CN108754137A - The method that metallic lead is produced using solvent extraction electrodeposition process - Google Patents
The method that metallic lead is produced using solvent extraction electrodeposition process Download PDFInfo
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- CN108754137A CN108754137A CN201810872489.XA CN201810872489A CN108754137A CN 108754137 A CN108754137 A CN 108754137A CN 201810872489 A CN201810872489 A CN 201810872489A CN 108754137 A CN108754137 A CN 108754137A
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- lead
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- electrodeposition
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
-
- 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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
-
- 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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- 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
-
- 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 present invention discloses a kind of method producing metallic lead using solvent extraction electrodeposition process, and step includes：A) lead-containing material is leached by that can generate the lead lysate of soluble lead salt, is filtered, and leaded leachate is made；B) leaded leachate carries out hybrid extraction, layering with extractant, obtains the organic and raffinate of load lead ion；C) the organic of load lead ion is washed using acidic cleaning liquid, is obtained washing rear organic and is washed Hou Shui.D) it washes rear organic use back washing agent to be stripped, obtains regenerating organic and back extraction rich solution；E) organic return to step b) is regenerated to recycle；F) back extraction rich solution obtains liquid before lead electrodeposition by air supporting, activated carbon oil removing；g）Liquid obtains metallic lead by electrodeposition before lead electrodeposition.Using this method from scrap lead battery, Pb-Zn deposits, lead oxide ore, the lead containing sludge of low taste complexity, leaded sludge separation and Extraction lead, have many advantages, such as simple for process, equipment investment is low, operating cost is low, cleaning, it is efficient.
Description
Technical field
It is especially a kind of that metallic lead is produced using solvent extraction electrodeposition process the present invention relates to the technique of extraction and separation lead
Method.
Background technology
Currently, the smelting mode of lead is nearly all pyrometallurgical smelting, to obtain lead bullion, obtained often by pyrometallurgical smelting
Lead bullion, then obtained lead bullion refined, is electrolysed to obtain lead bullion.Lead bullion is prepared using this method, not only long flow path, energy consumption
Height, and equipment investment is big, production cost is high.
In recent years, also there are many scholars to study the hydrometallurgy of lead, and develop a kind of leaching of alkali, removal of impurities,
Electrodeposition process prepares electric lead, this method by sodium hydroxide alkali soak in the way of lead dissolved to be formed containing lead solution, use later
Lead powder removes the impurity in solution, and the electric lead that purity is higher than 97% is obtained finally by electrodeposition.This method prepares electric lead, first
First due to being cleaned using lead powder, the metal ions such as some remaining alkalinous metals and zinc cannot be removed well in solution
It goes, leading to the recycling of solution, there are the qualities of problem and electric lead can only achieve 97% or more, does not arrive 99.94% or more；
Secondly, if containing zinc in raw material, zinc will also dissolve out under alkaline condition, then this method cannot be applicable in；If in addition, containing in raw material
The anion of some soluble-salts, these salt institute bands will enter in solution, and the separation of anion will be extremely difficult.
Invention content
In view of the deficiencies of the prior art, the present invention proposes a kind of side producing metallic lead using solvent extraction electrodeposition process
Method is not only able to obtain the lead of high-quality, and this method adaptability to raw material is strong, technological operation is simple and production cost is low.
To achieve the above object, the present invention provides following technical solutions：
A method of metallic lead being produced using solvent extraction electrodeposition process, which is characterized in that the method and step includes：
A) lead-containing material is leached by that can generate the lead lysate of soluble lead salt, is filtered, and leaded leachate is made；
B) the leaded leachate that above-mentioned steps a) is obtained carries out hybrid extraction, layering with extractant, obtains having for load lead ion
Machine and raffinate；
C) the load lead ion that above-mentioned steps b) is obtained is organic, is washed using acidic cleaning liquid, obtain washing it is rear it is organic with
And wash Hou Shui.
It is rear organic that d) above-mentioned steps c) was obtained wash, and is stripped using back washing agent, obtains regenerating organic and back extraction rich
Liquid；
E) the organic return to step b) of regeneration that above-mentioned steps d) is obtained is recycled；
F) the back extraction rich solution that above-mentioned steps d) is obtained obtains liquid before lead electrodeposition by air supporting, activated carbon oil removing；
g）Above-mentioned steps f）Liquid obtains metallic lead by electrodeposition before obtained lead electrodeposition.
