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 61
- 239000002140 antimony alloy Substances 0.000 title claims abstract description 61
- 238000000926 separation method Methods 0.000 title claims abstract description 51
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 219
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 219
- 239000007788 liquid Substances 0.000 claims abstract description 99
- 229910000978 Pb alloy Inorganic materials 0.000 claims abstract description 11
- 238000005345 coagulation Methods 0.000 claims description 136
- 230000015271 coagulation Effects 0.000 claims description 136
- 229910045601 alloy Inorganic materials 0.000 claims description 95
- 239000000956 alloy Substances 0.000 claims description 95
- 238000010438 heat treatment Methods 0.000 claims description 9
- 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
- 239000000155 melt Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 abstract description 44
- 238000009833 condensation Methods 0.000 abstract description 20
- 230000005494 condensation Effects 0.000 abstract description 19
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 238000009853 pyrometallurgy Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract 2
- 239000002893 slag Substances 0.000 description 20
- 239000000203 mixture Substances 0.000 description 18
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 150000004820 halides Chemical class 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 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
- 238000000746 purification Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000005204 segregation 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
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000009916 joint effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 150000002739 metals Chemical class 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
- 239000002244 precipitate Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- 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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- 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)
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Abstract
Description
技术领域technical field
本发明属于有色金属火法冶炼技术领域，具体涉及一种铅锑合金的分离方法。The invention belongs to the technical field of pyrometallurgy of nonferrous metals, and in particular relates to a method for separating lead-antimony alloys.
背景技术Background technique
在日常生活中，应用广泛的滑动轴承、配重材料、铅酸蓄电池板栅以及导电零件中含有大量的铅锑合金，每年从这些原料中回收的铅、锑可带来很高的经济价值。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 every year can bring high economic value.
目前对于铅锑合金的处理一般采用离心偏析法、真空蒸馏分离法或熔盐电解法。其中离心偏析法的单机分离效率低，很难实现工业化生产，同时对高速转子的材料要求高，增加生产成本；真空蒸馏分离法的处理温度较高、需要全程进行减压作业且对于物料的适应性较低，在处理含锑量较高的铅锑合金时，会极大地增加作业量以及耗电量；熔盐电解法存在电解周期长、原料消耗大等问题，同时阳极泥的回收以及电解液的净化会进一步增加工作量以及工作时长，对环境造成污染。At present, the treatment of lead-antimony alloys generally adopts centrifugal segregation method, vacuum distillation separation method or molten salt electrolysis method. Among them, the single-machine separation efficiency of centrifugal segregation method is low, and it is difficult to realize industrial production. At the same time, the material requirements for high-speed rotors are high, which increases production costs; When dealing with lead-antimony alloys with high antimony content, it will greatly increase the workload and power consumption; the molten salt electrolysis method has problems such as long electrolysis cycle and large consumption of raw materials. At the same time, the recovery of anode slime and electrolysis The purification of the liquid will further increase the workload and working hours, causing pollution to the environment.
公开号为CN109825719A的中国专利公开了一种铅锑合金的分离方法，首先将合金经加料系统连续输入旋转超重力分离反应腔室中，然后启动旋转超重力反应器，通过调速电动机驱动滚轴上的反应器旋转产生稳定、可调节的超重力场。在超重力场和温度场共同作用下，铅锑合金间原子扩散和传质过程大大加快，实现富铅液体与富锑熔体间的连续分离。但是上述方法对滚轴、滤板等设备的质量要求较高，增加生产成本。The Chinese patent with the publication number CN109825719A discloses a separation method of lead-antimony alloy. First, the alloy is continuously fed into the rotating high-gravity separation reaction chamber through the feeding system, and then the rotating high-gravity reactor is started, and the roller is driven by a speed-regulating motor. The rotation of the reactor above produces a stable, adjustable hypergravity field. Under the joint action of the supergravity field and the temperature field, the process of atomic diffusion and mass transfer between the lead-antimony alloys is greatly accelerated, and the continuous separation between the lead-rich liquid and the antimony-rich melt is realized. However, the above method has higher quality requirements for equipment such as rollers and filter plates, which increases production costs.
公开号为CN108842069A的中国专利公开了一种铅锑合金火法精炼的方法。首先将铅锑合金与纯铜混合得到混合料，然后在氮气或氩气气氛下将其熔化，利用铜锑间的结合力大于铅锑间的结合力，将锑组分与铅组分分离，再利用铜锑合金与铅熔点的差异性，进行结晶分离，最终得到去除锑的纯铅。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。The Chinese patent whose publication number is CN108842069A discloses a method for pyro-refining of lead-antimony alloy. First, mix the lead-antimony alloy with pure copper to obtain a mixture, and then melt it under nitrogen or argon atmosphere, and use the binding force between copper and antimony to be greater than that between lead and antimony to separate the antimony component from the lead component. Using the difference in the melting point of copper-antimony alloy and lead, crystallization and separation are carried out, and finally pure lead with antimony removed is obtained. However, the above method will introduce impurity metal copper, further prolonging the separation process of the whole lead-antimony alloy.
发明内容Contents of the invention
本发明的目的在于提供一种铅锑合金的分离方法，本发明提供的分离过程中不会引入新的杂质，且分离方法的原料普适性高，方法简单，同时对设备要求低。The purpose of the present invention is to provide a method for separating lead-antimony alloys. No new impurities will be introduced in the separation process provided by the present invention, and the raw materials of the separation method are highly universal, the method is simple, and the requirements for equipment are low.
