CN116445740A - Separation method of lead-antimony alloy - Google Patents
Separation method of lead-antimony alloy Download PDFInfo
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- CN116445740A CN116445740A CN202310499433.5A CN202310499433A CN116445740A CN 116445740 A CN116445740 A CN 116445740A CN 202310499433 A CN202310499433 A CN 202310499433A CN 116445740 A CN116445740 A CN 116445740A
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- 229910001245 Sb alloy Inorganic materials 0.000 title claims abstract description 64
- 239000002140 antimony alloy Substances 0.000 title claims abstract description 64
- 238000000926 separation method Methods 0.000 title claims abstract description 63
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 176
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 176
- 238000009833 condensation Methods 0.000 claims abstract description 163
- 230000005494 condensation Effects 0.000 claims abstract description 163
- 238000011282 treatment Methods 0.000 claims abstract description 162
- 239000007788 liquid Substances 0.000 claims abstract description 97
- 238000000034 method Methods 0.000 claims abstract description 48
- 229910000978 Pb alloy Inorganic materials 0.000 claims abstract description 11
- 229910045601 alloy Inorganic materials 0.000 claims description 92
- 239000000956 alloy Substances 0.000 claims description 92
- 238000004321 preservation Methods 0.000 claims description 50
- PALNZFJYSCMLBK-UHFFFAOYSA-K magnesium;potassium;trichloride;hexahydrate Chemical group O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-].[Cl-].[K+] PALNZFJYSCMLBK-UHFFFAOYSA-K 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims 1
- 238000002844 melting Methods 0.000 abstract description 6
- 230000008018 melting Effects 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 238000009853 pyrometallurgy Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract 2
- 239000002893 slag Substances 0.000 description 21
- 239000000203 mixture Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000000155 melt Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- KGHMFMDJVUVBRY-UHFFFAOYSA-N antimony copper Chemical compound [Cu].[Sb] KGHMFMDJVUVBRY-UHFFFAOYSA-N 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- -1 firstly Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
-
- 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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
-
- 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
- C22B7/001—Dry processes
- C22B7/004—Dry processes separating two or more metals by melting out (liquation), i.e. heating above the temperature of the lower melting metal component(s); by fractional crystallisation (controlled freezing)
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the technical field of nonferrous metal pyrometallurgy, and particularly relates to a separation method of lead-antimony alloy. The method comprises the steps of performing first condensation treatment on lead-antimony alloy melt at a specific temperature, fishing out and completely melting solid antimony-rich melt after condensation is finished, and performing second condensation treatment at a temperature higher than that of the first condensation treatment; and sequentially carrying out third condensation treatment, fourth condensation treatment, fifth condensation treatment, sixth condensation treatment, seventh condensation treatment, eighth condensation treatment, ninth condensation treatment and tenth condensation treatment with gradually increased temperature according to the method, finally obtaining solid high-antimony alloy after the tenth condensation treatment, and collecting liquid in the ten condensation processes to obtain the high-lead alloy. The invention can realize the separation of antimony from lead-antimony alloy, has high universality of raw materials, does not introduce new impurities, and has simple separation method and low equipment requirement.
Description
Technical Field
The invention belongs to the technical field of nonferrous metal pyrometallurgy, and particularly relates to a separation method of lead-antimony alloy.
Background
In daily life, a large amount of lead-antimony alloy is contained in sliding bearings, counterweight materials, lead-acid storage battery grids and conductive parts, and the lead and the antimony recovered from the raw materials can bring high economic value each year.
At present, a centrifugal segregation method, a vacuum distillation separation method or a fused salt electrolysis method is generally adopted for treating the lead-antimony alloy. The centrifugal segregation method has low single-machine separation efficiency, is difficult to realize industrial production, has high material requirements on a high-speed rotor, and increases production cost; the vacuum distillation separation method has higher treatment temperature, needs to perform decompression operation in the whole process, has lower adaptability to materials, and greatly increases the workload and the power consumption when treating lead-antimony alloy with higher antimony content; the fused salt electrolysis method has the problems of long electrolysis period, large raw material consumption and the like, and simultaneously, the recycling of anode slime and the purification of electrolyte can further increase the workload and the working time, thereby causing environmental pollution.