Preferably, in step a), lead lysate is one or more in hydrochloric acid, nitric acid, sodium chloride and ammonium chloride；It is leaded
The composition of material be lead oxide, ceruse, lead chloride, lead hydroxide or scrap lead in it is one or more when, directly with lead dissolve
Liquid reaction generates soluble lead salt；When raw material is lead sulfate, then need first sodium carbonate or sodium hydroxide to be used to carry out instead with lead sulfate
It answers, lead sulfate is made to be converted into ceruse or lead hydroxide and then carry out reacting the soluble lead salt of generation with lead lysate.
Preferably, in step b), used extractant is acidic extractant.
Preferably, in step c), the acidic cleaning liquid includes one in acetate solution, hydrochloric acid solution, nitric acid liquid, methylsulphur acid solution
Kind or a variety of carry out proportioning combination.
Preferably, in step d), back washing agent is using acetic acid, nitric acid, fluoboric acid, fluosilicic acid, one kind in methanesulfonic acid or more
Kind carries out proportioning combination.
Preferably, the lead-containing material includes Pb-Zn deposits, lead oxide ore, waste lead accumulator, low taste complexity containing lead skim
One or more of with leaded sludge.
Advantages of the present invention is：Adaptability to raw material is strong, technological operation is simple, production cost is low, equipment investment is few.
Description of the drawings
Process flow chart of the separation containing the lead in lead skim, sludge and Pb-Zn deposits that Fig. 1 is provided by the present embodiment；
The process flow chart of lead in the separation lead sulfate that Fig. 2 is provided by the present embodiment；
Another process flow chart of lead in the separation lead sulfate that Fig. 3 is provided by the present embodiment.
Specific implementation mode
The present invention is made further using the method that solvent extraction electrodeposition process produces metallic lead by Fig. 1 to Fig. 3
It is bright.
A method of metallic lead being produced using solvent extraction electrodeposition process, which is characterized in that step includes：
A) lead-containing material leached by that can generate the lead lysate of lead soluble-salt, filtered, leaded leachate is made.
In the present embodiment, the lead-containing material includes Pb-Zn deposits, lead oxide ore, waste lead accumulator, low taste complexity containing lead skim and contains
One or more of lead sludge；Lead lysate is one or more therefore leaded in hydrochloric acid, nitric acid, sodium chloride and ammonium chloride
Lead chloride, plumbi nitras can be obtained in leachate；It should be noted that lead lysate is not limited to above-mentioned several, the present embodiment
In, as long as the material of lead soluble-salt can be formed with lead；When carrying out extraction and separation to lead sulfate according to this method, then
It need to first be reacted with lead sulfate using sodium carbonate or sodium hydroxide, lead sulfate is made to be converted into after ceruse or lead hydroxide,
It carries out reacting the soluble lead salt of generation with lead lysate again.
B) the leaded leachate for obtaining step a) and extractant progress hybrid extraction, 20 DEG C~45 DEG C of the temperature of extraction,
After shaking 1~10min of time, stratification obtains organic, the raffinate of load lead ion；Obtained raffinate is extracting it
After his metal, returns to extracting stage and recycle；Extractant is acidic extractant in the present embodiment, and the control of acid extract agent content exists
10%~40%, diluent is using sulfonated kerosene, alkane solvent etc..
C) the load lead ion that step b) is obtained is organic, is washed using acidic cleaning liquid, obtain washing it is rear it is organic with
And Hou Shui is washed, it washes rear water return to step a) and uses；It is one or more in acetic acid, hydrochloric acid, nitric acid, methanesulfonic acid in the present embodiment
Configured in proportion, by the foreign ion of organic middle extraction, such as zinc, cadmium, calcium, copper, magnesium, iron and the extraction stoste of entrainment into
Row washing ensures into the organic pure of stripping section.
D) rear organic use back washing agent of washing that step c) is obtained is stripped, obtains regenerating organic and back extraction rich solution,
Comparing for back extraction is adjusted, control rich solution is leaded in 100~200g/l；The strip liquor uses acetic acid, nitric acid, the fluorine boron of high concentration
One or more in acid, fluosilicic acid, methanesulfonic acid are matched.