为了实现上述目的，本发明提供如下技术方案：In order to achieve the above object, the present invention provides the following technical solutions:
本发明提供了一种铅锑合金的分离方法，包括以下步骤：The invention provides a method for separating lead-antimony alloys, comprising the following steps:
将铅锑合金熔融液进行第一凝析处理，得到第一富锑熔体和第一合金液；所述第一凝析处理的温度为290～310℃，保温时间为1～2h；performing a first coagulation treatment on the lead-antimony alloy melt to obtain a first antimony-rich melt and a first alloy solution; the temperature of the first coagulation treatment is 290-310° C., and the holding time is 1-2 hours;
将所述第一富锑熔体进行第二凝析处理，得到第二富锑熔体和第二合金液；所述第二凝析处理的温度为360～380℃，保温时间为1～2h；performing a second coagulation treatment on the first antimony-rich melt to obtain a second antimony-rich melt and a second alloy liquid; the temperature of the second coagulation treatment is 360-380°C, and the holding time is 1-2h ;
将所述第二富锑熔体进行第三凝析处理，得到第三富锑熔体和第三合金液；所述第三凝析处理的温度为430～450℃，保温时间为1～2h；performing a third coagulation treatment on the second antimony-rich melt to obtain a third antimony-rich melt and a third alloy liquid; the temperature of the third coagulation treatment is 430-450°C, and the holding time is 1-2h ;
将所述第三富锑熔体进行第四凝析处理，得到第四富锑熔体和第四合金液；所述第四凝析处理的温度为490～510℃，保温时间为1～2h；performing a fourth coagulation treatment on the third antimony-rich melt to obtain a fourth antimony-rich melt and a fourth alloy liquid; the temperature of the fourth coagulation treatment is 490-510°C, and the holding time is 1-2h ;
将所述第四富锑熔体进行第五凝析处理，得到第五富锑熔体和第五合金液；所述第五凝析处理的温度为540～560℃，保温时间为1～2h；subjecting the fourth antimony-rich melt to the fifth condensate treatment to obtain the fifth antimony-rich melt and the fifth alloy solution; the temperature of the fifth condensate treatment is 540-560°C, and the holding time is 1-2h ;
将所述第五富锑熔体进行第六凝析处理，得到第六富锑熔体和第六合金液；所述第六凝析处理的温度为575～585℃，保温时间为1～2h；The fifth antimony-rich melt is subjected to the sixth coagulation treatment to obtain the sixth antimony-rich melt and the sixth alloy liquid; the temperature of the sixth coagulation treatment is 575-585°C, and the holding time is 1-20°C. 2h;
将所述第六富锑熔体进行第七凝析处理，得到第七富锑熔体和第七合金液；所述第七凝析处理的温度为595～605℃，保温时间为1～2h；Subjecting the sixth antimony-rich melt to the seventh condensate treatment to obtain the seventh antimony-rich melt and the seventh alloy liquid; the temperature of the seventh condensate treatment is 595-605°C, and the holding time is 1-2h ;
将所述第七富锑熔体进行第八凝析处理，得到第八富锑熔体和第八合金液；所述第八凝析处理的温度为608～613℃，保温时间为1～2h；performing an eighth coagulation treatment on the seventh antimony-rich melt to obtain an eighth antimony-rich melt and an eighth alloy liquid; the temperature of the eighth coagulation treatment is 608-613°C, and the holding time is 1-2h ;
将所述第八富锑熔体进行第九凝析处理，得到第九富锑熔体和第九合金液；所述第九凝析处理的温度为618～623℃，保温时间为1～2h；subjecting the eighth antimony-rich melt to the ninth condensate treatment to obtain the ninth antimony-rich melt and the ninth alloy liquid; the temperature of the ninth condensate treatment is 618-623°C, and the holding time is 1-2h ;
将所述第九富锑熔体进行第十凝析处理，得到高锑合金和第十合金液；所述第十凝析处理的温度为628～633℃，保温时间为1～2h。The ninth antimony-rich melt is subjected to a tenth condensate treatment to obtain a high-antimony alloy and a tenth alloy liquid; the temperature of the tenth condensate treatment is 628-633° C., and the holding time is 1-2 hours.
优选的，所述铅锑合金熔融液中锑的质量百分含量为11.2～95％。Preferably, the mass percentage of antimony in the lead-antimony alloy melt is 11.2-95%.
优选的，所述铅锑合金熔融液的温度为400～800℃。Preferably, the temperature of the lead-antimony alloy melt is 400-800°C.
优选的，所述第一凝析处理、第二凝析处理、第三凝析处理、第四凝析处理、第五凝析处理、第六凝析处理、第七凝析处理、第八凝析处理、第九凝析处理和第十凝析处理的升温速率均为20～40℃/min。Preferably, the first coagulation treatment, the second coagulation treatment, the third coagulation treatment, the fourth coagulation treatment, the fifth coagulation treatment, the sixth coagulation treatment, the seventh coagulation treatment, the eighth coagulation treatment The heating rates of the first condensate treatment, the ninth condensate treatment and the tenth condensate treatment are all 20-40°C/min.
优选的，在所述第一凝析处理、第二凝析处理、第三凝析处理、第四凝析处理、第五凝析处理、第六凝析处理、第七凝析处理、第八凝析处理、第九凝析处理和第十凝析处理的过程中均在体系的表面加入覆盖剂。Preferably, in the first coagulation treatment, the second coagulation treatment, the third coagulation treatment, the fourth coagulation treatment, the fifth coagulation treatment, the sixth coagulation treatment, the seventh coagulation treatment, the eighth coagulation treatment During the coagulation treatment, the ninth coagulation treatment and the tenth coagulation treatment, a covering agent is added to the surface of the system.
优选的，所述覆盖剂为光卤石。Preferably, the covering agent is carnallite.
优选的，所述第一富锑熔体、第二富锑熔体、第三富锑熔体、第四富锑熔体、第五富锑熔体、第六富锑熔体、第七富锑熔体、第八富锑熔体和第九富锑熔体的平均粒径独立的为40～80μm。Preferably, 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 average particle diameters of the antimony melt, the eighth antimony-rich melt and the ninth antimony-rich melt are independently 40-80 μm.
