CN109022816A - The leaching liquid and extract technology of remaining lead in a kind of lead ore - Google Patents
The leaching liquid and extract technology of remaining lead in a kind of lead ore Download PDFInfo
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- CN109022816A CN109022816A CN201810969996.5A CN201810969996A CN109022816A CN 109022816 A CN109022816 A CN 109022816A CN 201810969996 A CN201810969996 A CN 201810969996A CN 109022816 A CN109022816 A CN 109022816A
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- Prior art keywords
- lead
- leaching
- parts
- ore
- remaining
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Classifications
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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
- 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
- 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
- C22B3/045—Leaching using electrochemical 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
- 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
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
-
- 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 leaching liquid and extract technology of remaining lead, belong to lead preparation method technical field in a kind of lead ore.It is characterized in that, group becomes 12.2 ~ 17.9 parts of raw material copper chloride of water and following parts by weight, 36.5 ~ 44.3 parts of iron chloride, 33.7 ~ 38.9 parts of sodium chloride, 4.5 ~ 6.5 parts of yttrium chloride, 4.2 ~ 5.9 parts of hydrochloric acid.Leaching step: lead ore or slag are added to the leaching liquid of remaining lead；It carries out leaching under agitation while carrying out electrochemical reduction, it is obtained by filtration under leaching temperature after filtrate X1 is cooled to 20 DEG C of following crystallization and carries out that filtrate X11 and filter residue Y11 is obtained by filtration, filtrate X11 returns directly to remaining lead leaching liquid and reuses, and filter residue Y11 is washed to obtain lead chloride.The present invention can efficiently, completely go out the lead leaching separation in lead ore.Leaching liquid of the invention can be reused, without discharging of waste liquid, environmental protection and energy saving.
Description
Technical field
The leaching liquid and extract technology of remaining lead, belong to lead preparation method technical field in a kind of lead ore.
Background technique
Contain a large amount of lead element in lead concentrate, lead is a kind of metallic element, can be used as sulfuric acid corrosion resistant, anti-third kind penetrate
The material of line, battery etc..Its alloy can make font, bearing, cable sheathing etc. and be used, and can also make athletic sports appliance shot.
Current lead-smelting method mainly has pyrometallurgical smelting of lead and two kinds of electrorefining.
For refining lead based on pyrometallurgical smelting of lead, pyrometallurgical smelting of lead generally comprises raw material preparation (ingredient, granulation, sintering in the world at present
Roasting), reduction melting produce lead bullion and the big process of the refining of lead bullion three.Flue gas acid preparing, flue dust synthetical recovery and from the earth of positive pole return
Receive the important component that the noble metals such as gold and silver are also pyrometallurgical smelting of lead technique.But the pyrometallurgical smelting of lead consumption energy is larger, simultaneously also
There are the wastes such as flue gas to cause environmental pollution.
Electrolytic lead refining is typically now hereby proposed using the cypress for being 1901, is tentatively refined by lead bullion or by pyrogenic process
Semi-refined lead, the process being electrolysed in the aqueous solution of silicofluoric acid and fluosilicic lead plumbate.Its purpose is to obtain high-grade
Lead and recycle Americium and rare precious metal.But this preparation method production efficiency is lower, consumption is big.
Traditional preparation method problem too low there is also the recovery rate of lead in lead ore, causes a large amount of wasting of resources.
Summary of the invention
The technical problem to be solved by the present invention is overcoming the deficiencies of the prior art and provide a kind of high production efficiency, the energy disappears
The leaching liquid and extract technology of consumption remaining lead less and in the high lead ore of recovery rate.
The technical solution adopted by the present invention to solve the technical problems is: the leaching liquid of remaining lead, feature exist in the lead ore
Become 12.2 ~ 17.9 parts of raw material copper chloride of water and following parts by weight in, group, 36.5 ~ 44.3 parts of iron chloride, sodium chloride 33.7 ~
38.9 parts, 4.5 ~ 6.5 parts of yttrium chloride, 4.2 ~ 5.9 parts of hydrochloric acid.
Remaining lead leaching liquid of the invention is suitble to the lower lead ore of lead content or extracted carry out in the slag of a lead
More completely leach.Efficiently, completely the lead leaching separation in lead ore can be gone out.Leaching liquid of the invention can repeat to make
With without discharging of waste liquid, environmental protection and energy saving.Remaining element in ore is not destroyed, after leaching lead out, remaining element more holds
It is easily separated to produce.
