CN108893616A - A kind of method of chlorination lead skim wet clean processes - Google Patents
A kind of method of chlorination lead skim wet clean processes Download PDFInfo
- Publication number
- CN108893616A CN108893616A CN201810766208.2A CN201810766208A CN108893616A CN 108893616 A CN108893616 A CN 108893616A CN 201810766208 A CN201810766208 A CN 201810766208A CN 108893616 A CN108893616 A CN 108893616A
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- Prior art keywords
- lead
- chlorination
- electrodeposition
- anode
- lead skim
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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
- 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
- C22B7/04—Working-up slag
-
- 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
A kind of method of chlorination lead skim wet clean processes, includes the following steps：Step 1：The coordination of chlorination lead skim is leached, and is that coordination leaching agent carries out coordination leaching to chlorination lead skim with ammonium acetate solution, is separated by solid-liquid separation after leaching, obtains the leachate and leached mud containing lead source；Step 2：Leachate diaphragm electrodeposition extracts lead, and the leachate containing lead source that step 1 is obtained carries out diaphragm electrodeposition as anolyte using ammonium chloride solution and extract lead as catholyte；Step 3：It is electrolysed stripped solution to post-process, after electrodeposition, the catholyte stripped solution return that cathode chamber obtains is used to leach, return step two is used as anolyte after neutralizer adjustment pH is added in the indoor anode electrolysis stripped solution of anode.This method can carry out clean and effective processing to all kinds of chlorination lead skims, directly obtain the higher electric lead product of purity.The present invention has outstanding advantages of adaptability to raw material is strong, process flow is simple and clean and environmental protection.
Description
Technical field
The invention belongs to field of hydrometallurgy, and in particular to a kind of method of chlorination lead skim wet clean processes.
Background technique
Lead, bismuth smelting industry often produce a large amount of chlorination lead skims, wherein containing during carrying out the Refining of lead, bismuth
Lead is usually 60~70%.In addition, often going back argentiferous, bismuth and copper etc. in chlorination lead skim, grade is also usually higher, has and returns well
Receive utility value.
At present the method for lead chloride Slag treatment be mainly use reverberatory furnace 950~1250 DEG C at a temperature of, add lime to make chlorine
Change calcium slag and reduction coal is added to carry out reduction melting to lead therein, produces leaded 97% or so lead bullion and be thus enriched with other
Valuable metal.But chlorination lead skim often generates a large amount of chlorine in this fusion process and overflows, not only take away the valuable metals such as lead, silver,
It reduces it and smelts direct yield, and have heavy corrosion to burner hearth and steel smoke pipe, while chlorine also can seriously pollute big compression ring
Border.With the continuous improvement of Environmental protection, a kind of cleaning, efficient chlorination lead skim cleaning treatment technique are developed
With important energy economy & environment effect.
Summary of the invention
The technical problem to be solved by the present invention is in view of the deficiencies of the prior art, provide a kind of achievable chlorination lead skim
Cleaning, the high efficiente callback of middle lead, the method for the chlorination lead skim wet clean processes of the efficiently concentrating of Yi Jiyin, bismuth, copper etc..
The technical solution adopted by the present invention to solve the technical problems is：A kind of side of chlorination lead skim wet clean processes
Method includes the following steps：
Step 1：The coordination of chlorination lead skim is leached
It is that coordination leaching agent carries out coordination leaching to chlorination lead skim with ammonium acetate solution, is separated by solid-liquid separation, obtains after leaching
To leachate and leached mud containing lead source；
Step 2：Leachate diaphragm electrodeposition extracts lead
The leachate containing lead source that step 1 is obtained is as catholyte, using ammonium chloride solution as anode electrolysis
Liquid carries out diaphragm electrodeposition and extracts lead；
Step 3：It is electrolysed stripped solution post-processing
After electrodeposition, the catholyte stripped solution return that cathode chamber obtains is used to leach, the indoor anode electricity of anode
Return step two is used as anolyte after neutralizer adjustment pH is added in solution stripped solution.
Further, in step 1, the amount of ammonium acetate is that the lead in chlorination lead skim is formed lead acetate ammonium in ammonium acetate solution
1~5 times of required theoretical amount.
Further, in step 1, the solid-liquid quality volume of chlorination lead skim and ammonium acetate solution is 1:3~9, unit g:
ml。
Further, in step 1, extraction temperature is 20~90 DEG C, and preferably 50~80 DEG C, extraction time is 30~180min,
It is preferred that 60~120 DEG C.