优选的，所述高锑合金中锑的品位为98％以上。Preferably, the grade of antimony in the high antimony alloy is above 98%.
优选的，所述第十凝析处理后，还包括将所述第一合金液、第二合金液、第三合金液、第四合金液、第五合金液、第六合金液、第七合金液、第八合金液、第九合金液和第十合金液进行混合，得到高铅合金。Preferably, after the tenth condensate treatment, it also includes adding 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 alloy liquid, the eighth alloy liquid, the ninth alloy liquid and the tenth alloy liquid are mixed to obtain a high-lead alloy.
优选的，所述高铅合金中铅的品位为75～88.8wt％。Preferably, the grade of lead in the high-lead alloy is 75-88.8wt%.
本发明提供了一种铅锑合金的分离方法，包括以下步骤：将铅锑合金熔融液进行第一凝析处理，得到第一富锑熔体和第一合金液；所述第一凝析处理的温度为290～310℃，保温时间为1～2h；将所述第一富锑熔体进行第二凝析处理，得到第二富锑熔体和第二合金液；所述第二凝析处理的温度为360～380℃，保温时间为1～2h；将所述第二富锑熔体进行第三凝析处理，得到第三富锑熔体和第三合金液；所述第三凝析处理的温度为430～450℃，保温时间为1～2h；将所述第三富锑熔体进行第四凝析处理，得到第四富锑熔体和第四合金液；所述第四凝析处理的温度为490～510℃，保温时间为1～2h；将所述第四富锑熔体进行第五凝析处理，得到第五富锑熔体和第五合金液；所述第五凝析处理的温度为540～560℃，保温时间为1～2h；将所述第五富锑熔体进行第六凝析处理，得到第六富锑熔体和第六合金液；所述第六凝析处理的温度为575～585℃，保温时间为1～2h；将所述第六富锑熔体进行第七凝析处理，得到第七富锑熔体和第七合金液；所述第七凝析处理的温度为595～605℃，保温时间为1～2h；将所述第七富锑熔体进行第八凝析处理，得到第八富锑熔体和第八合金液；所述第八凝析处理的温度为608～613℃，保温时间为1～2h；将所述第八富锑熔体进行第九凝析处理，得到第九富锑熔体和第九合金液；所述第九凝析处理的温度为618～623℃，保温时间为1～2h；将所述第九富锑熔体进行第十凝析处理，得到高锑合金和第十合金液；所述第十凝析处理的温度为628～633℃，保温时间为1～2h。本发明在限定的程序下进行凝析处理，能够实现锑从铅锑合金中的分离，且分离的过程中没有杂质引入、分离效率高。本发明提供的分离方法简单，原料普适性高，同时对设备要求低。The invention provides a method for separating lead-antimony alloys, comprising the following steps: performing a first coagulation treatment on a lead-antimony alloy melt to obtain a first antimony-rich melt and a first alloy solution; the first coagulation treatment The temperature is 290-310°C, and the holding time is 1-2h; the first antimony-rich melt is subjected to a second condensate treatment to obtain a second antimony-rich melt and a second alloy liquid; the second condensate The temperature of the treatment is 360-380°C, and the holding time is 1-2 hours; the second antimony-rich melt is subjected to the third coagulation treatment to obtain the third antimony-rich melt and the third alloy liquid; the third coagulation The temperature of the analysis treatment is 430-450°C, and the holding time is 1-2 hours; the third antimony-rich melt is subjected to the fourth coagulation treatment to obtain the fourth antimony-rich melt and the fourth alloy liquid; the fourth antimony-rich melt is The temperature of the coagulation treatment is 490-510°C, and the holding time is 1-2 hours; the fourth antimony-rich melt is subjected to the fifth coagulation treatment to obtain the fifth antimony-rich melt and the fifth alloy liquid; The temperature of the fifth condensate treatment is 540-560°C, and the holding time is 1-2h; the fifth antimony-rich melt is subjected to the sixth condensate treatment to obtain the sixth antimony-rich melt and the sixth alloy liquid; The temperature of the sixth condensate treatment is 575-585°C, and the holding time is 1-2h; the sixth antimony-rich melt is subjected to the seventh condensate treatment to obtain the seventh antimony-rich melt and the seventh alloy solution; The temperature of the seventh condensate treatment is 595-605°C, and the holding time is 1-2h; the seventh antimony-rich melt is subjected to the eighth condensate treatment to obtain the eighth antimony-rich melt and the eighth alloy liquid The temperature of the eighth condensate treatment is 608-613°C, and the holding time is 1-2h; the ninth condensate treatment is performed on the eighth antimony-rich melt to obtain the ninth antimony-rich melt and the ninth alloy liquid; the temperature of the ninth condensate treatment is 618-623°C, and the holding time is 1-2h; the ninth antimony-rich melt is subjected to the tenth condensate treatment to obtain a high-antimony alloy and a tenth alloy liquid; The temperature of the tenth coagulation treatment is 628-633° C., and the holding time is 1-2 hours. The invention carries out coagulation treatment under a limited program, can realize the separation of antimony from the lead-antimony alloy, has no impurity introduction in the separation process, and has high separation efficiency. The separation method provided by the invention is simple, has high raw material universality, and has low requirements on equipment.