Preferably, group becomes 14.3 ~ 15.9 parts of raw material copper chloride of water and following parts by weight, and 38.2 ~ 41.3 parts of iron chloride,
34.7 ~ 36.8 parts of sodium chloride, 4.8 ~ 6.1 parts of yttrium chloride, 4.8 ~ 5.3 parts of hydrochloric acid.Preferred remaining lead leaching liquid proportion can be more
Leaching is faster completed under mild environment.
Preferably, the mass ratio of the yttrium chloride and hydrochloric acid is 1:0.87 ~ 1.Preferred proportion can be further improved leaching
Efficiency out.
A kind of extract technology of lead, which comprises the steps of:
1) leaching liquid of above-mentioned remaining lead, the leaching of lead ore or slag and remaining lead is added in the slag after lead ore or lead ore mention lead
The solid-to-liquid ratio g:L of liquid is 1 ~ 3:4 ~ 7；It carries out leaching while carrying out electrochemical reduction under agitation, leaching temperature is 80 DEG C
~ 90 DEG C, leaching time is 50 min ~ 70min；Filtrate X1 is obtained by filtration under leaching temperature；
2) filtrate X1 after being cooled to 20 DEG C of following crystallization carries out that filtrate X11 and filter residue Y11 is obtained by filtration, and filtrate X11 is directly returned
It is reused to remaining lead leaching liquid, filter residue Y11 is washed to obtain lead chloride.
The present invention provide it is a kind of by lead ore or extracted and directly leached in the slag of a lead, obtain lead chloride
Technique, lead chloride can be applied directly as product, can also be given to subsequent process and be obtained lead metal.Pass of the invention
Key is that leaching liquid, remaining lead leaching liquid are suitble to more completely be leached in the lower ore of lead content.It can efficiently, completely
The lead leaching separation in lead ore is gone out.Two kinds of leaching liquids of the invention can be reused, without discharging of waste liquid, environmental protection
Energy conservation.Preparation process of the invention is not destroyed to remaining element in ore, and after leaching lead out, remaining element is easier
Separation is produced.
Preferably, it is 0.5% that the content that the lead ore or lead ore mention lead in the slag after lead, which is calculated in mass percent,
~40%.Technique of the invention is especially suitable for leaching the lower ore of lead content, realizes complete lead separation.
Preferably, leaching temperature described in step 1) is 80 DEG C ~ 82 DEG C, and leaching time is 50 min ~ 53min.The leaching
Condition is taken to meet preferred lead leaching liquid proportion leaching.
Preferably, the solid-to-liquid ratio g:L of lead ore or slag and the leaching liquid of remaining lead in step 1) is 2:5 ~ 6.Preferred slag
It can faster complete to leach with the solid-to-liquid ratio of remaining lead leaching liquid.
Preferably, the voltage that electrochemical reduction is carried out described in step 1) is the V of 10V ~ 30, and electric current is 10 A ~ 100A, institute
Electrode is tungsten electrode.Preferred electrochemical reduction condition can preferably cooperate with leaching condition, more efficiently, completely
Separation.
Compared with prior art, possessed beneficial effect of the invention is: this preparation process is to the lead after once mentioning lead
Remaining lead in mine can carry out efficient sufficiently leaching at a lower temperature.Leaching liquid used can isolate it is required
It is standby that the slag for being recycled after lead, and being generated can be used for further made of metal, after more sufficiently extracting lead,
No longer kept the refinement of residual metallic element more convenient by the interference of lead when residual metallic element extraction.This preparation process is not only
Lead metal can efficiently be prepared, and required temperature is lower, energy consumption is smaller, in the process without any exhaust gas, waste residue, waste liquid
It generates, energy conservation and environmental protection.
Specific embodiment
The present invention will be further described combined with specific embodiments below, and wherein embodiment 1 is best implements.