Chinese patent publication No. CN109825719a discloses a separation method of lead-antimony alloy, firstly, alloy is continuously input into a rotary supergravity separation reaction chamber through a charging system, then a rotary supergravity reactor is started, and a reactor on a roller is driven to rotate by a speed regulating motor to generate a stable and adjustable supergravity field. Under the combined action of the supergravity field and the temperature field, the atomic diffusion and mass transfer process between the lead-antimony alloy is greatly accelerated, and the continuous separation between the lead-rich liquid and the antimony-rich melt is realized. However, the method has higher quality requirements on equipment such as rollers, filter plates and the like, and increases the production cost.
Chinese patent publication No. CN108842069a discloses a method for fire refining of lead-antimony alloy. Firstly, mixing lead-antimony alloy and pure copper to obtain a mixture, then melting the mixture under nitrogen or argon atmosphere, separating an antimony component from a lead component by utilizing the fact that the binding force between copper and antimony is larger than the binding force between lead and antimony, and finally obtaining pure lead with antimony removed by utilizing the difference between the melting points of the copper-antimony alloy and lead for crystallization separation. However, the method can introduce impurity metallic copper, and further prolong the whole separation process of the lead-antimony alloy.
Disclosure of Invention
The invention aims to provide a separation method of lead-antimony alloy, which can not introduce new impurities in the separation process, has high raw material universality, is simple and has low requirements on equipment.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a separation method of lead-antimony alloy, which comprises the following steps:
performing first condensation treatment on the lead-antimony alloy melt to obtain a first antimony-rich melt and a first alloy liquid; the temperature of the first condensation treatment is 290-310 ℃, and the heat preservation time is 1-2 h;
performing second condensation treatment on the first antimony-rich melt to obtain a second antimony-rich melt and a second alloy liquid; the temperature of the second condensation treatment is 360-380 ℃, and the heat preservation time is 1-2 h;
performing third condensation treatment on the second antimony-rich melt to obtain a third antimony-rich melt and a third alloy liquid; the temperature of the third condensation treatment is 430-450 ℃, and the heat preservation time is 1-2 h;
performing fourth condensation treatment on the third antimony-rich melt to obtain a fourth antimony-rich melt and a fourth alloy liquid; the temperature of the fourth condensation treatment is 490-510 ℃ and the heat preservation time is 1-2 h;
performing fifth condensation treatment on the fourth antimony-rich melt to obtain a fifth antimony-rich melt and a fifth alloy liquid; the temperature of the fifth condensation treatment is 540-560 ℃ and the heat preservation time is 1-2 h;
performing a sixth condensation treatment on the fifth antimony-rich melt to obtain a sixth antimony-rich melt and a sixth alloy liquid; the temperature of the sixth condensation treatment is 575-585 ℃, and the heat preservation time is 1-2 h;
performing seventh condensation treatment on the sixth antimony-rich melt to obtain a seventh antimony-rich melt and a seventh alloy liquid; the temperature of the seventh condensation treatment is 595-605 ℃, and the heat preservation time is 1-2 h;
performing eighth condensation treatment on the seventh antimony-rich melt to obtain an eighth antimony-rich melt and an eighth alloy liquid; the temperature of the eighth condensation treatment is 608-613 ℃, and the heat preservation time is 1-2 h;
performing a ninth condensation treatment on the eighth antimony-rich melt to obtain a ninth antimony-rich melt and a ninth alloy liquid; the temperature of the ninth condensation treatment is 618-623 ℃ and the heat preservation time is 1-2 h;
performing tenth condensation treatment on the ninth antimony-rich melt to obtain high-antimony alloy and tenth alloy liquid; the temperature of the tenth condensation treatment is 628-633 ℃, and the heat preservation time is 1-2 h.
Preferably, the mass percentage of antimony in the lead-antimony alloy melt is 11.2-95%.
Preferably, the temperature of the lead-antimony alloy melt is 400-800 ℃.
