CN105821218A - Method of removing impurity element copper in crude lead through supergravity - Google Patents
Method of removing impurity element copper in crude lead through supergravity Download PDFInfo
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- CN105821218A CN105821218A CN201610306293.5A CN201610306293A CN105821218A CN 105821218 A CN105821218 A CN 105821218A CN 201610306293 A CN201610306293 A CN 201610306293A CN 105821218 A CN105821218 A CN 105821218A
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- Prior art keywords
- hypergravity
- lead bullion
- lead
- impurity element
- copper
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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
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
-
- 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
- C22B13/02—Obtaining lead by dry 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
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
- C22B9/023—By filtering
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the technical field of refining of crude lead, and discloses a method of removing impurity element copper in crude lead through supergravity. The method comprises the following steps of: cooling melted crude lead melt mass at a cooling rate of less than 10 DEG C/min to obtain the pretreated crude lead; and carrying out supergravity separation treatment on the pretreated crude lead, wherein the treatment temperature is 330 DEG C-350 DEG C, the gravity coefficient is greater than 100, and the time of supergravity separation treatment is 10-20 minutes. The method has the beneficial effects that the relative movement of a solid copper phase and metallic lead liquid is greatly intensified by utilizing supergravity; the complete separation of an impurity copper phase and refined lead is completed within very short time, thereby realizing the purpose of purifying the crude lead by removing copper in the crude lead; meanwhile, the yield of metallic lead is also greatly increased, and the wasting and environmental pollution of the metallic lead are reduced; and the method is simple in technological process, low in cost, environmentally-friendly and suitable for popularization and application.
Description
Technical field
The present invention relates to refining of lead bullion technical field, remove impurity element copper in lead bullion particularly to a kind of hypergravity
Method.
Background technology
In industrial lead bullion, copper is topmost impurity element, therefore first has in refining of lead bullion purification process
Remove impurity copper therein.
Current industrial general employing pyro-refining adds electrorefining to purify lead bullion.The first step of pyro-refining is exactly
Removing impurity copper therein, conventional copper-removing method includes liquation decoppering method and adds sulfur copper removal method.Though both approaches
So the copper content in lead bullion can be reduced to reduced levels, but in liquation decoppering technique, need operator repeatedly
Salvaging copper ashes, therefore the activity duration is long, and labor strength is big；And add in sulfur copper removal technique, need to add in batches
Entering the sulfur of different content, therefore process route is more complicated, additionally, add the smoke exhaust of sulfur generation to human body and ring
There is the biggest harm in border, and the working environment of workers is severe.And kish lead content in the copper dross slag salvaged
More than 60wt%, cause a large amount of wastes of metallic lead.
The rise of high-gravity technology, provides new thinking for hypergravity application on Decoppering in lead bullion.
Summary of the invention
The purpose of the present invention overcomes the deficiencies in the prior art exactly, it is provided that a kind of hypergravity removes impurity unit in lead bullion
The method of element copper, including:
By molten bullion melt to cool down less than 10 DEG C/min cooldown rate, it is thus achieved that the step of pretreatment lead bullion；With
And
Described pretreatment lead bullion is carried out the step of hypergravity separating treatment.
Further, in described hypergravity separate processing step, treatment temperature is 330-350 DEG C, and gravity coefficient is big
In 100, i.e. hypergravity acceleration is more than 100g.
Further, described treatment temperature is 340 DEG C.
Further, in described hypergravity separate processing step, pretreatment lead bullion sample is put on the filter, outward
Set graphite crucible, puts into together and is warming up to 340 DEG C in hypergravity heating furnace, is incubated 10min, is then turned on being centrifuged
Machine carries out hypergravity separating treatment, and process takes out graphite crucible water-cooled after terminating.
Further, the filtering material of described filter is porous carbon felt material, and the average pore size of carbon fiber is
10～15 μm, thickness is 5mm.
Further, in lead bullion, the content of impurity copper is 0.6-3.25wt%.
Further, the time of hypergravity separating treatment is 10-20min.
Further, the sample that described pretreatment lead bullion obtains after carrying out hypergravity separating treatment carries out water-cooled process.
Further, the smelting temperature of lead bullion is not less than 820 DEG C, and temperature retention time is not less than 30min.
Further, during molten bullion melt cooling to 200 DEG C, take out sample and cool down in atmosphere.
