A method for separating a lead-antimony alloy
Patent Information
- Application Number
- CN202310499433.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-05
- Publication Date
- 2026-09-11
- Estimated Expiration
- 2043-05-05
AI Technical Summary
但是上述方法会引入杂质金属铜,进一步延长整个铅锑合金的分离过程
[0028]This invention provides a method for separating lead-antimony alloys, comprising the following steps: subjecting a lead-antimony alloy molten liquid to a first condensation treatment to obtain a first antimony-rich melt and a first alloy liquid; the temperature of the first condensation treatment is 290–310°C, and the holding time is 1–2 h; subjecting the first antimony-rich melt to a second condensation treatment to obtain a second antimony-rich melt and a second alloy liquid; the temperature of the second condensation treatment is 360–380°C, and the holding time is 1–2 h; subjecting the second antimony-rich melt to a third condensation treatment to obtain a third antimony-rich melt and a third alloy liquid; the temperature of the third condensation treatment is 430–450°C, and the holding time is 1–2 h; subjecting the third antimony-rich melt to a fourth condensation treatment to obtain a fourth antimony-rich melt and a fourth alloy liquid; the temperature of the fourth condensation treatment is 490–510°C, and the holding time is 1–2 h; subjecting the fourth antimony-rich melt to a fifth condensation treatment to obtain a fifth antimony-rich melt and a fifth alloy liquid; the temperature of the fifth condensation treatment is 540–560°C. The fifth antimony-rich melt is subjected to a sixth condensation treatment at 0℃ for 1–2 hours to obtain a sixth antimony-rich melt and a sixth alloy liquid. The sixth condensation treatment is performed at 575–585℃ for 1–2 hours. The sixth antimony-rich melt is then subjected to a seventh condensation treatment at 595–605℃ for 1–2 hours to obtain a seventh antimony-rich melt and a seventh alloy liquid. The seventh condensation treatment is performed at 595–605℃ for 1–2 hours. The seventh antimony-rich melt is then subjected to an eighth condensation treatment to obtain an eighth antimony-rich melt. The process involves a melt and an eighth alloy liquid; the eighth condensation treatment is performed at a temperature of 608–613°C for 1–2 hours; the eighth antimony-rich melt is then subjected to a ninth condensation treatment to obtain a ninth antimony-rich melt and a ninth alloy liquid; the ninth condensation treatment is performed at a temperature of 618–623°C for 1–2 hours; the ninth antimony-rich melt is then subjected to a tenth condensation treatment to obtain a high-antimony alloy and a tenth alloy liquid; the tenth condensation treatment is performed at a temperature of 628–633°C for 1–2 hours. This invention, through a defined procedure, enables the separation of antimony from lead-antimony alloys, with no impurities introduced during the separation process and high separation efficiency. The separation method provided by this invention is simple, has high raw material applicability, and low equipment requirements.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of non-ferrous metal pyrometallurgical technology, and specifically relates to a method for separating lead-antimony alloys. Background Technology
[0002] In daily life, widely used sliding bearings, counterweight materials, lead-acid battery grids, and conductive parts contain a large amount of lead-antimony alloys. The lead and antimony recovered from these raw materials each year can bring high economic value.
[0003] Currently, lead-antimony alloys are generally processed using centrifugal segregation, vacuum distillation, or molten salt electrolysis. Centrifugal segregation has low single-machine separation efficiency, making industrial-scale production difficult. It also requires high-quality materials for the high-speed rotor, increasing production costs. Vacuum distillation involves high processing temperatures, requires constant pressure reduction, and has low adaptability to materials; when processing lead-antimony alloys with high antimony content, it significantly increases workload and power consumption. Molten salt electrolysis suffers from long electrolysis cycles and high raw material consumption. Furthermore, the recovery of anode mud and purification of the electrolyte further increase workload and processing time, causing environmental pollution.