Further, in step 1, calcium lignosulfonate, the wood of 0.1~0.5wt% of chlorination lead skim need to be added in coordination when leaching
The mixture of one or both of quality sodium sulfonate.
Further, in step 2, when diaphragm electrodeposition, current density 50A/m2~500A/m2, preferably 150A/m2~
400A/m2, temperature is 20~80 DEG C, preferably 40~60 DEG C, heteropolar away from for 3~12cm, electrodeposition period >=20h/ times.
Further, in step 2, anode is paliform anode when electrodeposition, and the paliform anode is made of n root fence stick,
N >=2, the spacing of any adjacent two fence stick are 1~3cm.
Further, in step 2, when electrodeposition cathode be graphite plate, titanium plate, plating ruthenium titanium plate, stainless steel plate, in Lead initiated plate electrode
One kind；Anode is one of graphite, titanium, plating ruthenium titanium；Diaphragm is anionic membrane.
Further, in step 2, the concentration of ammonium chloride is 1~6mol/L in anolyte.
Further, in step 3, after electrodeposition, ammonium hydroxide is added and adjusts the pH value of anode stripped solution to step 2 interval
The initial pH value of anolyte before film electrodeposition.
The present invention has that " metal recovery rate is low, at high cost, pollution for existing chlorination lead skim pyrogenic process, wet processing process
Weight " status, propose it is a kind of with acetate ion be extraction chlorination lead skim in lead " carrier ", both realized lead in chlorination lead skim
Selectively leaching, while again can be by efficiently concentratings such as silver, bismuth, copper in chlorination lead skim.Obtained lead acetate leachate passes through spy
Fixed diaphragm electrolysis system electrolysis and electrolysis stripped solution post-processing, while can directly obtaining electric lead again can electrolyte circulation again
Raw reuse, the closed cycle of implementation process.
The technology of the present invention principle：Preferably go out ammonium acetate first and cooperates infusion solution system, it on the one hand will be in chlorination lead skim
Pb2+Leaching is converted into stable Pb (Ac)i 2-i(i=1,2,3,4) ion, on the other hand, with Ag, Bi, Cu etc. in chlorination lead skim
It is then hardly leached and is retained in leached mud due to the package action of the lignosulfonates of addition, not only realize it
Separated with a step of lead, and realize the enrichment in slag well, be conducive to next step classification extract, furthermore every
When film electrodeposition, the lignosulfonates of addition obtain fine and close smooth cathode lead to the inhibition of lead " whisker " and also function to crucial work
With.
Meanwhile Pb when, conventional electrolysis more for lead transition-metal ions2+Oxidation reaction easily occurs in anode and forms indissoluble PbOxResistance
The problem of hindering reaction to carry out, the present invention propose to use Diaphragm Electrolysis Technology by Pb (Ac)i 2-i(i=1,2,3,4) it is coordinated leachate
Directive is electrolysed to obtain high-purity electricity lead product, and anode surface is without Pb2+The generation of oxidation reaction, it is easily raw that there is no conventional methods
At PbOxThe problem of leading to anodic passivity and electrodeposition recycling lead can not be continued.In addition, being found by lot of experiments, using spy
The paliform anode of setting shape, anode surface PbO when being also beneficial to avoid being electrolysedxGeneration.In the present invention, anode reaction is：
4OH-- 4e=2H2O+O2, rather than generate the 2Cl of chlorine-- 2e=Cl2；Anode electrolysis stripped solution is added suitable ammonium hydroxide and adjusts pH
After value, and ammonium chloride solution is regenerated, can be directly used for anolyte of next stage when mentioning lead as diaphragm electrodeposition.
In the present invention, leaching rate >=98% of lead, purity >=99.9% of the electricity lead as obtained by diaphragm electrodeposition extraction lead.
The present invention uses lead in ammonium acetate+lignosulfonates cooperation Leaching Systems alternatively property recycling chlorination lead skim
Effectively " carrier ", and by continuously improving to handling each operation stage, make its mutual cooperation, it is all linked with one another.
Specific embodiment
The invention will be further described with reference to embodiments, but the present invention is not limited to the following embodiments.