Preferably, the heating rates of the first condensation treatment, the second condensation treatment, the third condensation treatment, the fourth condensation treatment, the fifth condensation treatment, the sixth condensation treatment, the seventh condensation treatment, the eighth condensation treatment, the ninth condensation treatment and the tenth condensation treatment are all 20-40 ℃/min.
Preferably, a covering agent is added to the surface of the system during the first condensation treatment, the second condensation treatment, the third condensation treatment, the fourth condensation treatment, the fifth condensation treatment, the sixth condensation treatment, the seventh condensation treatment, the eighth condensation treatment, the ninth condensation treatment and the tenth condensation treatment.
Preferably, the covering agent is carnallite.
Preferably, the average particle size of the first antimony-rich melt, the second antimony-rich melt, the third antimony-rich melt, the fourth antimony-rich melt, the fifth antimony-rich melt, the sixth antimony-rich melt, the seventh antimony-rich melt, the eighth antimony-rich melt and the ninth antimony-rich melt is independently 40-80 μm.
Preferably, the grade of antimony in the high-antimony alloy is 98% or more.
Preferably, after the tenth condensation treatment, the method further comprises mixing the first alloy liquid, the second alloy liquid, the third alloy liquid, the fourth alloy liquid, the fifth alloy liquid, the sixth alloy liquid, the seventh alloy liquid, the eighth alloy liquid, the ninth alloy liquid and the tenth alloy liquid to obtain the high lead alloy.
Preferably, the grade of lead in the high lead alloy is 75-88.8 wt%.
The invention provides a separation method of lead-antimony alloy, which comprises the following steps: performing first condensation treatment on the lead-antimony alloy melt to obtain a first antimony-rich melt and a first alloy liquid; the temperature of the first condensation treatment is 290-310 ℃, and the heat preservation time is 1-2 h; performing second condensation treatment on the first antimony-rich melt to obtain a second antimony-rich melt and a second alloy liquid; the temperature of the second condensation treatment is 360-380 ℃, and the heat preservation time is 1-2 h; performing third condensation treatment on the second antimony-rich melt to obtain a third antimony-rich melt and a third alloy liquid; the temperature of the third condensation treatment is 430-450 ℃, and the heat preservation time is 1-2 h; performing fourth condensation treatment on the third antimony-rich melt to obtain a fourth antimony-rich melt and a fourth alloy liquid; the temperature of the fourth condensation treatment is 490-510 ℃ and the heat preservation time is 1-2 h; performing fifth condensation treatment on the fourth antimony-rich melt to obtain a fifth antimony-rich melt and a fifth alloy liquid; the temperature of the fifth condensation treatment is 540-560 ℃ and the heat preservation time is 1-2 h; performing a sixth condensation treatment on the fifth antimony-rich melt to obtain a sixth antimony-rich melt and a sixth alloy liquid; the temperature of the sixth condensation treatment is 575-585 ℃, and the heat preservation time is 1-2 h; performing seventh condensation treatment on the sixth antimony-rich melt to obtain a seventh antimony-rich melt and a seventh alloy liquid; the temperature of the seventh condensation treatment is 595-605 ℃, and the heat preservation time is 1-2 h; performing eighth condensation treatment on the seventh antimony-rich melt to obtain an eighth antimony-rich melt and an eighth alloy liquid; the temperature of the eighth condensation treatment is 608-613 ℃, and the heat preservation time is 1-2 h; performing a ninth condensation treatment on the eighth antimony-rich melt to obtain a ninth antimony-rich melt and a ninth alloy liquid; the temperature of the ninth condensation treatment is 618-623 ℃ and the heat preservation time is 1-2 h; performing tenth condensation treatment on the ninth antimony-rich melt to obtain high-antimony alloy and tenth alloy liquid; the temperature of the tenth condensation treatment is 628-633 ℃, and the heat preservation time is 1-2 h. The invention carries out condensation treatment under a limited procedure, can realize the separation of antimony from lead-antimony alloy, and has no impurity introduction and high separation efficiency in the separation process. The separation method provided by the invention is simple, has high universality of raw materials and low requirements on equipment.