[0004] Chinese patent CN109825719A discloses a method for separating lead-antimony alloys. First, the alloy is continuously fed into a rotating hypergravity separation reaction chamber via a feeding system. Then, the rotating hypergravity reactor is activated, and a stable, adjustable hypergravity field is generated by rotating the reactor on a roller driven by a speed-regulating motor. Under the combined action of the hypergravity field and the temperature field, the atomic diffusion and mass transfer processes between the lead-antimony alloys are greatly accelerated, achieving continuous separation between lead-rich liquid and antimony-rich melt. However, this method places high demands on the quality of equipment such as rollers and filter plates, increasing production costs.
[0005] Chinese patent CN108842069A discloses a pyrometallurgical refining method for lead-antimony alloys. First, the lead-antimony alloy is mixed with pure copper to obtain a mixture. Then, it is melted under a nitrogen or argon atmosphere. Taking advantage of the greater bonding force between copper and antimony than between lead and antimony, the antimony component is separated from the lead component. Then, utilizing the difference in melting points between the copper-antimony alloy and lead, crystallization separation is performed, ultimately yielding pure lead free of antimony. However, this method introduces copper impurities, further prolonging the entire lead-antimony alloy separation process. Summary of the Invention
[0006] The purpose of this invention is to provide a method for separating lead-antimony alloys. The separation process provided by this invention does not introduce new impurities, and the raw materials used in the separation method are highly versatile, the method is simple, and the equipment requirements are low.
[0007] To achieve the above objectives, the present invention provides the following technical solution:
[0008] This invention provides a method for separating lead-antimony alloys, comprising the following steps:
[0009] The lead-antimony alloy molten liquid is subjected to a first condensation treatment to obtain a first antimony-rich melt and a first alloy liquid; the temperature of the first condensation treatment is 290-310℃, and the holding time is 1-2h;
[0010] The first antimony-rich melt is subjected to a second condensation treatment to obtain a second antimony-rich melt and a second alloy liquid; the temperature of the second condensation treatment is 360-380℃, and the holding time is 1-2h.
[0011] The second antimony-rich melt is subjected to a third condensation treatment to obtain a third antimony-rich melt and a third alloy liquid; the temperature of the third condensation treatment is 430-450℃, and the holding time is 1-2h.
[0012] The third antimony-rich melt is subjected to a fourth condensation treatment to obtain a fourth antimony-rich melt and a fourth alloy liquid; the temperature of the fourth condensation treatment is 490-510℃, and the holding time is 1-2h.
[0013] The fourth antimony-rich melt is subjected to a fifth condensation treatment to obtain a fifth antimony-rich melt and a fifth alloy liquid; the temperature of the fifth condensation treatment is 540-560℃, and the holding time is 1-2h.
[0014] The fifth antimony-rich melt is subjected to a sixth condensation treatment to obtain a sixth antimony-rich melt and a sixth alloy liquid; the temperature of the sixth condensation treatment is 575-585℃, and the holding time is 1-2h.
[0015] The sixth antimony-rich melt is subjected to a seventh condensation treatment to obtain a seventh antimony-rich melt and a seventh alloy liquid; the temperature of the seventh condensation treatment is 595-605℃, and the holding time is 1-2h.
[0016] The seventh antimony-rich melt is subjected to an eighth condensation treatment to obtain an eighth antimony-rich melt and an eighth alloy liquid; the temperature of the eighth condensation treatment is 608-613℃, and the holding time is 1-2h.
[0017] The eighth antimony-rich melt is subjected to a ninth condensation treatment to obtain a ninth antimony-rich melt and a ninth alloy liquid; the temperature of the ninth condensation treatment is 618-623℃, and the holding time is 1-2h.
[0018] The ninth antimony-rich melt is subjected to a tenth condensation treatment to obtain a high-antimony alloy and a tenth alloy liquid; the temperature of the tenth condensation treatment is 628-633℃, and the holding time is 1-2h.
[0019] Preferably, the antimony content in the lead-antimony alloy molten liquid is 11.2% to 95% by mass.
[0020] Preferably, the temperature of the lead-antimony alloy melt is 400–800°C.
[0021] Preferably, the heating rate 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 is 20 to 40 °C / min.
[0022] Preferably, 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.
[0023] Preferably, the covering agent is carnallite.