具体实施方式Detailed ways
本发明提供了一种铅锑合金的分离方法，包括以下步骤：The invention provides a method for separating lead-antimony alloys, comprising the following steps:
将铅锑合金熔融液进行第一凝析处理，得到第一富锑熔体和第一合金液；所述第一凝析处理的温度为290～310℃，保温时间为1～2h；performing a first coagulation treatment on the lead-antimony alloy melt to obtain a first antimony-rich melt and a first alloy solution; the temperature of the first coagulation treatment is 290-310° C., and the holding time is 1-2 hours;
将所述第一富锑熔体进行第二凝析处理，得到第二富锑熔体和第二合金液；所述第二凝析处理的温度为360～380℃，保温时间为1～2h；performing a second coagulation treatment on the first antimony-rich melt to obtain a second antimony-rich melt and a second alloy liquid; the temperature of the second coagulation treatment is 360-380°C, and the holding time is 1-2h ;
将所述第二富锑熔体进行第三凝析处理，得到第三富锑熔体和第三合金液；所述第三凝析处理的温度为430～450℃，保温时间为1～2h；performing a third coagulation treatment on the second antimony-rich melt to obtain a third antimony-rich melt and a third alloy liquid; the temperature of the third coagulation treatment is 430-450°C, and the holding time is 1-2h ;
将所述第三富锑熔体进行第四凝析处理，得到第四富锑熔体和第四合金液；所述第四凝析处理的温度为490～510℃，保温时间为1～2h；performing a fourth coagulation treatment on the third antimony-rich melt to obtain a fourth antimony-rich melt and a fourth alloy liquid; the temperature of the fourth coagulation treatment is 490-510°C, and the holding time is 1-2h ;
将所述第四富锑熔体进行第五凝析处理，得到第五富锑熔体和第五合金液；所述第五凝析处理的温度为540～560℃，保温时间为1～2h；subjecting the fourth antimony-rich melt to the fifth condensate treatment to obtain the fifth antimony-rich melt and the fifth alloy liquid; the temperature of the fifth condensate treatment is 540-560°C, and the holding time is 1-2h ;
将所述第五富锑熔体进行第六凝析处理，得到第六富锑熔体和第六合金液；所述第六凝析处理的温度为575～585℃，保温时间为1～2h；The fifth antimony-rich melt is subjected to the sixth coagulation treatment to obtain the sixth antimony-rich melt and the sixth alloy liquid; the temperature of the sixth coagulation treatment is 575-585°C, and the holding time is 1-20°C. 2h;
将所述第六富锑熔体进行第七凝析处理，得到第七富锑熔体和第七合金液；所述第七凝析处理的温度为595～605℃，保温时间为1～2h；Subjecting the sixth antimony-rich melt to the seventh condensate treatment to obtain the seventh antimony-rich melt and the seventh alloy liquid; the temperature of the seventh condensate treatment is 595-605°C, and the holding time is 1-2h ;
将所述第七富锑熔体进行第八凝析处理，得到第八富锑熔体和第八合金液；所述第八凝析处理的温度为608～613℃，保温时间为1～2h；performing an eighth coagulation treatment on the seventh antimony-rich melt to obtain an eighth antimony-rich melt and an eighth alloy liquid; the temperature of the eighth coagulation treatment is 608-613°C, and the holding time is 1-2h ;
将所述第八富锑熔体进行第九凝析处理，得到第九富锑熔体和第九合金液；所述第九凝析处理的温度为618～623℃，保温时间为1～2h；subjecting the eighth antimony-rich melt to the ninth condensate treatment to obtain the ninth antimony-rich melt and the ninth alloy liquid; the temperature of the ninth condensate treatment is 618-623°C, and the holding time is 1-2h ;
将所述第九富锑熔体进行第十凝析处理，得到高锑合金和第十合金液；所述第十凝析处理的温度为628～633℃，保温时间为1～2h。The ninth antimony-rich melt is subjected to a tenth condensate treatment to obtain a high-antimony alloy and a tenth alloy liquid; the temperature of the tenth condensate treatment is 628-633° C., and the holding time is 1-2 hours.
在本发明中，所述铅锑合金熔融液中锑的质量百分含量优选为11.2～95％，进一步优选为15～90％，更优选为20～80％。In the present invention, the mass percentage of antimony in the lead-antimony alloy melt is preferably 11.2-95%, more preferably 15-90%, and more preferably 20-80%.
在本发明中，所述铅锑合金熔融液的温度优选为400～800℃，进一步优选为450～700℃，更优选为500～600℃。In the present invention, the temperature of the lead-antimony alloy melt is preferably 400-800°C, more preferably 450-700°C, more preferably 500-600°C.
在本发明中，所述第一凝析处理的温度为290～310℃，进一步优选为295～305℃，更优选为300℃；保温时间为1～2h。所述第一凝析处理后，本发明还优选包括将所述第一富锑熔体和第一合金液进行分离，所述分离的方法优选为将所述第一富锑熔体从所述第一合金液的内部进行捞渣分离。本发明对所述捞渣分离的过程没有特殊的限定，采用本领域技术人员熟知的即可。在本发明中，所述第一富锑熔体中锑的质量百分含量优选为30～83％；铅的质量百分含量优选为17～70％。In the present invention, the temperature of the first coagulation treatment is 290-310° C., more preferably 295-305° C., more preferably 300° C.; the holding time is 1-2 hours. After the first coagulation treatment, the present invention also preferably includes separating the first antimony-rich melt from the first alloy liquid, and the separation method is preferably to separate the first antimony-rich melt from the Slag removal is carried out inside the first alloy liquid. In the present invention, there is no special limitation on the process of slag removal and separation, and the processes known to those skilled in the art can be used. In the present 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%.