Embodiment 1
1) slag after lead ore mention lead is added the leaching liquid of remaining lead, lead ore mention the content of lead in the slag after lead with
Mass percent is calculated as 5.5%；The solid-to-liquid ratio g:L of the leaching liquid of lead ore or slag and remaining lead is 2:5.5, the leaching liquid of remaining lead
Group becomes 15.1 parts of raw material copper chloride of water and following parts by weight, and 40.3 parts of iron chloride, 35.4 parts of sodium chloride, 5 parts of yttrium chloride, salt
5.2 parts of acid；It carries out leaching while carrying out electrochemical reduction under agitation, the voltage of electrochemical reduction is 20V, and electric current is
50A, electrode used are tungsten electrode；Leaching temperature is 80 DEG C, and leaching time is 50 min；Filter is obtained by filtration under leaching temperature
Liquid X1 and filter residue Y1；
2) filtrate X1 after being cooled to 20 DEG C of following crystallization carries out that filtrate X11 and filter residue Y11 is obtained by filtration, and filtrate X11 is directly returned
It is reused to remaining lead leaching liquid, filter residue Y11 is washed to obtain lead chloride；
Detecting the lead content in filter residue Y1 is 0.001%.
Embodiment 2
1) slag after lead ore mention lead is added the leaching liquid of remaining lead, lead ore mention the content of lead in the slag after lead with
Mass percent is calculated as 5.5%；The solid-to-liquid ratio g:L of the leaching liquid of lead ore or slag and remaining lead is 2:5, the group of the leaching liquid of remaining lead
As 14.3 parts of water and the raw material copper chloride of following parts by weight, 41.3 parts of iron chloride, 34.7 parts of sodium chloride, 6.1 parts of yttrium chloride, salt
5.3 parts of acid；It carries out leaching while carrying out electrochemical reduction under agitation, the voltage of electrochemical reduction is 15V, electric current 30
A, electrode used are tungsten electrode；Leaching temperature is 82 DEG C, leaching time 50min；Filtrate is obtained by filtration under leaching temperature
X1 and filter residue Y1；
2) filtrate X1 after being cooled to 20 DEG C of following crystallization carries out that filtrate X11 and filter residue Y11 is obtained by filtration, and filtrate X11 is directly returned
It is reused to remaining lead leaching liquid, filter residue Y11 is washed to obtain lead chloride；
Detecting the lead content in filter residue Y1 is 0.001%.
Embodiment 3
1) slag after lead ore mention lead is added the leaching liquid of remaining lead, lead ore mention the content of lead in the slag after lead with
Mass percent is calculated as 5.5%；The solid-to-liquid ratio g:L of the leaching liquid of lead ore or slag and remaining lead is 2:6, the group of the leaching liquid of remaining lead
As 15.9 parts of water and the raw material copper chloride of following parts by weight, 38.2 parts of iron chloride, 36.8 parts of sodium chloride, 4.8 parts of yttrium chloride, salt
4.8 parts of acid；It carries out leaching while carrying out electrochemical reduction under agitation, the voltage of electrochemical reduction is 25 V, and electric current is
70A, electrode used are tungsten electrode；Leaching temperature is 80 DEG C, leaching time 53min；Filter is obtained by filtration under leaching temperature
Liquid X1 and filter residue Y1；
2) filtrate X1 after being cooled to 20 DEG C of following crystallization carries out that filtrate X11 and filter residue Y11 is obtained by filtration, and filtrate X11 is directly returned
It is reused to remaining lead leaching liquid, filter residue Y11 is washed to obtain lead chloride；
Detecting the lead content in filter residue Y1 is 0.001%.
Embodiment 4
1) slag after lead ore mention lead is added the leaching liquid of remaining lead, lead ore mention the content of lead in the slag after lead with
Mass percent is calculated as 5.5%；The solid-to-liquid ratio g:L of the leaching liquid of lead ore or slag and remaining lead is 1:7, the group of the leaching liquid of remaining lead
As 12.2 parts of water and the raw material copper chloride of following parts by weight, 44.3 parts of iron chloride, 33.7 parts of sodium chloride, 6.5 parts of yttrium chloride, salt
4.2 parts of acid；It carries out leaching while carrying out electrochemical reduction under agitation, the voltage of electrochemical reduction is 10V, electric current 10
A, electrode used are tungsten electrode；Leaching temperature is 86 DEG C, leaching time 70min；Filtrate is obtained by filtration under leaching temperature
X1 and filter residue Y1；
2) filtrate X1 after being cooled to 20 DEG C of following crystallization carries out that filtrate X11 and filter residue Y11 is obtained by filtration, and filtrate X11 is directly returned
It is reused to remaining lead leaching liquid, filter residue Y11 is washed to obtain lead chloride；
Detecting the lead content in filter residue Y1 is 0.005%.