[0024] Preferably, the average particle size of the first, second, third, fourth, fifth, sixth, seventh, eighth, and ninth antimony-rich melts is independently 40–80 μm.
[0025] Preferably, the antimony content in the high-antimony alloy is 98% or higher.
[0026] Preferably, after the tenth condensation treatment, the mixture 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 a high-lead alloy.
[0027] Preferably, the lead content in the high-lead alloy is 75–88.8 wt%.
[0028] This invention provides a method for separating lead-antimony alloys, comprising the following steps: subjecting a lead-antimony alloy molten liquid to a first condensation treatment to obtain a first antimony-rich melt and a first alloy liquid; the temperature of the first condensation treatment is 290–310°C, and the holding time is 1–2 h; subjecting the first antimony-rich melt to a second condensation treatment to obtain a second antimony-rich melt and a second alloy liquid; the temperature of the second condensation treatment is 360–380°C, and the holding time is 1–2 h; subjecting the second antimony-rich melt to a third condensation treatment to obtain a third antimony-rich melt and a third alloy liquid; the temperature of the third condensation treatment is 430–450°C, and the holding time is 1–2 h; subjecting the third antimony-rich melt to a fourth condensation treatment to obtain a fourth antimony-rich melt and a fourth alloy liquid; the temperature of the fourth condensation treatment is 490–510°C, and the holding time is 1–2 h; subjecting the fourth antimony-rich melt to a fifth condensation treatment to obtain a fifth antimony-rich melt and a fifth alloy liquid; the temperature of the fifth condensation treatment is 540–560°C. The fifth antimony-rich melt is subjected to a sixth condensation treatment at 0℃ for 1–2 hours to obtain a sixth antimony-rich melt and a sixth alloy liquid. The sixth condensation treatment is performed at 575–585℃ for 1–2 hours. The sixth antimony-rich melt is then subjected to a seventh condensation treatment at 595–605℃ for 1–2 hours to obtain a seventh antimony-rich melt and a seventh alloy liquid. The seventh condensation treatment is performed at 595–605℃ for 1–2 hours. The seventh antimony-rich melt is then subjected to an eighth condensation treatment to obtain an eighth antimony-rich melt. The process involves a melt and an eighth alloy liquid; the eighth condensation treatment is performed at a temperature of 608–613°C for 1–2 hours; the eighth antimony-rich melt is then subjected to a ninth condensation treatment to obtain a ninth antimony-rich melt and a ninth alloy liquid; the ninth condensation treatment is performed at a temperature of 618–623°C for 1–2 hours; the ninth antimony-rich melt is then subjected to a tenth condensation treatment to obtain a high-antimony alloy and a tenth alloy liquid; the tenth condensation treatment is performed at a temperature of 628–633°C for 1–2 hours. This invention, through a defined procedure, enables the separation of antimony from lead-antimony alloys, with no impurities introduced during the separation process and high separation efficiency. The separation method provided by this invention is simple, has high raw material applicability, and low equipment requirements. Detailed Implementation
[0029] This invention provides a method for separating lead-antimony alloys, comprising the following steps:
[0030] The lead-antimony alloy molten liquid is subjected to a first condensation treatment to obtain a first antimony-rich melt and a first alloy liquid; the temperature of the first condensation treatment is 290-310℃, and the holding time is 1-2h;
[0031] The first antimony-rich melt is subjected to a second condensation treatment to obtain a second antimony-rich melt and a second alloy liquid; the temperature of the second condensation treatment is 360-380℃, and the holding time is 1-2h.
[0032] The second antimony-rich melt is subjected to a third condensation treatment to obtain a third antimony-rich melt and a third alloy liquid; the temperature of the third condensation treatment is 430-450℃, and the holding time is 1-2h.
[0033] The third antimony-rich melt is subjected to a fourth condensation treatment to obtain a fourth antimony-rich melt and a fourth alloy liquid; the temperature of the fourth condensation treatment is 490-510℃, and the holding time is 1-2h.
[0034] The fourth antimony-rich melt is subjected to a fifth condensation treatment to obtain a fifth antimony-rich melt and a fifth alloy liquid; the temperature of the fifth condensation treatment is 540-560℃, and the holding time is 1-2h.