在本发明中，所述第二凝析处理的温度为360～380℃，进一步优选为365～375℃，更优选为370℃；保温时间为1～2h。所述第二凝析处理后，本发明还优选包括将所述第二富锑熔体和第二合金液进行分离，所述分离的方法优选为将所述第二富锑熔体从所述第二合金液的内部进行捞渣分离。本发明对所述捞渣分离的过程没有特殊的限定，采用本领域技术人员熟知的即可。在本发明中，所述第二富锑熔体中锑的质量百分含量优选为40～85％；铅的质量百分含量优选为15～60％。In the present invention, the temperature of the second coagulation treatment is 360-380° C., more preferably 365-375° C., more preferably 370° C.; the holding time is 1-2 hours. After the second coagulation treatment, the present invention also preferably includes separating the second antimony-rich melt from the second alloy liquid, and the separation method is preferably separating the second antimony-rich melt from the Slag removal is carried out inside the second alloy liquid. In the present invention, there is no special limitation on the process of slag removal and separation, and the processes known to those skilled in the art can be used. In the present 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%.
在本发明中，所述第三凝析处理的温度为430～450℃，进一步优选为435～445℃，更优选为440℃；保温时间为1～2h。所述第三凝析处理后，本发明还优选包括将所述第三富锑熔体和第三合金液进行分离，所述分离的方法优选为将所述第三富锑熔体从所述第三合金液的内部进行捞渣分离。本发明对所述捞渣分离的过程没有特殊的限定，采用本领域技术人员熟知的即可。在本发明中，所述第三富锑熔体中锑的质量百分含量优选为53～87％；铅的质量百分含量优选为17～45％。In the present invention, the temperature of the third coagulation treatment is 430-450° C., more preferably 435-445° C., more preferably 440° C.; the holding time is 1-2 hours. After the third coagulation treatment, the present invention also preferably includes separating the third antimony-rich melt from the third alloy liquid, and the separation method is preferably to separate the third antimony-rich melt from the Slag removal is carried out inside the third alloy liquid. In the present invention, there is no special limitation on the process of slag removal and separation, and the processes known to those skilled in the art can be used. In the present 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%.
在本发明中，所述第四凝析处理的温度为490～510℃，进一步优选为495～505℃，更优选为500℃；保温时间为1～2h。所述第四凝析处理后，本发明还优选包括将所述第四富锑熔体和第四合金液进行分离，所述分离的方法优选为将所述第四富锑熔体从所述第四合金液的内部进行捞渣分离。本发明对所述捞渣分离的过程没有特殊的限定，采用本领域技术人员熟知的即可。在本发明中，所述第四富锑熔体中锑的质量百分含量优选为65～88％；铅的质量百分含量优选为12～35％。In the present invention, the temperature of the fourth coagulation treatment is 490-510° C., more preferably 495-505° C., more preferably 500° C.; the holding time is 1-2 hours. After the fourth coagulation treatment, the present invention also preferably includes separating the fourth antimony-rich melt and the fourth alloy liquid, and the separation method is preferably to separate the fourth antimony-rich melt from the Slag removal is carried out inside the fourth alloy liquid. In the present invention, there is no special limitation on the process of slag removal and separation, and the processes known to those skilled in the art can be used. In the present 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%.
在本发明中，所述第五凝析处理的温度为540～560℃，进一步优选为545～555℃，更优选为550℃；保温时间为1～2h。所述第五凝析处理后，本发明还优选包括将所述第五富锑熔体和第五合金液进行分离，所述分离的方法优选为将所述第五富锑熔体从所述第五合金液的内部进行捞渣分离。本发明对所述捞渣分离的过程没有特殊的限定，采用本领域技术人员熟知的即可。在本发明中，所述第五富锑熔体中锑的质量百分含量优选为77～90％；铅的质量百分含量优选为10～23％。In the present invention, the temperature of the fifth coagulation treatment is 540-560° C., more preferably 545-555° C., more preferably 550° C.; the holding time is 1-2 hours. After the fifth coagulation treatment, the present invention also preferably includes separating the fifth antimony-rich melt from the fifth alloy liquid, and the separation method is preferably to separate the fifth antimony-rich melt from the Slag removal is carried out inside the fifth alloy liquid. In the present invention, there is no special limitation on the process of slag removal and separation, and the processes known to those skilled in the art can be used. In the present 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%.
在本发明中，所述第六凝析处理的温度为575～585℃，进一步优选为578～582℃，更优选为580℃；保温时间为1～2h。所述第六凝析处理后，本发明还优选包括将所述第六富锑熔体和第六合金液进行分离，所述分离的方法优选为将所述第六富锑熔体从所述第六合金液的内部进行捞渣分离。本发明对所述捞渣分离的过程没有特殊的限定，采用本领域技术人员熟知的即可。在本发明中，所述第六富锑熔体中锑的质量百分含量优选为86～91％；铅的质量百分含量优选为9～14％。In the present invention, the temperature of the sixth coagulation treatment is 575-585° C., more preferably 578-582° C., more preferably 580° C.; the holding time is 1-2 hours. After the sixth coagulation treatment, the present invention also preferably includes separating the sixth antimony-rich melt and the sixth alloy liquid, and the separation method is preferably to separate the sixth antimony-rich melt from the Slag removal is carried out in the interior of the sixth alloy liquid. In the present invention, there is no special limitation on the process of slag removal and separation, and the processes known to those skilled in the art can be used. In the present 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%.
在本发明中，所述第七凝析处理的温度为595～605℃，进一步优选为598～602℃，更优选为600℃；保温时间为1～2h。所述第七凝析处理后，本发明还优选包括将所述第七富锑熔体和第七合金液进行分离，所述分离的方法优选为将所述第七富锑熔体从所述第七合金液的内部进行捞渣分离。本发明对所述捞渣分离的过程没有特殊的限定，采用本领域技术人员熟知的即可。在本发明中，所述第七富锑熔体中锑的质量百分含量优选为92～94％；铅的质量百分含量优选为6～8％。In the present invention, the temperature of the seventh coagulation treatment is 595-605°C, more preferably 598-602°C, more preferably 600°C; the holding time is 1-2h. After the seventh coagulation treatment, the present invention also preferably includes separating the seventh antimony-rich melt and the seventh alloy liquid, and the separation method is preferably to separate the seventh antimony-rich melt from the Slag removal is carried out inside the seventh alloy liquid. In the present invention, there is no special limitation on the process of slag removal and separation, and the processes known to those skilled in the art can be used. In the present 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%.