E) the organic return to step b) of regeneration that step d) is obtained is recycled.
F) the back extraction rich solution that step d) is obtained obtains liquid before lead electrodeposition by air supporting, activated carbon oil removing.
g）Above-mentioned steps f）Liquid obtains metallic lead by electrodeposition before obtained lead electrodeposition.
The present invention is to realize that the extraction to lead, extraction (1), back extraction (2) Principle of Process are as follows using acidic extractant：
2RH+Pb2+→R2Pb + 2H+ (1)
R2Pb + 2H+→2RH+Pb2+ (2)
In extraction process, pH under, realizes organic not saponification and directly extracts lead ion, single-stage extraction rate can in neutrallty condition
To reach 90% or more.
In stripping process, it is stripped to organic using the acid of high equivalent weight, by the proportion adjustment of organic phase and water phase,
Realize the enrichment of lead ion.
It is two concrete operations below：
Embodiment 1：
Leaded 20% is leached containing lead skim, leaded sludge, smelting charge of lead and zinc by hydrochloric acid, is filtered, leaded leachate is made,
By the liquid and extractant hybrid extraction, 3min is shaken, obtains the organic of load lead ion, this is organic to be washed by acidic cleaning liquid
Afterwards, it is stripped to obtain the leaded rich solution in 150g/L using back washing agent.The rich solution of the lead obtains after carrying out activated carbon oil removing
Liquid before lead electrodeposition of the oil-containing less than 5ppm.Liquid obtains metallic lead by electrodeposition before the electrodeposition.Extraction lead raffinate carries out other metals
Such as：After copper, cadmium, zinc, cobalt, nickel extraction and separation, returns and leach recycling.In above-described embodiment, acidic cleaning liquid by lead acetate,
Nitric acid forms, and back washing agent is made of nitric acid, acetic acid and methylsulphur acid solution.
Embodiment 2：
After the material of sulfur-bearing lead plumbate is leached by sodium carbonate liquor, detached, metabisulfite solution and carbonic acid are respectively obtained
Lead precipitates, and metabisulfite solution prepares saltcake by evaporative crystallization, and ceruse is leached using hydrochloric acid, filtered, and leaded leaching is made
Go out liquid；By the leaded leachate and extractant hybrid extraction, 5min is shaken, obtains the organic of load lead ion, this is organic to pass through
After acidic cleaning liquid washing, it is stripped to obtain the leaded rich solution in 150g/L using back washing agent.The lead rich solution carries out activated carbon
After oil removing, liquid before lead electrodeposition of the oil-containing less than 10ppm is obtained, liquid obtains metallic lead by electrodeposition before the electrodeposition.Extract lead raffinate
Carry out other metals such as：After copper, cadmium, zinc, cobalt, nickel extraction and separation, returns and leach recycling.In above-described embodiment, acidity is washed
It washs liquid to be made of nitric acid, methanesulfonic acid, back washing agent is made of nitric acid, acetic acid, methylsulphur acid solution.
In conclusion by the Solvent Extraction Separation lead, compared to traditional method：
First, low taste lead skim, leaded sludge, the Pb-Zn deposits etc. that can not largely comprehensively utilize are allowed in wet lead-zinc method smelting process
The higher raw material containing other impurities has obtained comprehensive comprehensive utilization, improves the added value of lead；
Secondly, the purification process of solution is eliminated, is stripped by extracting, keeps lead strip liquor very pure, without other metals sun
The anion that the raw materials such as ion and fluorine, chlorine are brought into so that the production lead that later process is obtained by electrodeposition can reach national standard
It is required that in addition the technique can also reduce the production cost of electric lead；
Third, the wet processing compared with pyrometallurgical smelting for, there is very strong environmentally friendly competitiveness, the nothing of lead smelting process may be implemented
Waste water, heavy metal free soot emissions.