[0035] The fifth antimony-rich melt is subjected to a sixth condensation treatment to obtain a sixth antimony-rich melt and a sixth alloy liquid; the temperature of the sixth condensation treatment is 575-585℃, and the holding time is 1-2h.
[0036] The sixth antimony-rich melt is subjected to a seventh condensation treatment to obtain a seventh antimony-rich melt and a seventh alloy liquid; the temperature of the seventh condensation treatment is 595-605℃, and the holding time is 1-2h.
[0037] The seventh antimony-rich melt is subjected to an eighth condensation treatment to obtain an eighth antimony-rich melt and an eighth alloy liquid; the temperature of the eighth condensation treatment is 608-613℃, and the holding time is 1-2h.
[0038] The eighth antimony-rich melt is subjected to a ninth condensation treatment to obtain a ninth antimony-rich melt and a ninth alloy liquid; the temperature of the ninth condensation treatment is 618-623℃, and the holding time is 1-2h.
[0039] The ninth antimony-rich melt is subjected to a tenth condensation treatment to obtain a high-antimony alloy and a tenth alloy liquid; the temperature of the tenth condensation treatment is 628-633℃, and the holding time is 1-2h.
[0040] In this invention, the mass percentage of antimony in the lead-antimony alloy melt is preferably 11.2-95%, more preferably 15-90%, and even more preferably 20-80%.
[0041] In this invention, the temperature of the lead-antimony alloy melt is preferably 400-800°C, more preferably 450-700°C, and even more preferably 500-600°C.
[0042] In this invention, the temperature of the first condensation treatment is 290–310°C, more preferably 295–305°C, and even more preferably 300°C; the holding time is 1–2 hours. After the first condensation treatment, this invention preferably further includes separating the first antimony-rich melt and the first alloy liquid, and the separation method is preferably to remove slag from the interior of the first antimony-rich melt. This invention does not have a specific limitation on the slag removal process, and any method well known to those skilled in the art can be used. In this 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%.
[0043] In this invention, the temperature of the second condensation treatment is 360–380°C, more preferably 365–375°C, and even more preferably 370°C; the holding time is 1–2 hours. After the second condensation treatment, this invention preferably further includes separating the second antimony-rich melt and the second alloy liquid. The separation method is preferably to remove slag from the interior of the second antimony-rich melt. This invention does not have a specific limitation on the slag removal process, and any method well known to those skilled in the art can be used. In this 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%.
[0044] In this invention, the temperature of the third condensation treatment is 430–450°C, more preferably 435–445°C, and even more preferably 440°C; the holding time is 1–2 hours. After the third condensation treatment, this invention preferably further includes separating the third antimony-rich melt and the third alloy liquid, and the separation method is preferably to remove slag from the interior of the third alloy liquid. This invention does not have a specific limitation on the slag removal process, and any method well known to those skilled in the art can be used. In this 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%.
[0045] In this invention, the temperature of the fourth condensation treatment is 490–510°C, more preferably 495–505°C, and even more preferably 500°C; the holding time is 1–2 hours. After the fourth condensation treatment, this invention preferably further includes separating the fourth antimony-rich melt and the fourth alloy liquid, and the separation method is preferably to remove slag from the interior of the fourth alloy liquid. This invention does not have a specific limitation on the slag removal process, and any method well known to those skilled in the art can be used. In this 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%.
[0046] In this invention, the temperature of the fifth condensation treatment is 540–560°C, more preferably 545–555°C, and even more preferably 550°C; the holding time is 1–2 hours. After the fifth condensation treatment, this invention preferably further includes separating the fifth antimony-rich melt and the fifth alloy liquid, and the separation method is preferably to remove slag from the interior of the fifth antimony-rich melt. This invention does not have a specific limitation on the slag removal process, and any method well known to those skilled in the art can be used. In this 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%.
[0047] In this invention, the temperature of the sixth condensation treatment is 575–585°C, more preferably 578–582°C, and even more preferably 580°C; the holding time is 1–2 hours. After the sixth condensation treatment, this invention preferably further includes separating the sixth antimony-rich melt and the sixth alloy liquid, and the separation method is preferably to remove slag from the interior of the sixth alloy liquid. This invention does not have a specific limitation on the slag removal process, and any method well known to those skilled in the art can be used. In this 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%.
