to obtain solid lead oxide; (3) preparing a sodium hydroxide solution as the electrolyte, mixing a proper amount of electrolyte and lead oxide, stirring to obtain paste, evenly painting the paste on a negative electrode plate, installing the negative electrode plate and a positive electrode plate into an electrolysis tank, and carrying out electrolysis; (4) after the electrolysis, peeling off the sponge lead from the negative electrode plate, pressing the sponge lead into balls, and casting the lead balls into lead ingots. The provided method can solve the problems existing in the process of recovering lead from chlorinated leachate of vulcanized lead concentrate through a conversion-solid electrolysis technology, and has the advantages of friendly operation environment, strong operability, high current efficiency, and low production cost.
Description
Technical field
The present invention relates to a kind of method that wet method refines lead, more particularly to a kind of to adopt Solid phase electrolysis reduction technique from oxidation
The method extracted in lead and reclaim metallic lead, belongs to technical field of wet metallurgy.
Background technology
The smelting process of lead has two kinds of pyrogenic process and wet method, and at present in the world based on pyrogenic process, wet method refining lead is still in test
Conceptual phase.As environmental protection increasingly strict and competition in the international market is growing more intense, countries in the world are superseded SO2With lead dust pollution compared with
Substantial amounts of refining lead new technology R＆D work is carried out for serious sintering-blast furnace tradition refining splicer's skill, has successively developed
The direct lead-smelting method such as QSL, Kivcet, Kaldo, Ausmelt, ISA, SKS.These novel techniques for smelting lead eliminate burning
Knot operation, fundamentally solves sintering low concentration SO2Pollution and improvement.However, the pollution of pyrometallurgical smelting of lead is thoroughly eliminated,
Environmental protection and relevant discharge standard and the requirement of Industrial department are reached, is difficult to do from technical pyrometallurgical smelting of lead technique is administered
Arrive.Just because of this, the research of wet method refining splicer's skill is increasingly subject to people's attention.
In recent decades, various countries metallargist has carried out substantial amounts of research to the hydrometallurgy of concentrate of lead sulfide ore, exploitation
The wet processing process of various concentrate of lead sulfide ore, but some techniques are at aspects such as economic and technical norms, adaptability, practical operations
Also exist some it is unsatisfactory where.Such as the direct electrolysis method of concentrate of lead sulfide ore, it is only suitable for processing siliceous low vulcanized lead essence
Ore deposit, needs the lead sponge and anode chamber's ore pulp for periodically processing negative electrode generation in electrolytic process, production is difficult to long-term continuous equilibrium to be carried out.
The non-oxide leaching process of concentrate of lead sulfide ore can produce poisonous H2S gases, are difficult to realize in production.
The Oxidation Leaching technical study of concentrate of lead sulfide ore is more, and the potassium cloride especially with ferric chloride as oxidant is studied most
For abundant, the lab scale of the method and expanding test are more successful.The potassium cloride of concentrate of lead sulfide ore is to change the sulfur in lead concentrate
For elementary sulfur, lead is transformed into intermediate products PbCl2, then, lead is extracted and reclaimed from lead chloride.Extract from lead chloride and return
Receiving the main Technology for adopting of early stage research of lead includes：Lead chloride molten-salt electrolysis, without barrier film lead chloride aqueous solution electrolysises, makes
With the lead chloride aqueous solution electrolysises of anionic membrane, using the lead chloride aqueous solution electrolysises etc. of cationic membrane.However, in above-mentioned electrolysis
In technique, also exist and chlorine separated out on anode, easily cause chlorine to escape and leak, deteriorate operating condition, cause environmental pollution,
And production cost is high, the problems such as process bad control.
For the deficiency that the above-mentioned hydrometallurgic recovery metallic lead technique from lead chloride is present, the present inventor develops one kind chlorine
Change lead and change into the method for lead oxide, and apply for patent of invention（Number of patent application：201210256121.3）.Here research
On the basis of, the present inventor has done and develop lead oxide and be further processed into metallic lead after substantial amounts of test and repeated screening again
Hydrometallurgical processes, i.e., be reduced into lead sponge using Solid phase electrolysis reduction technique by lead oxide, and lead pig is made in lead sponge founding.