Detailed Description
The invention provides a separation method of lead-antimony alloy, which comprises the following steps:
performing first condensation treatment on the lead-antimony alloy melt to obtain a first antimony-rich melt and a first alloy liquid; the temperature of the first condensation treatment is 290-310 ℃, and the heat preservation time is 1-2 h;
performing second condensation treatment on the first antimony-rich melt to obtain a second antimony-rich melt and a second alloy liquid; the temperature of the second condensation treatment is 360-380 ℃, and the heat preservation time is 1-2 h;
performing third condensation treatment on the second antimony-rich melt to obtain a third antimony-rich melt and a third alloy liquid; the temperature of the third condensation treatment is 430-450 ℃, and the heat preservation time is 1-2 h;
performing fourth condensation treatment on the third antimony-rich melt to obtain a fourth antimony-rich melt and a fourth alloy liquid; the temperature of the fourth condensation treatment is 490-510 ℃ and the heat preservation time is 1-2 h;
performing fifth condensation treatment on the fourth antimony-rich melt to obtain a fifth antimony-rich melt and a fifth alloy liquid; the temperature of the fifth condensation treatment is 540-560 ℃ and the heat preservation time is 1-2 h;
performing a sixth condensation treatment on the fifth antimony-rich melt to obtain a sixth antimony-rich melt and a sixth alloy liquid; the temperature of the sixth condensation treatment is 575-585 ℃, and the heat preservation time is 1-2 h;
performing seventh condensation treatment on the sixth antimony-rich melt to obtain a seventh antimony-rich melt and a seventh alloy liquid; the temperature of the seventh condensation treatment is 595-605 ℃, and the heat preservation time is 1-2 h;
performing eighth condensation treatment on the seventh antimony-rich melt to obtain an eighth antimony-rich melt and an eighth alloy liquid; the temperature of the eighth condensation treatment is 608-613 ℃, and the heat preservation time is 1-2 h;
performing a ninth condensation treatment on the eighth antimony-rich melt to obtain a ninth antimony-rich melt and a ninth alloy liquid; the temperature of the ninth condensation treatment is 618-623 ℃ and the heat preservation time is 1-2 h;
performing tenth condensation treatment on the ninth antimony-rich melt to obtain high-antimony alloy and tenth alloy liquid; the temperature of the tenth condensation treatment is 628-633 ℃, and the heat preservation time is 1-2 h.
In the present invention, the content of antimony in the lead-antimony alloy melt is preferably 11.2 to 95% by mass, more preferably 15 to 90% by mass, and still more preferably 20 to 80% by mass.
In the present invention, the temperature of the lead-antimony alloy melt is preferably 400 to 800 ℃, more preferably 450 to 700 ℃, and even more preferably 500 to 600 ℃.
In the present invention, the temperature of the first condensation treatment is 290 to 310 ℃, more preferably 295 to 305 ℃, still more preferably 300 ℃; the heat preservation time is 1-2 h. After the first condensation treatment, the method of the invention further preferably comprises separating the first antimony-rich melt from the first alloy liquid, wherein the separation method is preferably that the first antimony-rich melt is fished out of the first alloy liquid for slag separation. The process of the slag separation is not particularly limited, and the process is well known to those skilled in the art. In the invention, the mass percentage of antimony in the first antimony-rich melt is preferably 30-83%; the mass percentage of lead is preferably 17-70%.
In the present invention, the temperature of the second condensation treatment is 360 to 380 ℃, more preferably 365 to 375 ℃, still more preferably 370 ℃; the heat preservation time is 1-2 h. After the second condensation treatment, the method of the invention also preferably comprises separating the second antimony-rich melt from the second alloy liquid, wherein the separation method is preferably that the second antimony-rich melt is fished out of the second alloy liquid for slag separation. The process of the slag separation is not particularly limited, and the process is well known to those skilled in the art. In the invention, the mass percentage of antimony in the second antimony-rich melt is preferably 40-85%; the mass percentage of lead is preferably 15-60%.