[0048] In this invention, the temperature of the seventh condensation treatment is 595–605°C, more preferably 598–602°C, and even more preferably 600°C; the holding time is 1–2 hours. After the seventh condensation treatment, this invention preferably further includes separating the seventh antimony-rich melt and the seventh alloy liquid, and the separation method is preferably to remove slag from the interior of the seventh alloy liquid. This invention does not have a specific limitation on the slag removal process, and any method well known to those skilled in the art can be used. In this 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%.
[0049] In this invention, the temperature of the eighth condensation treatment is 608–613°C, more preferably 609–611°C, and even more preferably 610°C; the holding time is 1–2 hours. After the eighth condensation treatment, this invention preferably further includes separating the eighth antimony-rich melt and the eighth alloy liquid, and the separation method is preferably to remove slag from the interior of the eighth antimony-rich melt. This invention does not have a specific limitation on the slag removal process, and any method well known to those skilled in the art can be used. In this 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%.
[0050] In this invention, the temperature of the ninth condensation treatment is 618–623°C, more preferably 619–621°C, and even more preferably 620°C; the holding time is 1–2 hours. After the ninth condensation treatment, this invention preferably further includes separating the ninth antimony-rich melt and the ninth alloy liquid, and the separation method is preferably to remove slag from the interior of the ninth antimony-rich melt. This invention does not have a specific limitation on the slag removal process, and any method well known to those skilled in the art can be used. In this 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%.
[0051] In this invention, the temperature of the tenth condensation treatment is 628–633°C, more preferably 631–633°C, and even more preferably 633°C; the holding time is 1–2 hours. After the tenth condensation treatment, this invention preferably further includes separating the high-antimony alloy and the tenth alloy liquid, and the separation method is preferably to remove slag from the interior of the tenth alloy liquid. This invention does not have a special limitation on the slag removal and separation process, and any method well known to those skilled in the art can be used.
[0052] In this invention, the heating rate 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 is preferably 20 to 40 °C / min.
[0053] In this invention, a covering agent is preferably added to the surface of the system during the first, second, third, fourth, fifth, sixth, seventh, eighth, ninth, and tenth condensation treatments. In this invention, the covering agent is preferably carnallite. This invention does not have a particular limitation on the amount of covering agent added; any agent well known to those skilled in the art can be used. In this invention, by adding a covering agent to the surface of the system, oxidation can be prevented during the condensation process.
[0054] In the condensation process of this invention, it is necessary to ensure that the heating temperatures set by the ten heating devices are the same as the corresponding alloy temperatures, forming a necessary condition for the stable precipitation of antimony-rich melt. Due to the difference in solubility between the antimony-rich melt and the lead-antimony alloy melt at the defined temperature in the solid-liquid phase, during condensation, the antimony-rich melt enters the solid phase and precipitates from the lead-antimony alloy melt. A slag-removal method is used to separate the antimony-rich melt from the lead-antimony alloy melt. During the separation process, some lead-antimony alloy melt is inevitably entrained. Therefore, after the removed antimony-rich melt is melted again, a lead-antimony alloy melt with a higher antimony content is obtained. Since the melting point of lead is lower than that of antimony, during the continuous slag-melting-condensation process, as the antimony content in the lead-antimony alloy melt gradually increases after the antimony-rich melt melts, its melting point also increases. To achieve the precipitation of antimony-rich melt with a higher antimony content from the lead-antimony alloy melt and ultimately obtain a high-antimony alloy, a stepped heating condensation process with gradually increasing temperature is required. As the gradient heating process continued, a high-antimony alloy was finally obtained after the tenth condensation process. The antimony content in the remaining lead-antimony alloy melt was significantly reduced, and it was collected to obtain a high-lead alloy.
[0055] In this invention, the average particle size of the first, second, third, fourth, fifth, sixth, seventh, eighth, and ninth antimony-rich melts is preferably 40–80 μm.