Embodiment 5
1) slag after lead ore mention lead is added the leaching liquid of remaining lead, lead ore mention the content of lead in the slag after lead with
Mass percent is calculated as 5.5%；The solid-to-liquid ratio g:L of the leaching liquid of lead ore or slag and remaining lead is 3:4, the group of the leaching liquid of remaining lead
As 17.9 parts of water and the raw material copper chloride of following parts by weight, 36.5 parts of iron chloride, 38.9 parts of sodium chloride, 4.5 parts of yttrium chloride, salt
5.9 parts of acid；It carries out leaching while carrying out electrochemical reduction under agitation, the voltage of electrochemical reduction is 30 V, and electric current is
100A, electrode used are tungsten electrode；Leaching temperature is 90 DEG C, leaching time 66min；Filter is obtained by filtration under leaching temperature
Liquid X1 and filter residue Y1；
2) filtrate X1 after being cooled to 20 DEG C of following crystallization carries out that filtrate X11 and filter residue Y11 is obtained by filtration, and filtrate X11 is directly returned
It is reused to remaining lead leaching liquid, filter residue Y11 is washed to obtain lead chloride；
Detecting the lead content in filter residue Y1 is 0.004%.
Comparative example 1
1) slag after lead ore mention lead is added the leaching liquid of remaining lead, lead ore mention the content of lead in the slag after lead with
Mass percent is calculated as 5.5%；The solid-to-liquid ratio g:L of the leaching liquid of lead ore or slag and remaining lead is 2:5.5, the leaching liquid of remaining lead
Group becomes 15.1 parts of raw material copper chloride, 40.3 parts of iron chloride, 35.4 parts of sodium chloride, 5.2 parts of hydrochloric acid of water and following parts by weight；?
It carries out leaching while carrying out electrochemical reduction under stirring condition, the voltage of electrochemical reduction is 20V, electric current 50A, electricity used
Extremely tungsten electrode；Leaching temperature is 80 DEG C, and leaching time is 50 min；Filtrate X1 and filter residue are obtained by filtration under leaching temperature
Y1；
2) filtrate X1 after being cooled to 20 DEG C of following crystallization carries out that filtrate X11 and filter residue Y11 is obtained by filtration, and filtrate X11 is directly returned
It is reused to remaining lead leaching liquid, filter residue Y11 is washed to obtain lead chloride；
Detecting the lead content in filter residue Y1 is 5.2%.
Comparative example 2
1) slag after lead ore mention lead is added the leaching liquid of remaining lead, lead ore mention the content of lead in the slag after lead with
Mass percent is calculated as 5.5%；The solid-to-liquid ratio g:L of the leaching liquid of lead ore or slag and remaining lead is 2:5.5, the leaching liquid of remaining lead
Group becomes 35.4 parts of raw material copper chloride of water and following parts by weight, and 15.1 parts of iron chloride, 40.3 parts of sodium chloride, 5 parts of yttrium chloride, salt
5.2 parts of acid；It carries out leaching while carrying out electrochemical reduction under agitation, the voltage of electrochemical reduction is 20V, and electric current is
50A, electrode used are tungsten electrode；Leaching temperature is 80 DEG C, and leaching time is 50 min；Filter is obtained by filtration under leaching temperature
Liquid X1 and filter residue Y1；
2) filtrate X1 after being cooled to 20 DEG C of following crystallization carries out that filtrate X11 and filter residue Y11 is obtained by filtration, and filtrate X11 is directly returned
It is reused to remaining lead leaching liquid, filter residue Y11 is washed to obtain lead chloride；
Detecting the lead content in filter residue Y1 is 4.9%.
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Imitate embodiment.But without departing from the technical solutions of the present invention, according to the technical essence of the invention to above embodiments institute
Any simple modification, equivalent variations and the remodeling made, still fall within the protection scope of technical solution of the present invention.
Claims (8)
1. the leaching liquid of remaining lead in a kind of lead ore, which is characterized in that group become the raw material copper chlorides 12.2 of water and following parts by weight ~
17.9 parts, 36.5 ~ 44.3 parts of iron chloride, 33.7 ~ 38.9 parts of sodium chloride, 4.5 ~ 6.5 parts of yttrium chloride, 4.2 ~ 5.9 parts of hydrochloric acid.