Embodiment 1
Hunan company provide lead chloride slag ingredient and content (mass percent) be：Pb 71.3%, Cu 1.1%,
Bi 0.22%, Sb 0.37%, As 0.13%, Cl-26.7%, Ag 833g/t.
Take chlorination lead skim 1000g, configuration 5L ammonium acetate solution is that leachate carries out coordination leaching to it, and when leaching is added
The calcium lignosulfonate of 2g is into leachate.The amount of ammonium acetate is that the lead in the chlorination lead skim is formed acetic acid in ammonium acetate solution
2 times of theoretical amount needed for lead ammonium.Extraction temperature is 50 DEG C, extraction time 90min.Solid-liquor separation after leaching, analysis filter
Pb in liquid2+Concentration, calculate its leaching rate be 99.2%, analyze leachate in Cu, Bi, Sb, As and Ag concentration, find it
It is not almost leached.Obtained leachate 4.97L is all pumped into the cathode chamber in diaphragm cell as catholyte
Liquid, the ammonium chloride solution 5.0L in addition configuring 3.5mol/L is that anolyte carries out anion membrane electrodeposition extraction lead.Diaphragm electrodeposition
When current density be 150A/m2, 30 DEG C of temperature, heteropolar away from 5cm, Lead initiated plate electrode is cathode, and anode is to be pressed from both sides to join through copper by 4 graphite rods
Tie the paliform anode of composition, rodlike fence spacing 1cm.Diaphragm electrodeposition is for 24 hours with this condition.It is obtained after electrolysis in cathode
The fine and close smooth electric lead of pattern, current efficiency 98.2%.The purity of gained electricity lead is 99.92%.Tank voltage in electrolytic process
It maintains always to stabilize to 2.1~2.3V, anode surface is also precipitated without solid product.
Embodiment 2
Yunnan company provide lead chloride slag ingredient and content (mass percent) be：Pb 66.8%, Cu 1.9%,
Bi 0.91%, Sb 0.57%, As 0.22%, Cl-25.0%, Ag 1135g/t.
Take chlorination lead skim 1000g, configuration 6L ammonium acetate solution is that leachate carries out coordination leaching to it, and when leaching is added
The sodium lignin sulfonate of 4g is into leachate.The amount of ammonium acetate is that the lead in the chlorination lead skim is formed acetic acid in ammonium acetate solution
4.5 times of theoretical amount needed for lead ammonium.Extraction temperature is 80 DEG C, extraction time 160min.Solid-liquor separation after leaching, analysis
Pb in filtrate2+Concentration, calculate its leaching rate is 98.8%, analyze the concentration of Cu, Bi, Sb, As and Ag etc. in leachate, hair
Existing its is not almost leached.Obtained leachate 5.89L is all pumped into the cathode chamber in diaphragm cell as cathode
Electrolyte, the ammonium chloride solution 6.0L in addition configuring 5mol/L is that anolyte carries out anion membrane electrodeposition extraction lead.Diaphragm electricity
Current density is 450A/m when product2, temperature 50 C is heteropolar away from 8cm, and stainless steel plate is cathode, and anode is to be passed through by 3 plating ruthenium titanium sticks
Copper folder is coupled the paliform anode of composition, rodlike fence spacing 2.5cm.Diaphragm electrodeposition is for 24 hours with this condition.After electrolysis
Cathode obtains the fine and close smooth electric lead of pattern, current efficiency 99.0%.The purity of gained electricity lead is 99.95%.Electrolytic process
Middle tank voltage maintains to stabilize to 2.1~2.5V always, and anode surface is also precipitated without solid product.
Embodiment 3
Chlorination lead skim 1000g in Example 1 takes the catholyte stripped solution 5L in embodiment 2 as above as leaching
The calcium lignosulfonate of 3g is added when leaching into leachate for liquid.Extraction temperature is 30 DEG C, extraction time 60min.Leach knot
Solid-liquor separation after beam analyzes Pb in filtrate2+Concentration, calculate its leaching rate be 98.1%, analyze leachate in Cu, Bi, Sb,
The concentration of As and Ag finds that it is not almost leached.Obtained leachate 4.96L is all pumped into diaphragm cell
Cathode chamber takes the anode electrolysis stripped solution 5L in embodiment 2 as above, is charged with ammonium hydroxide and adjusts its pH as catholyte
It is worth to the initial pH value (pH 5.0) of its anolyte before diaphragm electrodeposition.Later by the solution for having adjusted after pH value be pumped into every
Anode chamber in membrane electrolysis cells carries out diaphragm electrodeposition as anolyte and extracts lead.Current density is 250A/ when diaphragm electrodeposition
m2, 30 DEG C of temperature, heteropolar away from 5cm, plating ruthenium titanium plate is cathode, and anode is to be coupled the paliform formed sun through copper folder by 5 studs
Pole, rodlike fence spacing 1.5cm.Diaphragm electrodeposition 20h with this condition.It is fine and close smooth in cathode acquisition pattern after electrolysis
Electric lead, current efficiency 99.3%.The purity of gained electricity lead is 99.92%.Tank voltage maintains to stabilize to always in electrolytic process
2.1~2.5V, anode surface are also precipitated without solid product.