[0056] In this invention, the antimony content in the high-antimony alloy is preferably 98% or higher, more preferably 98-99.6%, and even more preferably 99-99.5%. In this invention, the recovery rate of the metallic antimony is preferably 98% or higher.
[0057] 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 a high-lead alloy.
[0058] In this invention, the lead content in the high-lead alloy is preferably 75-88.8%, more preferably 75-88%, and even more preferably 80-87%. In this invention, the recovery rate of the high-lead alloy is preferably 98% or higher.
[0059] After obtaining the high-antimony alloy and the high-lead alloy, the present invention preferably further includes purifying the high-antimony alloy and the high-lead alloy separately, wherein the refined antimony and refined lead obtained after purification preferably have a grade greater than 99.9%. The present invention does not have any special limitations on the purification process, and any process well known to those skilled in the art can be used.
[0060] The lead-antimony alloy separation method provided by this invention has high raw material versatility and can process lead-antimony alloys with a wide range of antimony contents; the separation method is simple; it does not introduce new impurities; and it has low equipment requirements, which can reduce operating costs.
[0061] To further illustrate the present invention, the following detailed description of a method for separating lead-antimony alloys provided by the present invention is provided in conjunction with embodiments, but these should not be construed as limiting the scope of protection of the present invention.
[0062] Example 1
[0063] 100 kg of lead-antimony alloy molten liquid at 500℃ (preferably with an antimony mass percentage of 21.56% and a lead mass percentage of 78.22%) was covered with carnallite on the surface of the liquid. Condensation treatment was carried out under the carnallite covering condition. The average particle size of the first, second, third, fourth, fifth, sixth, seventh, eighth and ninth antimony-rich melts was 78.85 μm. The conditions and parameters of the condensation treatment are shown in Table 1. The composition of the products obtained in the condensation treatment process is shown in Table 2.
[0064] Example 2
[0065] 100 kg of lead-antimony alloy molten liquid at 550℃ (preferably with an antimony mass percentage of 41.24% and a lead mass percentage of 58.69%) was covered with carnallite on the surface of the liquid. Condensation treatment was carried out under the carnallite covering condition. The average particle size of the first, second, third, fourth, fifth, sixth, seventh, eighth and ninth antimony-rich melts was 72.29 μm. The conditions and parameters of the condensation treatment are shown in Table 1. The composition of the products obtained in the condensation treatment process is shown in Table 2.
[0066] Example 3
[0067] 100 kg of lead-antimony alloy molten liquid at 575℃ (preferably with an antimony mass percentage of 62.59% and a lead mass percentage of 37.36%) was covered with carnallite on the surface of the liquid. Condensation treatment was carried out under the carnallite covering condition. The average particle size of the first, second, third, fourth, fifth, sixth, seventh, eighth and ninth antimony-rich melts was 68.87 μm. The conditions and parameters of the condensation treatment are shown in Table 1. The composition of the products obtained in the condensation treatment process is shown in Table 2.
[0068] Example 4
[0069] 100 kg of lead-antimony alloy molten liquid at 630℃ (preferably with an antimony mass percentage of 79.35% and a lead mass percentage of 20.63%) was covered with carnallite on the surface of the liquid. Condensation treatment was carried out under the carnallite covering condition. The average particle size of the first, second, third, fourth, fifth, sixth, seventh, eighth and ninth antimony-rich melts was 62.05 μm. The conditions and parameters of the condensation treatment are shown in Table 1. The composition of the products obtained in the condensation treatment process is shown in Table 2.
[0070] Comparative Example 1
[0071] 100 kg of lead-antimony alloy molten liquid at 500℃ (preferably with an antimony mass percentage of 21.56% and a lead mass percentage of 78.22%) was covered with carnallite on the surface of the liquid. Condensation treatment was carried out under the carnallite covering condition. The average particle size of the first, second, third, fourth, fifth, sixth, seventh, eighth and ninth antimony-rich melts was 42.68 μm. The conditions and parameters of the condensation treatment are shown in Table 1. The composition of the products obtained in the condensation treatment process is shown in Table 2.