2. the leaching liquid of remaining lead in a kind of lead ore according to claim 1, it is characterised in that: group becomes water and following weight
14.3 ~ 15.9 parts of raw material copper chloride of part, 38.2 ~ 41.3 parts of iron chloride, 34.7 ~ 36.8 parts of sodium chloride, yttrium chloride 4.8 ~ 6.1
Part, 4.8 ~ 5.3 parts of hydrochloric acid.
3. the leaching liquid of remaining lead in a kind of lead ore according to claim 1 or 2, it is characterised in that: the yttrium chloride with
The mass ratio of hydrochloric acid is 1:0.87 ~ 1.
4. a kind of extract technology of lead, which comprises the steps of:
1) leaching liquid of any one of claim 1 ~ 3 remaining lead, lead ore is added in the slag after lead ore or lead ore mention lead
Or the solid-to-liquid ratio g:L of slag and the leaching liquid of remaining lead, it is 1 ~ 3:4 ~ 7；It carries out leaching under agitation while carrying out electrochemistry
Reduction, leaching temperature are 80 DEG C ~ 90 DEG C, and leaching time is 50 min ~ 70min；Filtrate X1 is obtained by filtration under leaching temperature；
2) filtrate X1 after being cooled to 20 DEG C of following crystallization carries out that filtrate X11 and filter residue Y11 is obtained by filtration, and filtrate X11 is directly returned
It is reused to remaining lead leaching liquid, filter residue Y11 is washed to obtain lead chloride.
5. a kind of extract technology of lead according to claim 4, it is characterised in that: the lead ore or lead ore carries out mentioning lead
It is 0.5% ~ 40% that the content of lead, which is calculated in mass percent, in slag afterwards.
6. a kind of extract technology of lead according to claim 4, it is characterised in that: leaching temperature described in step 1) is
80 DEG C ~ 82 DEG C, leaching time is 50min ~ 53min.
7. a kind of extract technology of lead according to claim 4, it is characterised in that: lead ore or slag and remaining lead in step 1)
Leaching liquid solid-to-liquid ratio g:L, be 2:5 ~ 6.
8. a kind of extract technology of lead according to claim 4, it is characterised in that: progress electrochemistry described in step 1) is also
Former voltage is the V of 10V ~ 30, and electric current is 10 A ~ 100A, and electrode used is tungsten electrode.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810969996.5A CN109022816A (en) | 2018-08-24 | 2018-08-24 | The leaching liquid and extract technology of remaining lead in a kind of lead ore |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810969996.5A CN109022816A (en) | 2018-08-24 | 2018-08-24 | The leaching liquid and extract technology of remaining lead in a kind of lead ore |
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| CN201810969996.5A Pending CN109022816A (en) | 2018-08-24 | 2018-08-24 | The leaching liquid and extract technology of remaining lead in a kind of lead ore |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105779774A (en) * | 2016-04-22 | 2016-07-20 | 王树立 | Lead concentrate and zinc anode mud combined recycling method |
| CN105907960A (en) * | 2016-04-22 | 2016-08-31 | 王树立 | Method for combined resourceful treatment of lead concentrate and zinc anode mud |
| CN107245579A (en) * | 2017-04-28 | 2017-10-13 | 贵州宏达环保科技有限公司 | A kind of method that Zn, Mn, Pb, Ag are extracted in the earth of positive pole from zinc electrolysis |
| CN108034831A (en) * | 2018-01-15 | 2018-05-15 | 安徽工业大学 | A kind of integrated conduct method containing miscellaneous Gold Concentrate under Normal Pressure melting flue dust |
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2018
- 2018-08-24 CN CN201810969996.5A patent/CN109022816A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105779774A (en) * | 2016-04-22 | 2016-07-20 | 王树立 | Lead concentrate and zinc anode mud combined recycling method |
| CN105907960A (en) * | 2016-04-22 | 2016-08-31 | 王树立 | Method for combined resourceful treatment of lead concentrate and zinc anode mud |
| CN107245579A (en) * | 2017-04-28 | 2017-10-13 | 贵州宏达环保科技有限公司 | A kind of method that Zn, Mn, Pb, Ag are extracted in the earth of positive pole from zinc electrolysis |
| CN108034831A (en) * | 2018-01-15 | 2018-05-15 | 安徽工业大学 | A kind of integrated conduct method containing miscellaneous Gold Concentrate under Normal Pressure melting flue dust |
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Application publication date: 20181218 |