The invention have the benefit that and utilize hypergravity greatly to enhance solid copper phase fortune relative with metallic lead liquid
Dynamic, complete being completely separated of impurity copper phase and lead bullion within a very short time, it is achieved thereby that the mesh that Decoppering in lead bullion purifies
, the most also substantially increase the recovery rate of metallic lead, decrease waste and the environmental pollution of metallic lead, technique stream
Journey is simple, with low cost, and environmental protection is suitable to popularization and application.
Accompanying drawing explanation
Fig. 1 show hypergravity implementation schematic diagram in the embodiment of the present invention.
Fig. 2 show view before and after filtration device structure and sample filtration separate in the embodiment of the present invention.
Fig. 3 show the sample macroscopic view separating effect figure filtered after separating.
Fig. 4 show macrostructure's figure of lead bullion in the sample filtered after separating.
Fig. 5 show the microscopic appearance figure of lead bullion in the sample filtered after separating.
Fig. 6 show the microscopic appearance figure of copper ashes in the sample filtered after separating.
Fig. 7 show the macro-effect figure of control sample.
Fig. 8 show the macro morphology figure in control sample within lead bullion.
Fig. 9 show the microscopic appearance figure in control sample within lead bullion.
Wherein, the lead bullion liquid after the molten bullion before 1-filters, the copper ashes after 2-filtration, 3-filtration.
Detailed description of the invention
The specific embodiment of the invention is described in detail below in conjunction with concrete accompanying drawing.It should be noted that, following embodiment
Described in technical characteristic or the combination of technical characteristic be not construed as isolating, they can be by mutual group
Close thus reach superior technique effect.In the accompanying drawing of following embodiment, the identical label generation that each accompanying drawing is occurred
Feature that table is identical or parts, can be applicable in different embodiment.
A kind of hypergravity of the embodiment of the present invention removes the method for impurity element copper in lead bullion, including:
By molten bullion melt to cool down less than 10 DEG C/min cooldown rate, it is thus achieved that the step of pretreatment lead bullion；With
And
Described pretreatment lead bullion is carried out the step of hypergravity separating treatment.
In described hypergravity separate processing step, when treatment temperature is 330-350 DEG C, gravity coefficient is more than 100,
When i.e. hypergravity acceleration is more than 100g, treatment effect is preferable.
Preferably, when described treatment temperature is 340 DEG C, treatment effect is optimal.
Preferably, in described hypergravity separate processing step, pretreatment lead bullion sample is placed on filter top, will
Whole filter is put in a graphite crucible, puts into the most together and is warming up to 340 DEG C in hypergravity heating furnace, protects
Temperature 10min, is then turned on centrifuge and carries out hypergravity separating treatment, and process takes out graphite crucible water-cooled after terminating；
Fig. 2 showing, lead bullion filters the state before and after separating.
Preferably, the filtering material of described filter is porous carbon felt material, the average pore size of carbon fiber be 10～
15 μm, thickness is 5mm.
In lead bullion, the content of impurity copper is 0.6-3.25wt%, substantially covers containing of cupra matter in actual industrial production
Weight range.
Preferably, the time of hypergravity separating treatment is 10-20min, processes the time too short, and effect is difficult to protect
Card；In view of production efficiency, process the time also unsuitable long.
The sample that described pretreatment lead bullion obtains after carrying out hypergravity separating treatment can carry out water-cooled process.
Preferably, the smelting temperature of lead bullion is not less than 820 DEG C, and temperature retention time is not less than 30min, it is ensured that metal is complete
Full-fusing；Cooldown rate is less than 10 DEG C/min, during molten bullion melt cooling to 200 DEG C, takes out sample at sky
Gas cools down.
Embodiment
In actual industrial production, the content range of cupra matter is 0.6-3.25wt%, real for the more accurate evaluation present invention
Executing the effect of example method, on the premise of without loss of generality, the present embodiment uses technical pure Pb (lead) and industry
Pure Cu (copper) is melted is prepared as Pb-Cu binary lead bullion, to above-mentioned Pb-Cu binary lead bullion application the inventive method pair
It processes.
In the present embodiment, technical pure Pb used can any one metal Pb material known to those skilled in the art
Material, not particularly requirement.Such as, the metal Pb block of employing can be purchased from Beijing kingfisher platinum woods non-ferrous metal skill
The technical pure Pb block of art development centre, purity is 99.99%.
Technical pure Cu used can any one technical pure Cu material known to those skilled in the art, there is no spy
Other requirement.Such as, technical pure Cu of employing can be purchased from Beijing Cui Bolin non-ferrous metal technology development center
Technical pure Cu block, purity is 99.99%.