The content of the invention
It is an object of the invention to overcome pyrogenic process and existing wet method refining lead technology above shortcomings, for existing from chlorine
Change and reclaim in lead the problem that lead is present, propose a kind of method that metallic lead is reclaimed from lead chloride conversion product-lead oxide.New
Lead-smelting method is that the product lead oxide that lead chloride conversion is obtained is raw material, by Solid phase electrolysis with concentrate of lead sulfide ore potassium cloride
Method lead oxide is reduced into into metallic lead.
The technical solution that the present invention is given is：This employing Solid phase electrolysis technology reclaims metallic lead from lead oxide
Method, is characterized in being made up of following steps.
It is prepared by 1 lead oxide：Concentrate of lead sulfide ore is carried out into potassium cloride, leachate crystallisation by cooling obtains solid chlorine lead；
Then lead chloride is changed into into lead oxide.
（1）First solid chlorine lead and calcium oxide are pressed into liquid-solid ratio=4～7:1 inserts in the conversion tank with stirring, carries out
The first step is converted, reaction equation is：
2PbCl2+CaO+H2O→2PbOHCl↓+CaCl2
Wherein mass ratio=8～10.5 of solid chlorine lead and calcium oxide:1,20～80 DEG C of reaction temperature, the response time is not
Less than 60min.
（2）The mineral yellow (PbOHCl) that the first step is converted into carries out second step and turns with sodium hydroxide solution effect
Change, generate liquid after solid oxidation lead and twice transformation, its chemical equation is：
PbOHCl+NaOH→PbO↓+NaCl+H2O。
In second conversion process, mass ratio=3.85～5 of mineral yellow and sodium hydroxide:1, sodium hydroxide is molten
15～22.5%, 60～85 DEG C of reaction temperature, the response time is not less than 30min to the control of liquid concentration.
2 prepare electrolyte and coated plate：Sodium hydroxide is configured to certain density sodium hydroxide solution as electrolyte；
Mixed with raw material lead oxide with appropriate electrolyte, and stir into paste；The oxidation lead plaster being stirred equably is coated in into panel
On the minus plate of type stainless steel.The material of yin, yang pole plate can be titanium system.
3 electroreductions：The minus plate for coating and stainless steel anode plate are put equipped with electrolyte by suitable pole span
Electrolysis bath in, the material of yin, yang pole plate can select titanium.Connecting yin, yang pole plate power supply carries out the solid phase electricity of lead oxide
Solution.Electrolysis process technical conditions are：In 6～10 %, electrolyte temperature is room temperature～65 DEG C for the concentration control of sodium hydroxide solution,
The A/m of electric current density 400～9002, it is 80～100 mm suitably with pole span scope.The Solid phase electrolysis course of reaction of lead oxide is such as
Under：
Cathode reaction：PbO + H2O + 2e→Pb↓+ 2OH-
Anode reaction：2OH- - 2e→1/2O2↑+ H2O
Solid phase electrolysis overall reaction equation is：PbO→Pb + 1/2O2↑。
4 lead sponges are peeled off and founding：Drastically raise when tank voltage moment, and along generation gas on the liquid level of minus plate
When terminate electrolysis.Minus plate is taken out from electrolysis bath, the lead sponge of precipitation is peeled from minus plate, founding is into lead after briquetting
Ingot.
Compared with wet method refining splicer's skill of the existing direct extraction of metal lead from lead chloride, beneficial effects of the present invention exist
In：
（1）Before electrolysis lead chloride is changed into into lead oxide, not only working environment is friendly, and solves chlorination lead water
Lead chloride is easily crystallized in solution electrolytic process, blocking circulating line the problems such as, it is workable；
（2）Current efficiency is high, and power consumption is low, and lead power consumption per ton can reduce 35kW.h～700kW.h；
（3）Expensive barrier film is not needed in electrolytic process, sodium hydroxide is not consumed, production cost is substantially reduced.