In the present invention, the temperature of the third condensation treatment is 430 to 450 ℃, more preferably 435 to 445 ℃, still more preferably 440 ℃; the heat preservation time is 1-2 h. After the third condensation treatment, the method of the invention further preferably comprises separating the third antimony-rich melt from the third alloy liquid, wherein the separation method is preferably that the third antimony-rich melt is fished out of the third alloy liquid for slag separation. The process of the slag separation is not particularly limited, and the process is well known to those skilled in the art. In the invention, the mass percentage of antimony in the third antimony-rich melt is preferably 53-87%; the mass percentage of lead is preferably 17-45%.
In the present invention, the temperature of the fourth condensation treatment is 490 to 510 ℃, more preferably 495 to 505 ℃, still more preferably 500 ℃; the heat preservation time is 1-2 h. After the fourth condensation treatment, the method of the invention further preferably comprises separating the fourth antimony-rich melt from the fourth alloy liquid, wherein the separation method is preferably that the fourth antimony-rich melt is fished out of the fourth alloy liquid for slag separation. The process of the slag separation is not particularly limited, and the process is well known to those skilled in the art. In the invention, the mass percentage of antimony in the fourth antimony-rich melt is preferably 65-88%; the mass percentage of lead is preferably 12-35%.
In the present invention, the temperature of the fifth condensation treatment is 540 to 560 ℃, more preferably 545 to 555 ℃, and still more preferably 550 ℃; the heat preservation time is 1-2 h. After the fifth condensation treatment, the method of the invention further preferably comprises separating the fifth antimony-rich melt from the fifth alloy liquid, wherein the separation method is preferably that the fifth antimony-rich melt is fished out of the fifth alloy liquid for slag separation. The process of the slag separation is not particularly limited, and the process is well known to those skilled in the art. In the invention, the mass percentage of antimony in the fifth antimony-rich melt is preferably 77-90%; the mass percentage of lead is preferably 10-23%.
In the present invention, the temperature of the sixth condensation treatment is 575 to 585 ℃, more preferably 578 to 582 ℃, still more preferably 580 ℃; the heat preservation time is 1-2 h. After the sixth condensation treatment, the method of the invention further preferably comprises separating the sixth antimony-rich melt from the sixth alloy liquid, wherein the separation method is preferably that the sixth antimony-rich melt is fished out of the sixth alloy liquid for slag separation. The process of the slag separation is not particularly limited, and the process is well known to those skilled in the art. In the invention, the mass percentage of antimony in the sixth antimony-rich melt is preferably 86-91%; the mass percentage of lead is preferably 9-14%.
In the present invention, the temperature of the seventh condensation treatment is 595 to 605 ℃, more preferably 598 to 602 ℃, still more preferably 600 ℃; the heat preservation time is 1-2 h. After the seventh condensation treatment, the invention also preferably comprises separating the seventh antimony-rich melt from the seventh alloy liquid, wherein the separation method preferably comprises the step of slag skimming and separating the seventh antimony-rich melt from the inside of the seventh alloy liquid. The process of the slag separation is not particularly limited, and the process is well known to those skilled in the art. In the invention, the mass percentage of antimony in the seventh antimony-rich melt is preferably 92-94%; the mass percentage of lead is preferably 6-8%.
In the present invention, the temperature of the eighth condensation treatment is 608 to 613 ℃, more preferably 609 to 611 ℃, still more preferably 610 ℃; the heat preservation time is 1-2 h. After the eighth condensation treatment, the method of the invention further preferably comprises separating the eighth antimony-rich melt from the eighth alloy liquid, wherein the separation method is preferably that the eighth antimony-rich melt is fished out of the eighth alloy liquid for slag separation. The process of the slag separation is not particularly limited, and the process is well known to those skilled in the art. In the invention, the mass percentage of antimony in the eighth antimony-rich melt is preferably 95-97%; the mass percentage of lead is preferably 3-5%.