In the preparation of Pb-Cu binary lead bullion, the proportioning of Pb and Cu is according to impurity Cu in the lead bullion of actual industrial production
Content determine, and because of in industrial lead bullion the fluctuation of impurity copper content relatively big, enter in this capping value
Row assessment.Proportional quantity for Pb and Cu does not finish the requirement of fully hard property.
In the Pb-Cu binary lead bullion melting preparation of the present embodiment, smelting temperature is not less than 820 DEG C, and temperature retention time is not
Less than 30min to guarantee that metal is the most melted, cooldown rate is less than 10 DEG C/min, treats that sample is cooled to 200 DEG C
Take out sample to cool down in atmosphere.
In the present embodiment use filter, filtering material is porous carbon felt material, average pore size be 10～
15 μm, thickness is 5mm, and the diameter of carbon fiber matches with crucible.
The bracing frame of filter bottom is self manufacture, is two pieces of mutual decussations of technical pure iron plate, cross
On put a rounded porous iron plate, it is to prevent porous in hypergravity processing procedure that crucible bottom places bracing frame
Carbon felt moves downward.
For the effect of objective evaluation embodiment of the present invention method, the instrument used is as follows: (model is scanning electron microscope
SEM-EDS, MLA250), optical microscope (model is 9XB-PC), chemical composition test uses ICP-OES
(model is OPTIMA7000DV).
A kind of hypergravity of the embodiment of the present invention removes the method for impurity element copper in lead bullion, comprises the steps:
The silica crucible of step one, the fetching pure Cu of the most appropriate pure Pb and 3wt%, puts into graphite crucible, then
Put into hypergravity heating furnace together；It is warming up to 820 DEG C, is incubated 30 minutes, and stirs, then with 5 DEG C
/ min cooling rate cools down, and treats that temperature is down to 200 DEG C and is taken out sample water-cooled, obtains pretreatment lead bullion；
Step 2, pretreatment lead bullion is loaded in separator crucible, add graphite crucible set and put into hypergravity heating together
Being warming up to 340 DEG C in stove, be incubated 10min, being then turned on centrifuge and being adjusted to rotating speed is 600r/min, corresponding
Gravity coefficient is G=100, starts to carry out hypergravity process under 340 DEG C of constant temperatures, after pending 10min, closes
Close centrifuge, take out sample water-cooled.Take pictures with digital camera and observe macroscopic view filter effect, as shown in Figure 3；Incited somebody to action
Filter is cut open from centre to the lead bullion of crucible bottom along hypergravity direction, wherein half through inlaying, number, grind,
Polishing, takes pictures with digital camera and observes the internal macro morphology of sample, and result is as shown in Figure 4；Use metallography microscope
The quantity of impurity copper phase and microscopic appearance in sem observation sample, result is as shown in Figure 5；Use scanning electron microscopic observation copper ashes
Microscopic appearance result, result is as shown in Figure 6.
For the treatment effect of the embodiment of the present invention is described, comparative example is used to be verified, in comparative example, above-mentioned step
After rapid one processes, being loaded in separator crucible by pretreatment lead bullion, overcoat graphite crucible is put into hypergravity together and is added
It is warming up to 340 DEG C in hot stove, is incubated 20min, then takes out sample water-cooled.Take pictures with digital camera and observe macroscopic view
Filter effect, as shown in Figure 7.Being cut open along hypergravity direction from centre by sample, wherein half is through inlaying, compiling
Number, grind, polishing, take pictures the observation internal macro morphology of sample with digital camera, result as shown in Figure 8,
With the quantity of impurity copper phase in metallography microscope sem observation sample and microscopic appearance, result is as shown in Figure 9.
Table 1 shows the chemical composition of sample after separating in normal gravitational field with hypergravity, and purifying rate and metal are received
Rate.
Table 1
As can be found from Table 1, not occurring to filter segregation phenomenon in comparative example, in lead bullion, copper content remains
3.032；And after hypergravity filters and separates, the impurity copper content in lead bullion is reduced to only 0.157wt%, with
Time separation efficiency also reached 96.18%, in copper ashes, kish Pb content only has 23.56wt%, substantially increases
The recovery rate of metal, illustrates that hypergravity is the very efficient separation method of one.
Comparison diagram 3 and Fig. 7 is it can be seen that often sample can't occur segregation phenomenon in gravitational field, and at hypergravity
In Chang, lead bullion liquid almost all has been split into the bottom of crucible, and impurity copper is trapped within the top of carbon felt mutually.