Specific embodiment
In conjunction with embodiment, technical scheme is described in detail.
Embodiment 1.
The potassium cloride of concentrate of lead sulfide ore is carried out first, and leachate crystallisation by cooling obtains solid chlorine lead.Secondly, by solid
Lead chloride, calcium oxide and water carry out first step conversion by certain liquid-solid ratio, and the technical conditions of lead chloride first step conversion are：Chlorine
Change mass ratio=9 of lead and calcium oxide:1, liquid-solid ratio 4:1,60 DEG C of conversion temperature, response time 90min after completion of the reaction, enters
Row solid-liquor separation；The conversion slag PbOHCl that first step conversion is obtained is carried out into second step in certain density sodium hydroxide solution
Conversion, carries out solid-liquor separation after the completion of reaction, obtain converting slag PbO and sodium chloride solution, and the technical conditions of second step conversion are：
Mass ratio=5 of mineral yellow PbOHCl and sodium hydroxide:1, concentration of sodium hydroxide solution 15%, 75 DEG C of conversion reaction temperature,
Response time 75min.Finally, compound concentration be the sodium hydroxide solution of 8 % as electrolyte, with appropriate sodium hydroxide solution
Mixed with lead oxide, stirred into paste, the oxidation lead plaster being stirred equably is coated in the stainless steel of panel type
On minus plate；Load the sodium hydroxide solution for preparing in electrolysis bath, and the minus plate for coating is arrived with stainless steel anode board placing
In electrolysis bath, Solid phase electrolysis technical conditions are：45 DEG C of electrolysis temperature, with the mm of pole span 100, the A/m of electric current density 6002。
As a result：The % of current efficiency 95.07
The V of tank voltage 1.752
The straight electricity kWh.t of unit consumption 477-1 。
Embodiment 2.
The potassium cloride of concentrate of lead sulfide ore is carried out first, and leachate crystallisation by cooling obtains solid chlorine lead.Secondly, by solid
Lead chloride, calcium oxide and water carry out first step conversion by certain liquid-solid ratio, and the technical conditions of lead chloride first step conversion are：Chlorine
Change mass ratio=9 of lead and calcium oxide:1, liquid-solid ratio 5:1,70 DEG C of conversion temperature, response time 120min after completion of the reaction, enters
Row solid-liquor separation；The conversion slag PbOHCl that first step conversion is obtained is carried out into second step in certain density sodium hydroxide solution
Conversion, carries out solid-liquor separation after the completion of reaction, obtain converting slag PbO and sodium chloride solution, and the technical conditions of second step conversion are：
Mass ratio=4 of mineral yellow PbOHCl and sodium hydroxide:1, concentration of sodium hydroxide solution 15%, 75 DEG C of conversion reaction temperature,
Response time 30min.Finally, compound concentration be the sodium hydroxide solution of 10 % as electrolyte, then with appropriate hydroxide
Sodium solution is mixed with lead oxide, stirs into paste, and the oxidation lead plaster being stirred equably is coated in into the rustless steel of panel type
On the minus plate of material；Load the sodium hydroxide solution for preparing in electrolysis bath, and by the minus plate for coating and stainless steel anode plate
Put in electrolysis bath, Solid phase electrolysis technical conditions are：55 DEG C of electrolysis temperature, with the mm of pole span 80, the A/m of electric current density 8002。
As a result：The % of current efficiency 95.12
The V of tank voltage 1.742
The straight electricity kWh.t of unit consumption 474-1 。
Embodiment 3.