In the present invention, the temperature of the ninth condensation treatment is 618 to 623 ℃, more preferably 619 to 621 ℃, still more preferably 620 ℃; the heat preservation time is 1-2 h. After the ninth condensation treatment, the method of the invention further preferably comprises separating the ninth antimony-rich melt from the ninth alloy liquid, wherein the separation method is preferably that the ninth antimony-rich melt is fished out of the ninth alloy liquid for slag separation. The process of the slag separation is not particularly limited, and the process is well known to those skilled in the art. In the invention, the mass percentage of antimony in the ninth antimony-rich melt is preferably 97-99%; the mass percentage of lead is preferably 1-3%.
In the present invention, the temperature of the tenth condensation treatment is 628 to 633 ℃, more preferably 631 to 633 ℃, and still more preferably 633 ℃; the heat preservation time is 1-2 h. After the tenth condensation treatment, the present invention further preferably includes separating the high-antimony alloy from the tenth alloy liquid, and the separation method is preferably a method of skimming and separating the high-antimony alloy from the inside of the tenth alloy liquid. The process of the slag separation is not particularly limited, and the process is well known to those skilled in the art.
In the present invention, the heating rates of the first, second, third, fourth, fifth, sixth, seventh, eighth, ninth, and tenth condensation are preferably 20 to 40 ℃/min.
In the present invention, it is preferable that a covering agent is added to the surface of the system during the first, second, third, fourth, fifth, sixth, seventh, eighth, ninth, and tenth condensation treatments. In the present invention, the covering agent is preferably carnallite. The amount of the covering agent to be added in the present invention is not particularly limited, and may be any one known to those skilled in the art. In the present invention, the surface of the system is added with a covering agent, so that oxidation during condensation can be prevented.
In the condensation treatment process of the invention, the heating temperature set by ten heating devices is required to be ensured to be the same as the alloy temperature correspondingly heated, so that the necessary condition that the antimony-rich melt can be stably precipitated is formed. Because the solubility of the antimony-rich melt and the lead-antimony alloy melt at a limited temperature is different between solid phases, the antimony-rich melt enters the solid phase in the condensation process, is separated out from the lead-antimony alloy melt, and is separated from the lead-antimony alloy melt by adopting a slag dragging means. In the separation process, the entrainment phenomenon of part of the lead-antimony alloy melt cannot be avoided, so that the fished-out antimony-rich melt is melted again to obtain the lead-antimony alloy melt with higher antimony content. The melting point of lead is lower than that of antimony, so that in the process of continuously carrying out slag dragging, melting and condensation, the melting point of the lead-antimony alloy melt is gradually increased along with the gradual increase of the antimony content in the lead-antimony alloy melt after the antimony-rich melt is melted, and in order to separate the antimony-rich melt with higher antimony content from the lead-antimony alloy melt and finally obtain high-antimony alloy, the high-antimony alloy needs to be subjected to gradual heating condensation treatment with gradual temperature rise. And along with the continuous proceeding of the gradient heating treatment process, finally obtaining the high-antimony alloy after the tenth condensation process, obviously reducing the antimony content in the residual lead-antimony alloy melt, and collecting the high-lead alloy.
In the invention, the average particle size of the first antimony-rich melt, the second antimony-rich melt, the third antimony-rich melt, the fourth antimony-rich melt, the fifth antimony-rich melt, the sixth antimony-rich melt, the seventh antimony-rich melt, the eighth antimony-rich melt and the ninth antimony-rich melt is preferably 40-80 μm independently.
In the present invention, the grade of antimony in the high-antimony alloy is preferably 98% or more, more preferably 98 to 99.6%, and still more preferably 99 to 99.5%. In the present invention, the recovery rate of metallic antimony is preferably 98% or more.
After the tenth condensation treatment, the present invention preferably further includes mixing the first alloy liquid, the second alloy liquid, the third alloy liquid, the fourth alloy liquid, the fifth alloy liquid, the sixth alloy liquid, the seventh alloy liquid, the eighth alloy liquid, the ninth alloy liquid and the tenth alloy liquid to obtain the high lead alloy.
In the present invention, the grade of lead in the high lead alloy is preferably 75 to 88.8%, more preferably 75 to 88%, and even more preferably 80 to 87%. In the present invention, the recovery rate of the high lead alloy is preferably 98% or more.