The present invention has as a result,：The advantages such as adaptability to raw material is strong, with good investment, flow is short, low energy consumption, operating cost is low.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (6)
1. a kind of method producing metallic lead using solvent extraction electrodeposition process, which is characterized in that the method and step includes：
A) lead-containing material is leached by that can generate the lead lysate of soluble lead salt, is filtered, and leaded leachate is made；
B) the leaded leachate that above-mentioned steps a) is obtained carries out hybrid extraction, layering with extractant, obtains having for load lead ion
Machine and raffinate；
C) the load lead ion that above-mentioned steps b) is obtained is organic, is washed using acidic cleaning liquid, obtain washing it is rear it is organic with
And wash Hou Shui；
It is rear organic that d) above-mentioned steps c) was obtained wash, and is stripped using back washing agent, obtains regenerating organic and back extraction rich solution；
E) the organic return to step b) of regeneration that above-mentioned steps d) is obtained is recycled；
F) the back extraction rich solution that above-mentioned steps d) is obtained obtains liquid before lead electrodeposition by air supporting, activated carbon oil removing；
g）Above-mentioned steps f）Liquid obtains metallic lead by electrodeposition before obtained lead electrodeposition.
2. the method according to claim 1 that metallic lead is produced using solvent extraction electrodeposition process, it is characterized in that：Step
A) in, lead lysate is one or more in hydrochloric acid, nitric acid, sodium chloride and ammonium chloride；The composition of lead-containing material be lead oxide,
When one or more in ceruse, lead chloride, lead hydroxide or scrap lead, directly reacted with lead lysate and generate dissoluble lead
Salt；When raw material is lead sulfate, then needs first sodium carbonate or sodium hydroxide to be used to be reacted with lead sulfate, lead sulfate is made to be converted into carbon
Lead plumbate or lead hydroxide and then react the soluble lead salt of generation with lead lysate.
3. the method according to claim 1 that metallic lead is produced using solvent extraction electrodeposition process, it is characterized in that：Step b)
In, used extractant is acidic extractant.
4. the method according to claim 1 that metallic lead is produced using solvent extraction electrodeposition process, it is characterized in that：Step c)
In, the acidic cleaning liquid is using including one or more progress in acetate solution, hydrochloric acid solution, nitric acid liquid, methylsulphur acid solution
Proportioning combination.
5. the method according to claim 1 that metallic lead is produced using solvent extraction electrodeposition process, it is characterized in that：Step d)
In, back washing agent is that acetic acid, nitric acid, fluoboric acid, fluosilicic acid, one or more in methanesulfonic acid carry out proportioning combination.
6. the method according to claim 1 that metallic lead is produced using solvent extraction electrodeposition process, it is characterized in that：Described
Lead-containing material include Pb-Zn deposits, lead oxide ore, waste lead accumulator, low taste complexity containing in lead skim and leaded sludge it is a kind of with
On.
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| CN201810872489.XA CN108754137A (en) | 2018-08-02 | 2018-08-02 | The method that metallic lead is produced using solvent extraction electrodeposition process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109626632A (en) * | 2018-12-18 | 2019-04-16 | 江苏永葆环保科技有限公司 | A kind of method of leaded waste acid recycling |
| CN112501451A (en) * | 2020-11-13 | 2021-03-16 | 桐乡市思远环保科技有限公司 | Method for producing metallic lead by adopting solvent extraction electrodeposition process |
| WO2023191737A1 (en) * | 2022-03-31 | 2023-10-05 | İlbak Holdi̇ng Anoni̇m Şi̇rketi̇ | A method for obtaining zn and pb metals from zn-pb ore |
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| CN104039991A (en) * | 2012-11-13 | 2014-09-10 | 巴斯夫欧洲公司 | Recovering lead from a mixed oxidized material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109626632A (en) * | 2018-12-18 | 2019-04-16 | 江苏永葆环保科技有限公司 | A kind of method of leaded waste acid recycling |
| CN112501451A (en) * | 2020-11-13 | 2021-03-16 | 桐乡市思远环保科技有限公司 | Method for producing metallic lead by adopting solvent extraction electrodeposition process |
| WO2023191737A1 (en) * | 2022-03-31 | 2023-10-05 | İlbak Holdi̇ng Anoni̇m Şi̇rketi̇ | A method for obtaining zn and pb metals from zn-pb ore |
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Application publication date: 20181106 |