The potassium cloride of concentrate of lead sulfide ore is carried out first, and leachate crystallisation by cooling obtains solid chlorine lead.Secondly, by solid
Lead chloride, calcium oxide and water carry out first step conversion by certain liquid-solid ratio, and the technical conditions of lead chloride first step conversion are：Chlorine
Change mass ratio=10 of lead and calcium oxide:1, liquid-solid ratio 4:1,60 DEG C of conversion temperature, response time 120min, after completion of the reaction,
Carry out solid-liquor separation；The conversion slag PbOHCl that first step conversion is obtained is carried out into second in certain density sodium hydroxide solution
Step conversion, carries out solid-liquor separation after the completion of reaction, obtain converting slag PbO and sodium chloride solution, the technical conditions of second step conversion
For：Mass ratio=4.5 of mineral yellow PbOHCl and sodium hydroxide:1, concentration of sodium hydroxide solution 17.5%, conversion reaction temperature
75 DEG C of degree, response time 75min.Finally, compound concentration be the sodium hydroxide solution of 8 % as electrolyte, then with appropriate
Sodium hydroxide solution is mixed with lead oxide, stirs into paste, and the oxidation lead plaster being stirred equably is coated in into panel type
On the minus plate of stainless steel；Load the sodium hydroxide solution for preparing in electrolysis bath, and by the minus plate for coating and rustless steel
To in electrolysis bath, Solid phase electrolysis technical conditions are anode board placing：55 DEG C of electrolysis temperature, with the mm of pole span 80, electric current density 600
A/m2。
As a result：The % of current efficiency 95.16
The V of tank voltage 1.736
The straight electricity kWh.t of unit consumption 472-1 。
Claims (5)
1. a kind of method that employing Solid phase electrolysis technology reclaims metallic lead from lead oxide, it is characterised in that by following steps structure
Into：
（1）It is prepared by lead oxide：Concentrate of lead sulfide ore is carried out into potassium cloride, leachate crystallisation by cooling obtains solid chlorine lead；Then
Using number of patent application：201210256121.3 lead chloride is changed into lead oxide by technology；
（2）Prepare electrolyte and coated plate：Sodium hydroxide is configured to certain density sodium hydroxide solution as electrolyte；With suitable
The electrolyte of amount mixes with raw material lead oxide, and stirs into paste；The oxidation lead plaster being stirred equably is coated in into panel type not
On the minus plate of rust steel matter, as the % of concentration of sodium hydroxide solution 6～10 of electrolyte；
（3）Electroreduction：The minus plate for coating and stainless steel anode plate are put into the electricity equipped with electrolyte by suitable pole span
In solution groove, connecting yin, yang pole plate power supply carries out the Solid phase electrolysis of lead oxide, and electrolysis process technical conditions are：Sodium hydroxide solution
Concentration control in 6～10 %, electrolyte temperature is room temperature～65 DEG C, the A/m of electric current density 400～9002, suitable same pole span
Scope is 80～100 mm；
（4）Lead sponge is peeled off and founding：Drastically raise when tank voltage moment, and along knot when producing gas on the liquid level of minus plate
Beam is electrolysed, and minus plate is taken out from electrolysis bath, and the lead sponge of precipitation is peeled from minus plate, and founding is into lead pig after briquetting；
Wherein step（1）Described in number of patent application：201210256121.3 technology is：
a）First solid chlorine lead and calcium oxide are pressed into liquid-solid ratio=4～7:1 inserts in the conversion tank with stirring, carries out first
Step dechlorination is converted, and reaction equation is：
2PbCl2+CaO+H2O→2PbOHCl↓+CaCl2
Wherein mass ratio=8～10.5 of solid chlorine lead and calcium oxide:1,20～80 DEG C of reaction temperature, the response time is not little
In 1 h；
b）The mineral yellow PbOHCl that first step dechlorination is converted into carries out second step dechlorination with sodium hydroxide solution effect
Conversion, generates solid oxidation lead and sodium chloride solution, and its chemical equation is：
PbOHCl+NaOH→PbO+NaCl+H2O
In second dechlorination conversion process, mass ratio=3.85～5 of mineral yellow and sodium hydroxide:1, sodium hydroxide is molten
The control of liquid concentration is not less than 0.5 h in 15～22.5 %, 60～85 DEG C of reaction temperature, response time.