Comparison diagram 4,5 and Fig. 8,9 it can be seen that in normal gravitational field impurity copper be still present in mutually in lead bullion,
And hypergravity separate after, lead bullion does not find impurity copper phase, copper is the most all trapped within carbon felt top, lead bullion because of
This has obtained purification.
From Fig. 6 it is found that impurity copper is dendroid mutually, at interdendritic residual fraction lead liquid after hypergravity separation,
But residual lead content is fewer, and therefore hypergravity drastically increases the recovery rate of metallic lead.
The invention have the benefit that and utilize hypergravity greatly to enhance solid copper phase fortune relative with metallic lead liquid
Dynamic, complete being completely separated of impurity copper phase and lead bullion within a very short time, it is achieved thereby that the mesh that Decoppering in lead bullion purifies
, the most also substantially increase the recovery rate of metallic lead, decrease waste and the environmental pollution of metallic lead, technique stream
Journey is simple, with low cost, and environmental protection is suitable to popularization and application.
Although having been presented for several embodiments of the present invention herein, but those skilled in the art should managing
Solve, without departing from the spirit of the invention, the embodiments herein can be changed.Above-described embodiment is only
It is exemplary, should be using the embodiments herein as the restriction of interest field of the present invention.
Claims (10)
1. a hypergravity removes the method for impurity element copper in lead bullion, it is characterised in that including:
By molten bullion melt to cool down less than 10 DEG C/min cooldown rate, it is thus achieved that the step of pretreatment lead bullion；And
Described pretreatment lead bullion is carried out the step of hypergravity separating treatment.
2. hypergravity as claimed in claim 1 removes the method for impurity element copper in lead bullion, it is characterised in that in described hypergravity separate processing step, treatment temperature is 330-350 DEG C, and gravity coefficient is more than 100, i.e. hypergravity acceleration is more than 100g.
3. hypergravity as claimed in claim 2 removes the method for impurity element copper in lead bullion, it is characterised in that described treatment temperature is 340 DEG C.
4. hypergravity as claimed in claim 3 removes the method for impurity element copper in lead bullion, it is characterized in that, in described hypergravity separate processing step, pretreatment lead bullion sample is put on the filter, overcoat graphite crucible, puts into together and is warming up to 340 DEG C in hypergravity heating furnace, is incubated 10min, being then turned on centrifuge and carry out hypergravity separating treatment, process takes out graphite crucible water-cooled after terminating.
5. hypergravity as claimed in claim 4 removes the method for impurity element copper in lead bullion, it is characterised in that the filtering material of described filter is porous carbon felt material, and the average pore size of carbon fiber is 10～15 μm, and thickness is 5mm.
6. hypergravity as claimed in claim 1 removes the method for impurity element copper in lead bullion, it is characterised in that in lead bullion, the content of impurity copper is 0.6-3.25wt%.
7. hypergravity as claimed in claim 1 removes the method for impurity element copper in lead bullion, it is characterised in that the time of hypergravity separating treatment is 10-20min.
8. hypergravity as claimed in claim 1 removes the method for impurity element copper in lead bullion, it is characterised in that the sample that described pretreatment lead bullion obtains after carrying out hypergravity separating treatment carries out water-cooled process.
9. remove the method for impurity element copper in lead bullion such as any one hypergravity of claim 1-8, it is characterised in that the smelting temperature of lead bullion is not less than 820 DEG C, and temperature retention time is not less than 30min.
10. hypergravity as claimed in claim 9 removes the method for impurity element copper in lead bullion, it is characterised in that during molten bullion melt cooling to 200 DEG C, takes out sample and cools down in atmosphere.