Comparative example 1
Other conditions are identical as above-described embodiment 1, the ammonium acetate in leaching agent only changed into calcium acetate, after leaching
Solid-liquor separation analyzes Pb in filtrate2+Concentration, calculate to obtain its leaching rate only 51.1%.
Comparative example 2
Other conditions are identical as above-described embodiment 1, the ammonium acetate in leaching agent only changed into sodium acetate, after leaching
Solid-liquor separation analyzes Pb in filtrate2+Concentration, calculate to obtain its leaching rate only 53.5%.
Comparative example 3
Other conditions are identical as above-described embodiment 1, and calcium lignosulfonate or wooden is not only added in leachate when leaching
Plain sodium sulfonate.Solid-liquor separation after leaching analyzes Pb in filtrate2+Concentration, calculate its leaching rate be 98.1%, but analyze
The concentration of Cu, Bi, Sb, As and Ag in solution find the leaching rate of Cu, As, Ag more than 20%.The electric lead that diaphragm electrodeposition obtains
In also detect that Cu, As, Ag impurity, electric lead grade 98.52%.
Comparative example 4
Other conditions are same as Example 1, and only when diaphragm electrodeposition, current density is set as 600A/m2.It is electric with this condition
Cathode surface has bubble generation when product, is judged as and liberation of hydrogen side reaction occurs.And anode also has a small amount of chlorine to be precipitated, and slot pressure is rapid
It is increased to 4.0V or more；Cathode generation is not loose porous fine and close, is easy to fall off from cathode surface.After electrodeposition 6h, cathode can not be at
Fine and close plate, current efficiency are determined to 71.4%.
Comparative example 5
Other conditions are same as Example 1, and only obtained leachate is all pumped into plain electrolysers as electrolysis
Liquid carries out direct current electrodeposition and extracts lead.But experiment discovery, with this condition only electrodeposition arrive 2h when, due to anode surface be precipitated largely it is brown
Color oily insoluble matter causes slot pressure constantly to increase, and the brown insoluble matter is increasing with the extension of electrodeposition time, is accumulated in
Near anode and cathode, so that anode and cathode is short-circuit and causes electrodeposition that can not go on.Collect cathode product drying weighing, analyze its at
Point calculate to obtain cathode efficiency only 45.2%.
Comparative example 6
Other conditions are same as Example 1, only use common graphite plate for anode in diaphragm electrodeposition.With this condition
When diaphragm electrodeposition is to 10h, it can obviously be observed in anode plate surface and be covered with one layer of brown insoluble matter, slot pressure electricity by just
2.1V when product rises to 3.5V.When continuing electrodeposition, slot pressure continues to increase, and anode surface brown insoluble matter increases aggravation, cathode table
Face is precipitated lead pattern and runs down, and can only stop electrodeposition reaction.Cathode product drying analysis is collected, cathode efficiency is calculated to obtain
67.6%.
Comparative example 7
Other conditions are same as Example 1, and anode is to be joined by two graphite rods by copper conductive clip when being only diaphragm electrodeposition
Paliform anode made of knot, graphite rod spacing are 5cm.When diaphragm electrodeposition is to 12h with this condition, can in anode plate surface
It obviously observes and is covered with one layer of brown insoluble matter, 2.1V of the slot pressure by just when electrodeposition rises to 3.5V.When continuing electrodeposition, slot
Pressure continues to increase, and anode surface brown insoluble matter increases aggravation, and cathode surface is precipitated lead pattern and runs down, and can only stop electrodeposition
Reaction.Cathode product drying analysis is collected, cathode efficiency 78.1% is calculated to obtain.