2. the method that employing Solid phase electrolysis technology according to claim 1 reclaims metallic lead from lead oxide, its feature exists
In step（3）In electrolysis process technical conditions be：The concentration of sodium hydroxide solution is controlled in 8 %, and electrolyte temperature is 45
DEG C, the A/m of electric current density 6002, it is 100 mm with pole span.
3. the method that employing Solid phase electrolysis technology according to claim 1 reclaims metallic lead from lead oxide, its feature exists
In step（3）In electrolysis process technical conditions be：The concentration of sodium hydroxide solution is controlled in 10 %, and electrolyte temperature is 55
DEG C, the A/m of electric current density 8002, it is 80 mm with pole span.
4. the method that employing Solid phase electrolysis technology according to claim 1 reclaims metallic lead from lead oxide, its feature exists
In step（3）In electrolysis process technical conditions be：The concentration of sodium hydroxide solution is controlled in 8 %, and electrolyte temperature is 55
DEG C, the A/m of electric current density 6002, it is 80 mm with pole span.
5. the method that employing Solid phase electrolysis technology according to claim 1 reclaims metallic lead from lead oxide, its feature exists
In step（3）In the material of yin, yang pole plate be titanium system.
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| CN201310670718.7A CN104711637B (en) | 2013-12-12 | 2013-12-12 | Method for recovering metal lead from solid lead oxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110697765A (en) * | 2019-11-26 | 2020-01-17 | 中原工学院 | Room temperature solid phase synthesis method of basic lead chloride material |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106065485B (en) | 2016-07-19 | 2018-12-14 | 云南祥云飞龙再生科技股份有限公司 | A kind of ammonium sulfate ammonia electroreduction produces splicer's skill |
| CN109022817A (en) * | 2018-07-27 | 2018-12-18 | 郴州雄风环保科技有限公司 | The new process of high chlorine lead smelting gas dechlorination |
| CN111575743A (en) * | 2020-05-26 | 2020-08-25 | 中国恩菲工程技术有限公司 | Method for producing metallic lead |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1428957A (en) * | 1972-11-17 | 1976-03-24 | Imi Refinery Holdings Ltd | Electrolytic recovery of lead |
| CN85200287U (en) * | 1985-04-01 | 1985-11-10 | 中国科学院化工冶金研究所 | Electrolyzer for solid state substance containning pb |
| US4650553A (en) * | 1986-03-21 | 1987-03-17 | Pennwalt Corporation | Electrolytic recovery of lead from scrap |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103290225A (en) * | 2013-06-20 | 2013-09-11 | 长沙华明复合材料科技有限公司 | Method for recovering lead from lead-containing solid wastes |
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2013
- 2013-12-12 CN CN201310670718.7A patent/CN104711637B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1428957A (en) * | 1972-11-17 | 1976-03-24 | Imi Refinery Holdings Ltd | Electrolytic recovery of lead |
| CN85200287U (en) * | 1985-04-01 | 1985-11-10 | 中国科学院化工冶金研究所 | Electrolyzer for solid state substance containning pb |
| US4650553A (en) * | 1986-03-21 | 1987-03-17 | Pennwalt Corporation | Electrolytic recovery of lead from scrap |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110697765A (en) * | 2019-11-26 | 2020-01-17 | 中原工学院 | Room temperature solid phase synthesis method of basic lead chloride material |
| CN110697765B (en) * | 2019-11-26 | 2022-04-29 | 中原工学院 | Room temperature solid phase synthesis method of basic lead chloride material |
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Address after: 110141 No. 7, No. 6, No. seven road, Shenyang economic and Technological Development Zone, Shenyang, Liaoning. Patentee after: Shenyang Nonferrous Metal Research Institute Co., Ltd. Address before: 110141 Shenyang Nonferrous Metal Research Institute, No. seven, Shenyang economic and Technological Development Zone, Shenyang, China, No. 7, No. 6, China Patentee before: Shenyang Research Institute of Nonferrous Metals |