在本发明中，所述第八凝析处理的温度为608～613℃，进一步优选为609～611℃，更优选为610℃；保温时间为1～2h。所述第八凝析处理后，本发明还优选包括将所述第八富锑熔体和第八合金液进行分离，所述分离的方法优选为将所述第八富锑熔体从所述第八合金液的内部进行捞渣分离。本发明对所述捞渣分离的过程没有特殊的限定，采用本领域技术人员熟知的即可。在本发明中，所述第八富锑熔体中锑的质量百分含量优选为95～97％；铅的质量百分含量优选为3～5％。In the present invention, the temperature of the eighth coagulation treatment is 608-613°C, more preferably 609-611°C, more preferably 610°C; the holding time is 1-2h. After the eighth coagulation treatment, the present invention also preferably includes separating the eighth antimony-rich melt and the eighth alloy liquid, and the separation method is preferably to separate the eighth antimony-rich melt from the eighth alloy liquid Slag removal is carried out inside the eighth alloy liquid. In the present invention, there is no special limitation on the process of slag removal and separation, and the processes known to those skilled in the art can be used. In the present 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%.
在本发明中，所述第九凝析处理的温度为618～623℃，进一步优选为619～621℃，更优选为620℃；保温时间为1～2h。所述第九凝析处理后，本发明还优选包括将所述第九富锑熔体和第九合金液进行分离，所述分离的方法优选为将所述第九富锑熔体从所述第九合金液的内部进行捞渣分离。本发明对所述捞渣分离的过程没有特殊的限定，采用本领域技术人员熟知的即可。在本发明中，所述第九富锑熔体中锑的质量百分含量优选为97～99％；铅的质量百分含量优选为1～3％。In the present invention, the temperature of the ninth coagulation treatment is 618-623°C, more preferably 619-621°C, more preferably 620°C; the holding time is 1-2h. After the ninth coagulation treatment, the present invention also preferably includes separating the ninth antimony-rich melt and the ninth alloy liquid, and the separation method is preferably to separate the ninth antimony-rich melt from the Slag removal is carried out inside the ninth alloy liquid. In the present invention, there is no special limitation on the process of slag removal and separation, and the processes known to those skilled in the art can be used. In the present 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%.
在本发明中，所述第十凝析处理的温度为628～633℃，进一步优选为631～633℃，更优选为633℃；保温时间为1～2h。所述第十凝析处理后，本发明还优选包括将所述高锑合金和第十合金液进行分离，所述分离的方法优选为将所述高锑合金从所述第十合金液的内部进行捞渣分离。本发明对所述捞渣分离的过程没有特殊的限定，采用本领域技术人员熟知的即可。In the present invention, the temperature of the tenth coagulation treatment is 628-633° C., more preferably 631-633° C., more preferably 633° C.; the holding time is 1-2 hours. After the tenth condensate treatment, the present invention also preferably includes separating the high-antimony alloy from the tenth alloy liquid, and the separation method is preferably to separate the high-antimony alloy from the inside of the tenth alloy liquid Carry out slag separation. In the present invention, there is no special limitation on the process of slag removal and separation, and the processes known to those skilled in the art can be used.
在本发明中，所述第一凝析处理、第二凝析处理、第三凝析处理、第四凝析处理、第五凝析处理、第六凝析处理、第七凝析处理、第八凝析处理、第九凝析处理和第十凝析处理的升温速率均优选为20～40℃/min。In the present invention, the first coagulation treatment, the second coagulation treatment, the third coagulation treatment, the fourth coagulation treatment, the fifth coagulation treatment, the sixth coagulation treatment, the seventh coagulation treatment, the The heating rates of the eighth coagulation treatment, the ninth coagulation treatment and the tenth coagulation treatment are all preferably 20-40° C./min.
在本发明中，所述第一凝析处理、第二凝析处理、第三凝析处理、第四凝析处理、第五凝析处理、第六凝析处理、第七凝析处理、第八凝析处理、第九凝析处理和第十凝析处理的过程中均优选在体系的表面加入覆盖剂。在本发明中，所述覆盖剂优选为光卤石。本发明对所述覆盖剂的加入量没有特殊的限定，采用本领域技术人员熟知的即可。在本发明中，通过在体系的表面加入覆盖剂，能够防止在凝析的过程中发生氧化。In the present invention, the first coagulation treatment, the second coagulation treatment, the third coagulation treatment, the fourth coagulation treatment, the fifth coagulation treatment, the sixth coagulation treatment, the seventh coagulation treatment, the During the eighth coagulation treatment, the ninth coagulation treatment and the tenth coagulation treatment, it is preferable to add a covering agent on the surface of the system. In the present invention, the covering agent is preferably carnallite. In the present invention, there is no special limitation on the addition amount of the covering agent, and what is well known by those skilled in the art can be used. In the present invention, by adding a covering agent on the surface of the system, oxidation during the coagulation process can be prevented.