Claims (10)
1. a kind of method of chlorination lead skim wet clean processes, which is characterized in that include the following steps：
Step 1：The coordination of chlorination lead skim is leached
It is that coordination leaching agent carries out coordination leaching to chlorination lead skim with ammonium acetate solution, is separated by solid-liquid separation, is contained after leaching
The leachate and leached mud of lead source；
Step 2：Leachate diaphragm electrodeposition extracts lead
The leachate containing lead source that step 1 is obtained as catholyte, using ammonium chloride solution as anolyte into
Row diaphragm electrodeposition extracts lead；
Step 3：It is electrolysed stripped solution post-processing
After electrodeposition, the catholyte stripped solution return that cathode chamber obtains is used to leach, the indoor anode electrolysis of anode is poor
Change return step two after neutralizer adjustment pH is added in liquid to use as anolyte.
2. the method for chlorination lead skim wet clean processes according to claim 1, it is characterised in that：In step 1, acetic acid
The amount of ammonium acetate is 1~5 times of theoretical amount needed for the lead in chlorination lead skim is formed lead acetate ammonium in ammonium salt solution.
3. the method for chlorination lead skim wet clean processes according to claim 2, it is characterised in that：In step 1, chlorination
The solid-liquid quality volume of lead skim and ammonium acetate solution is 1:3~9, unit g:ml.
4. the method for chlorination lead skim wet clean processes according to claim 3, it is characterised in that：In step 1, leach
Temperature is 20~90 DEG C；Extraction time is 30~180min.
5. the method for chlorination lead skim wet clean processes described in -4 any claims according to claim 1, which is characterized in that
In step 1, the calcium lignosulfonate of 0.1~0.5wt% of chlorination lead skim need to be added, in sodium lignin sulfonate in coordination when leaching
One or two kinds of mixtures.
6. the method for chlorination lead skim wet clean processes described in -4 any claims according to claim 1, it is characterised in that：
In step 2, when diaphragm electrodeposition, current density 50A/m2~500A/m2, temperature is 20~80 DEG C, it is heteropolar away from for 3~12cm,
The electrodeposition period >=20h/ times.
7. the method for chlorination lead skim wet clean processes according to claim 6, it is characterised in that：In step 2, electrodeposition
When anode be paliform anode；The paliform anode is made of n root fence stick, n >=2, between any adjacent two fence stick
Away from for 1~3cm.
8. the method for chlorination lead skim wet clean processes according to claim 7, it is characterised in that：In step 2, electrodeposition
When cathode be graphite plate, titanium plate, plating ruthenium titanium plate, stainless steel plate, one of Lead initiated plate electrode；Anode is graphite, titanium, plates in ruthenium titanium
One kind；Diaphragm is anionic membrane.
9. the method for chlorination lead skim wet clean processes according to claim 8, it is characterised in that：In step 2, anode
The concentration of ammonium chloride is 1~6mol/L in liquid.
10. the method for chlorination lead skim wet clean processes according to claim 9, it is characterised in that：In step 3, electrodeposition
After, the initial pH value of anolyte before ammonium hydroxide adjusts the pH value of anode stripped solution to step 2 septation electrodeposition is added.
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| CN201810766208.2A CN108893616A (en) | 2018-07-12 | 2018-07-12 | A kind of method of chlorination lead skim wet clean processes |
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| CN201810766208.2A CN108893616A (en) | 2018-07-12 | 2018-07-12 | A kind of method of chlorination lead skim wet clean processes |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110157913A (en) * | 2019-05-22 | 2019-08-23 | 北京矿冶科技集团有限公司 | A kind of method of copper ashes integrated treatment |
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2018
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| US4352786A (en) * | 1981-02-24 | 1982-10-05 | Institute Of Nuclear Energy Research | Treatment of copper refinery anode slime |
| CN101173326A (en) * | 2007-11-30 | 2008-05-07 | 浙江工业大学 | Method for recovery utilization of acid waste liquid generated in waste lead acid accumulator lead -recovery process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110157913A (en) * | 2019-05-22 | 2019-08-23 | 北京矿冶科技集团有限公司 | A kind of method of copper ashes integrated treatment |
| CN110157913B (en) * | 2019-05-22 | 2020-11-27 | 北京矿冶科技集团有限公司 | Method for comprehensively treating copper slag |
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