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Cited By (14)
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|---|---|---|---|---|
| CN108165756A (en) * | 2018-01-10 | 2018-06-15 | 北京科技大学 | The method and device of metallic copper in a kind of hypergravity low temperature quick separating copper ashes |
| CN108950246A (en) * | 2018-07-03 | 2018-12-07 | 昆明理工大学 | A kind of hypergravity is removed containing method silver-colored in silver-tin alloy |
| CN109825719A (en) * | 2019-03-20 | 2019-05-31 | 北京科技大学 | A kind of method and device of hypergravity separation lead-antimony alloy |
| CN110484733A (en) * | 2019-09-19 | 2019-11-22 | 紫金矿业集团股份有限公司 | A kind of method of the waste and old aluminium base metal insoluble anode of high efficiente callback |
| CN111172393A (en) * | 2019-09-02 | 2020-05-19 | 昆明理工大学 | Method for separating Al-Sn-Cu ternary alloy by virtue of supergravity |
| CN114480867A (en) * | 2020-11-13 | 2022-05-13 | 内蒙古君成科技有限公司 | Method for remelting centrifugal magnetic separation and graded purification of ferro-silicon-aluminum alloy |
| CN114480865A (en) * | 2020-11-13 | 2022-05-13 | 内蒙古君成科技有限公司 | Method for low-temperature remelting centrifugal separation and fractional purification of ferro-silicon-aluminum alloy |
| CN114480866A (en) * | 2020-11-13 | 2022-05-13 | 内蒙古君成科技有限公司 | Method for remelting centrifugal flotation and graded purification of ferro-silicon-aluminum alloy |
| CN114477187A (en) * | 2020-11-13 | 2022-05-13 | 内蒙古君成科技有限公司 | Method for extracting industrial silicon from ferro-silicon-aluminum alloy |
| CN114480855A (en) * | 2020-11-13 | 2022-05-13 | 内蒙古君成科技有限公司 | Method for preparing ferro-silicon-aluminum alloy by using high-alumina fly ash and purifying ferro-silicon-aluminum alloy in grading mode |
| CN116200605A (en) * | 2023-01-05 | 2023-06-02 | 中国科学院过程工程研究所 | Production method for efficiently removing impurities from copper enameled wire after paint removal |
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| CN118006917A (en) * | 2024-04-08 | 2024-05-10 | 北京科技大学 | Method for reducing lead oxide slag source in electrolytic lead remelting process |
| CN118006917B (en) * | 2024-04-08 | 2024-06-28 | 北京科技大学 | Method for reducing lead oxide slag source in electrolytic lead remelting process |
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| CN108165756A (en) * | 2018-01-10 | 2018-06-15 | 北京科技大学 | The method and device of metallic copper in a kind of hypergravity low temperature quick separating copper ashes |
| CN108165756B (en) * | 2018-01-10 | 2019-03-29 | 北京科技大学 | The method and device of metallic copper in a kind of hypergravity low temperature quick separating copper ashes |
| CN108950246A (en) * | 2018-07-03 | 2018-12-07 | 昆明理工大学 | A kind of hypergravity is removed containing method silver-colored in silver-tin alloy |
| CN109825719A (en) * | 2019-03-20 | 2019-05-31 | 北京科技大学 | A kind of method and device of hypergravity separation lead-antimony alloy |
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| CN111172393A (en) * | 2019-09-02 | 2020-05-19 | 昆明理工大学 | Method for separating Al-Sn-Cu ternary alloy by virtue of supergravity |
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| CN110484733B (en) * | 2019-09-19 | 2021-03-16 | 紫金矿业集团股份有限公司 | Method for efficiently recovering waste aluminum-based lead alloy insoluble anode |
| CN114480866A (en) * | 2020-11-13 | 2022-05-13 | 内蒙古君成科技有限公司 | Method for remelting centrifugal flotation and graded purification of ferro-silicon-aluminum alloy |
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| CN114477187B (en) * | 2020-11-13 | 2024-04-19 | 内蒙古君成科技有限公司 | Method for extracting industrial silicon from aluminum-silicon-iron alloy |
| CN114480865A (en) * | 2020-11-13 | 2022-05-13 | 内蒙古君成科技有限公司 | Method for low-temperature remelting centrifugal separation and fractional purification of ferro-silicon-aluminum alloy |
| CN114480865B (en) * | 2020-11-13 | 2024-06-25 | 内蒙古君成科技有限公司 | Method for purifying aluminum-silicon-iron alloy by low-temperature remelting centrifugal separation and classification |
| CN114480855B (en) * | 2020-11-13 | 2024-05-14 | 内蒙古君成科技有限公司 | Method for preparing aluminum-silicon-iron alloy by using high-alumina fly ash and purifying in grading manner |
| CN116200605A (en) * | 2023-01-05 | 2023-06-02 | 中国科学院过程工程研究所 | Production method for efficiently removing impurities from copper enameled wire after paint removal |
| CN118006916A (en) * | 2024-04-07 | 2024-05-10 | 北京科技大学 | In-situ online copper removal process for crude lead |
| CN118006916B (en) * | 2024-04-07 | 2024-06-07 | 北京科技大学 | In-situ online copper removal process for crude lead |
| CN118006917A (en) * | 2024-04-08 | 2024-05-10 | 北京科技大学 | Method for reducing lead oxide slag source in electrolytic lead remelting process |
| CN118006917B (en) * | 2024-04-08 | 2024-06-28 | 北京科技大学 | Method for reducing lead oxide slag source in electrolytic lead remelting process |
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