在本发明的凝析处理过程中，需保证十个加热装置所设定的加热温度与其对应加热的合金温度相同，形成富锑熔体能够稳定析出的必要条件。由于限定温度下的富锑熔体与铅锑合金熔融液在固液相间的溶解度存在差异，因此在凝析过程中，富锑熔体进入固相，从铅锑合金熔融液中析出，采用捞渣的手段将富锑熔体与铅锑合金熔融液进行分离。分离过程中，无法避免部分铅锑合金熔融液的夹带现象，因此捞出的富锑熔体再次融化后，得到锑含量更高的铅锑合金熔融液。而铅的熔点低于锑的熔点，因此在不断进行捞渣-融化-凝析的过程中，随着富锑熔体融化后铅锑合金熔融液中锑含量的逐渐升高，其熔点也在随之升高，为实现锑含量更高的富锑熔体从铅锑合金熔融液中析出并最终得到高锑合金，需对其进行逐渐升温的梯级加热凝析处理。随着梯度加热处理过程的持续进行，最终在第十次凝析过程后得到高锑合金，剩余的铅锑合金熔融液中的锑含量明显降低，将其收集后得到高铅合金。In the coagulation treatment process of the present invention, it is necessary to ensure that the heating temperatures set by the ten heating devices are the same as the corresponding heating alloy temperature, so as to form a necessary condition for the stable precipitation of the antimony-rich melt. Due to the difference in solubility between the solid-liquid phase of the antimony-rich melt and the lead-antimony alloy melt at a limited temperature, during the coagulation process, the antimony-rich melt enters the solid phase and precipitates from the lead-antimony alloy melt. Slagging means to separate the antimony-rich melt from the lead-antimony alloy melt. During the separation process, entrainment of part of the lead-antimony alloy melt cannot be avoided. Therefore, after the extracted antimony-rich melt is melted again, a lead-antimony alloy melt with higher antimony content is obtained. The melting point of lead is lower than that of antimony, so in the process of slagging-melting-condensation, as the antimony-rich melt melts, the antimony content in the lead-antimony alloy melt gradually increases, and its melting point is also Then it rises, in order to realize the precipitation of the antimony-rich melt with higher antimony content from the lead-antimony alloy melt and finally obtain the high-antimony alloy, it is necessary to carry out the stepwise heating and condensing treatment with gradually increasing temperature. As the gradient heating process continues, a high-antimony alloy is finally obtained after the tenth condensate process, and the antimony content in the remaining lead-antimony alloy melt is significantly reduced, and the high-lead alloy is obtained after being collected.
在本发明中，所述第一富锑熔体、第二富锑熔体、第三富锑熔体、第四富锑熔体、第五富锑熔体、第六富锑熔体、第七富锑熔体、第八富锑熔体和第九富锑熔体的平均粒径独立的优选为40～80μm。In the present invention, 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 The average particle size of the seventh antimony-rich melt, the eighth antimony-rich melt and the ninth antimony-rich melt is independently preferably 40-80 μm.
在本发明中，所述高锑合金中锑的品位优选为98％以上，进一步优选为98～99.6％，更优选为99～99.5％。在本发明中，所述金属锑的回收率优选为98％以上。In the present invention, the grade of antimony in the high-antimony alloy is preferably above 98%, more preferably 98-99.6%, more preferably 99-99.5%. In the present invention, the recovery rate of the metal antimony is preferably above 98%.
所述第十凝析处理后，本发明还优选包括将所述第一合金液、第二合金液、第三合金液、第四合金液、第五合金液、第六合金液、第七合金液、第八合金液、第九合金液和第十合金液进行混合，得到高铅合金。After the tenth coagulation treatment, the present invention also preferably includes adding 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 alloy liquid, the eighth alloy liquid, the ninth alloy liquid and the tenth alloy liquid are mixed to obtain a high-lead alloy.
在本发明中，所述高铅合金中铅的品位优选为75～88.8％，进一步优选为75～88％，更优选为80～87％。在本发明中，所述高铅合金的回收率优选为98％以上。In the present invention, the grade of lead in the high-lead alloy is preferably 75-88.8%, more preferably 75-88%, and more preferably 80-87%. In the present invention, the recovery rate of the high-lead alloy is preferably above 98%.
得到高锑合金和高铅合金后，本发明还优选包括对所述高锑合金和高铅合金分别进行提纯处理，提纯后得到的精锑和精铅的品位均优选为大于99.9％。本发明对所述提纯处理的过程没有特殊的限定，采用本领域技术人员熟知的过程进行即可。After the high-antimony alloy and the high-lead alloy are obtained, the present invention preferably further includes purifying the high-antimony alloy and the high-lead alloy respectively, and the grades of refined antimony and refined lead obtained after purification are preferably greater than 99.9%. In the present invention, there is no special limitation on the process of the purification treatment, which can be carried out by adopting a process well known to those skilled in the art.
本发明所提供的铅锑合金分离方法原料普适性高，可处理含锑范围广的铅锑合金；分离方法简单；不引入新杂质；设备要求低，可减少作业成本。The lead-antimony alloy separation method provided by the invention has high raw material universality, can process lead-antimony alloys containing a wide range of antimony; the separation method is simple; new impurities are not introduced; equipment requirements are low, and operating costs can be reduced.
为了进一步说明本发明，下面结合实施例对本发明提供的一种铅锑合金的分离方法进行详细地描述，但不能将它们理解为对本发明保护范围的限定。In order to further illustrate the present invention, a method for separating a lead-antimony alloy provided by the present invention is described in detail below in conjunction with examples, but they cannot be interpreted as limiting the protection scope of the present invention.
实施例1Example 1
将100kg温度为500℃的铅锑合金熔融液(其中锑的质量百分含量优选为21.56％；铅的质量百分含量优选为78.22％)，在液面上加入光卤石进行覆盖，在光卤石覆盖的条件下进行凝析处理，第一富锑熔体、第二富锑熔体、第三富锑熔体、第四富锑熔体、第五富锑熔体、第六富锑熔体、第七富锑熔体、第八富锑熔体和第九富锑熔体的平均粒径为78.85μm，凝析处理的条件参数如表1所示，在凝析处理过程中得到的产物的成分如表2所示。100kg of lead-antimony alloy molten liquid (wherein the mass percentage composition of antimony is preferably 21.56%; the mass percentage composition of lead is preferably 78.22%) at 500°C is covered by adding carnallite on the liquid surface. Condensation treatment is carried out under the condition of halide cover, 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 average particle size of the melt, the seventh antimony-rich melt, the eighth antimony-rich melt and the ninth antimony-rich melt is 78.85 μm, and the conditions and parameters of the coagulation treatment are shown in Table 1. The composition of the product is shown in Table 2.