After the high-antimony alloy and the high-lead alloy are obtained, the invention also preferably comprises the steps of respectively purifying the high-antimony alloy and the high-lead alloy, and the grade of refined antimony and refined lead obtained after purification is preferably more than 99.9 percent. The process of the purification treatment is not particularly limited, and may be performed by a process known to those skilled in the art.
The lead-antimony alloy separation method provided by the invention has high universality of raw materials, and can be used for treating lead-antimony alloy with wide antimony content range; the separation method is simple; no new impurities are introduced; the equipment requirement is low, and the operation cost can be reduced.
In order to further illustrate the present invention, a method for separating lead-antimony alloys according to the present invention will be described in detail with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
100kg of molten lead-antimony alloy having a temperature of 500 ℃ in which the mass percentage of antimony is preferably 21.56% and the mass percentage of lead is preferably 78.22% was covered by adding carnallite to the liquid surface, and performing a condensation treatment under carnallite-covered conditions in which the average particle size of the first, second, third, fourth, fifth, sixth, seventh, eighth and ninth antimony-rich melts is 78.85 μm, and the conditions of the condensation treatment are as shown in table 1, and the composition of the product obtained during the condensation treatment is as shown in table 2.
Example 2
100kg of molten lead-antimony alloy having a temperature of 550 ℃ in which the mass percentage of antimony is preferably 41.24% and the mass percentage of lead is preferably 58.69% was covered by adding carnallite to the liquid surface, and performing a condensation treatment under carnallite-covered conditions in which the average particle size of the first, second, third, fourth, fifth, sixth, seventh, eighth and ninth antimony-rich melts is 72.29 μm, and the conditions of the condensation treatment are as shown in table 1, and the composition of the product obtained during the condensation treatment is as shown in table 2.
Example 3
100kg of molten lead-antimony alloy at a temperature of 575 c, in which the mass percentage of antimony is preferably 62.59% and the mass percentage of lead is preferably 37.36%, was covered by adding carnallite on the surface of the liquid, and subjected to a condensation treatment under carnallite-covered conditions, the average particle diameters of the first, second, third, fourth, fifth, sixth, seventh, eighth and ninth antimony-rich melts being 68.87 μm, and the conditions of the condensation treatment being as shown in table 1, and the composition of the product obtained during the condensation treatment being as shown in table 2.
Example 4
100kg of molten lead-antimony alloy at 630 deg.c, in which the mass percentage of antimony is preferably 79.35% and the mass percentage of lead is preferably 20.63%, was covered with carnallite on the surface of the liquid, and subjected to a condensation treatment under carnallite-covered conditions, the average particle diameters of the first, second, third, fourth, fifth, sixth, seventh, eighth and ninth antimony-rich melts being 62.05 μm, and the conditions of the condensation treatment being as shown in table 1, and the composition of the product obtained during the condensation treatment being as shown in table 2.
Comparative example 1
100kg of molten lead-antimony alloy having a temperature of 500 ℃ in which the mass percentage of antimony is preferably 21.56% and the mass percentage of lead is preferably 78.22% was covered by adding carnallite to the liquid surface, and performing a condensation treatment under carnallite-covered conditions in which the average particle size of the first, second, third, fourth, fifth, sixth, seventh, eighth and ninth antimony-rich melts is 42.68 μm, and the conditions of the condensation treatment are as shown in table 1, and the composition of the product obtained during the condensation treatment is as shown in table 2.
TABLE 1 Condition parameters of the coagulation treatment in examples 1 to 4 and comparative example 1
TABLE 2 composition tables of products during gradient treatment of examples 1 to 4 and comparative example 1
As can be seen from Table 2, the present invention requires precise control of the temperature of each heating treatment to separate antimony from the lead high antimony alloy.
Although the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments may be obtained according to the present embodiments without departing from the scope of the invention.