[0072] Table 1. Condition parameters for condensation treatment in Examples 1-4 and Comparative Example 1.
[0073]
[0074] Table 2. Composition of products from the gradient treatment process in Examples 1-4 and Comparative Example 1.
[0075]
[0076]
[0077] As can be seen from Table 2, the present invention requires precise control of the temperature of each heating process in order to separate antimony from the lead-antimony alloy.
[0078] Although the above embodiments have provided a detailed description of the present invention, they are only some embodiments of the present invention, and not all embodiments. Other embodiments can be obtained based on these embodiments without creative effort, and these embodiments all fall within the protection scope of the present invention.
Claims
1. A method for separating lead-antimony alloys, characterized in that, Includes the following steps: The lead-antimony alloy molten liquid is subjected to a first condensation treatment to obtain a first antimony-rich melt and a first alloy liquid; the temperature of the first condensation treatment is 290~310℃, and the holding time is 1~2h; After the first antimony-rich melt is heated and melted, a second condensation treatment is performed to obtain a second antimony-rich melt and a second alloy liquid; the temperature of the second condensation treatment is 360~380℃, and the holding time is 1~2h; After the second antimony-rich melt is heated and melted, a third condensation treatment is performed to obtain a third antimony-rich melt and a third alloy liquid; the temperature of the third condensation treatment is 430~450℃, and the holding time is 1~2h. After the third antimony-rich melt is heated and melted, a fourth condensation treatment is performed to obtain a fourth antimony-rich melt and a fourth alloy liquid; the temperature of the fourth condensation treatment is 490~510℃, and the holding time is 1~2h. After the fourth antimony-rich melt is heated and melted, a fifth condensation treatment is performed to obtain a fifth antimony-rich melt and a fifth alloy liquid; the temperature of the fifth condensation treatment is 540~560℃, and the holding time is 1~2h. After the fifth antimony-rich melt is heated and melted, a sixth condensation treatment is performed to obtain a sixth antimony-rich melt and a sixth alloy liquid; the temperature of the sixth condensation treatment is 575~585℃, and the holding time is 1~2h. After the sixth antimony-rich melt is heated and melted, a seventh condensation treatment is performed to obtain a seventh antimony-rich melt and a seventh alloy liquid; the temperature of the seventh condensation treatment is 595~605℃, and the holding time is 1~2h. After the seventh antimony-rich melt is heated and melted, an eighth condensation treatment is performed to obtain an eighth antimony-rich melt and an eighth alloy liquid; the temperature of the eighth condensation treatment is 608~613℃, and the holding time is 1~2h. After the eighth antimony-rich melt is heated and melted, a ninth condensation treatment is performed to obtain a ninth antimony-rich melt and a ninth alloy liquid; the temperature of the ninth condensation treatment is 618~623℃, and the holding time is 1~2h. After the ninth antimony-rich melt is heated and melted, a tenth condensation treatment is performed to obtain a high-antimony alloy and a tenth alloy liquid; the temperature of the tenth condensation treatment is 628~633℃, and the holding time is 1~2h. In the processes of the first, second, third, fourth, fifth, sixth, seventh, eighth, ninth, and tenth condensation treatments, a covering agent is added to the surface of the system.
2. The separation method according to claim 1, characterized in that, The antimony content in the lead-antimony alloy molten liquid is 11.2% to 95% by mass.
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, characterized in that, The heating rate for the first, second, third, fourth, fifth, sixth, seventh, eighth, ninth, and tenth condensation treatments is 20~40℃ / min.
5. The separation method according to claim 1, characterized in that, The covering agent is carnallite.
6. The separation method according to claim 1, characterized in that, The average particle size of the first, second, third, fourth, fifth, sixth, seventh, eighth, and ninth antimony-rich melts is 40~80μm, respectively.
7. The separation method according to claim 1 or 6, characterized in that, The antimony content in the high-antimony alloy is above 98%.
8. The separation method according to claim 1, characterized in that, The tenth condensation treatment 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 a high-lead alloy.
9. The separation method according to claim 8, characterized in that, The lead content in the high-lead alloy is 75~88.8 wt%.
Citation Information
Patent Citations
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