Claims (10)
1. A method for separating lead-antimony alloy, comprising the steps of:
performing first condensation treatment on the lead-antimony alloy melt to obtain a first antimony-rich melt and a first alloy liquid; the temperature of the first condensation treatment is 290-310 ℃, and the heat preservation time is 1-2 h;
performing second condensation treatment on the first antimony-rich melt to obtain a second antimony-rich melt and a second alloy liquid; the temperature of the second condensation treatment is 360-380 ℃, and the heat preservation time is 1-2 h;
performing third condensation treatment on the second antimony-rich melt to obtain a third antimony-rich melt and a third alloy liquid; the temperature of the third condensation treatment is 430-450 ℃, and the heat preservation time is 1-2 h;
performing fourth condensation treatment on the third antimony-rich melt to obtain a fourth antimony-rich melt and a fourth alloy liquid; the temperature of the fourth condensation treatment is 490-510 ℃ and the heat preservation time is 1-2 h;
performing fifth condensation treatment on the fourth antimony-rich melt to obtain a fifth antimony-rich melt and a fifth alloy liquid; the temperature of the fifth condensation treatment is 540-560 ℃ and the heat preservation time is 1-2 h;
performing a sixth condensation treatment on the fifth antimony-rich melt to obtain a sixth antimony-rich melt and a sixth alloy liquid; the temperature of the sixth condensation treatment is 575-585 ℃, and the heat preservation time is 1-2 h;
performing seventh condensation treatment on the sixth antimony-rich melt to obtain a seventh antimony-rich melt and a seventh alloy liquid; the temperature of the seventh condensation treatment is 595-605 ℃, and the heat preservation time is 1-2 h;
performing eighth condensation treatment on the seventh antimony-rich melt to obtain an eighth antimony-rich melt and an eighth alloy liquid; the temperature of the eighth condensation treatment is 608-613 ℃, and the heat preservation time is 1-2 h;
performing a ninth condensation treatment on the eighth antimony-rich melt to obtain a ninth antimony-rich melt and a ninth alloy liquid; the temperature of the ninth condensation treatment is 618-623 ℃ and the heat preservation time is 1-2 h;
performing tenth condensation treatment on the ninth antimony-rich melt to obtain high-antimony alloy and tenth alloy liquid; the temperature of the tenth condensation treatment is 628-633 ℃, and the heat preservation time is 1-2 h.
2. The separation method according to claim 1, wherein the mass percentage of antimony in the lead-antimony alloy melt is 11.2-95%.
3. The separation method according to claim 1 or 2, characterized in that the temperature of the lead-antimony alloy melt is 400-800 ℃.
4. The separation method according to claim 1, wherein the first, second, third, fourth, fifth, sixth, seventh, eighth, ninth, and tenth condensation treatments each have a temperature rise rate of 20 to 40 ℃/min.
5. The separation method according to claim 1, wherein a covering agent is added to the surface of the system during each of the first, second, third, fourth, fifth, sixth, seventh, eighth, ninth, and tenth condensation treatments.
6. The separation method of claim 5, wherein the coating agent is carnallite.
7. The separation method according to claim 1, wherein the average particle size of the first antimony-rich melt, the second antimony-rich melt, the third antimony-rich melt, the fourth antimony-rich melt, the fifth antimony-rich melt, the sixth antimony-rich melt, the seventh antimony-rich melt, the eighth antimony-rich melt and the ninth antimony-rich melt is independently 40 to 80 μm.
8. The separation method according to claim 1 or 7, wherein the grade of antimony in the high-antimony alloy is 98% or more.
9. The separation method according to claim 1, further comprising mixing the first alloy liquid, the second alloy liquid, the third alloy liquid, the fourth alloy liquid, the fifth alloy liquid, the sixth alloy liquid, the seventh alloy liquid, the eighth alloy liquid, the ninth alloy liquid, and the tenth alloy liquid after the tenth condensation treatment, to obtain a high lead alloy.
10. The separation method according to claim 9, wherein the grade of lead in the high lead alloy is 75 to 88.8wt%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117887980A (en) * | 2024-01-17 | 2024-04-16 | 昆明理工大学 | Method for separating and recovering antimony from lead-antimony alloy |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117887980A (en) * | 2024-01-17 | 2024-04-16 | 昆明理工大学 | Method for separating and recovering antimony from lead-antimony alloy |
| 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 |
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