实施例2Example 2
将100kg温度为550℃的铅锑合金熔融液(其中锑的质量百分含量优选为41.24％；铅的质量百分含量优选为58.69％)，在液面上加入光卤石进行覆盖，在光卤石覆盖的条件下进行凝析处理，第一富锑熔体、第二富锑熔体、第三富锑熔体、第四富锑熔体、第五富锑熔体、第六富锑熔体、第七富锑熔体、第八富锑熔体和第九富锑熔体的平均粒径为72.29μm，凝析处理的条件参数如表1所示，在凝析处理过程中得到的产物的成分如表2所示。100kg temperature is 550 ℃ lead-antimony alloy molten liquid (wherein the mass percentage composition of antimony is preferably 41.24%; The mass percentage composition of lead is preferably 58.69%), add carnallite on the liquid surface and cover, in light Condensation treatment is carried out under the condition of halide cover, 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 average particle size of the melt, the seventh antimony-rich melt, the eighth antimony-rich melt and the ninth antimony-rich melt is 72.29 μm, and the conditions and parameters of the coagulation treatment are shown in Table 1. The composition of the product is shown in Table 2.
实施例3Example 3
将100kg温度为575℃的铅锑合金熔融液(其中锑的质量百分含量优选为62.59％；铅的质量百分含量优选为37.36％)，在液面上加入光卤石进行覆盖，在光卤石覆盖的条件下进行凝析处理，第一富锑熔体、第二富锑熔体、第三富锑熔体、第四富锑熔体、第五富锑熔体、第六富锑熔体、第七富锑熔体、第八富锑熔体和第九富锑熔体的平均粒径为68.87μm，凝析处理的条件参数如表1所示，在凝析处理过程中得到的产物的成分如表2所示。100kg temperature is 575 ℃ lead-antimony alloy molten liquid (wherein the mass percentage composition of antimony is preferably 62.59%; The mass percentage composition of lead is preferably 37.36%), add carnallite on the liquid surface and cover, in light Condensation treatment is carried out under the condition of halide cover, 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 average particle size of the melt, the seventh antimony-rich melt, the eighth antimony-rich melt and the ninth antimony-rich melt is 68.87 μm, and the conditions and parameters of the coagulation treatment are shown in Table 1. The composition of the product is shown in Table 2.
实施例4Example 4
将100kg温度为630℃的铅锑合金熔融液(其中锑的质量百分含量优选为79.35％；铅的质量百分含量优选为20.63％)，在液面上加入光卤石进行覆盖，在光卤石覆盖的条件下进行凝析处理，第一富锑熔体、第二富锑熔体、第三富锑熔体、第四富锑熔体、第五富锑熔体、第六富锑熔体、第七富锑熔体、第八富锑熔体和第九富锑熔体的平均粒径为62.05μm，凝析处理的条件参数如表1所示，在凝析处理过程中得到的产物的成分如表2所示。100kg of lead-antimony alloy molten liquid (wherein the mass percent composition of antimony is preferably 79.35%; the mass percent composition of lead is preferably 20.63%) at 630° C. is covered with carnallite on the liquid surface. Condensation treatment is carried out under the condition of halide cover, 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 average particle size of the melt, the seventh antimony-rich melt, the eighth antimony-rich melt and the ninth antimony-rich melt is 62.05 μm, and the conditions and parameters of the coagulation treatment are shown in Table 1. The composition of the product is shown in Table 2.
对比例1Comparative example 1
将100kg温度为500℃的铅锑合金熔融液(其中锑的质量百分含量优选为21.56％；铅的质量百分含量优选为78.22％)，在液面上加入光卤石进行覆盖，在光卤石覆盖的条件下进行凝析处理，第一富锑熔体、第二富锑熔体、第三富锑熔体、第四富锑熔体、第五富锑熔体、第六富锑熔体、第七富锑熔体、第八富锑熔体和第九富锑熔体的平均粒径为42.68μm，凝析处理的条件参数如表1所示，在凝析处理过程中得到的产物的成分如表2所示。100kg of lead-antimony alloy molten liquid (wherein the mass percentage composition of antimony is preferably 21.56%; the mass percentage composition of lead is preferably 78.22%) at 500°C is covered by adding carnallite on the liquid surface. Condensation treatment is carried out under the condition of halide cover, 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 average particle size of the melt, the seventh antimony-rich melt, the eighth antimony-rich melt and the ninth antimony-rich melt is 42.68 μm, and the conditions and parameters of the coagulation treatment are shown in Table 1. The composition of the product is shown in Table 2.
表1实施例1～4和对比例1中凝析处理的条件参数The condition parameter of coagulation treatment in the embodiment 1～4 of table 1 and comparative example 1
表2实施例1～4和对比例1梯度处理过程中产物的成分表The composition table of the product in the gradient treatment process of table 2 embodiment 1～4 and comparative example 1
根据表2可以看出，本发明需通过精确控制各加热处理的温度，才能够将锑从铅高锑合金中分离。According to Table 2, it can be seen that the present invention can separate antimony from the lead-high antimony alloy only by precisely controlling the temperature of each heat treatment.
尽管上述实施例对本发明做出了详尽的描述，但它仅仅是本发明一部分实施例，而不是全部实施例，还可以根据本实施例在不经创造性前提下获得其他实施例，这些实施例都属于本发明保护范围。Although the foregoing embodiment has described the present invention in detail, it is only a part of the embodiments of the present invention, rather than all embodiments, and other embodiments can also be obtained according to the present embodiment without inventive step, and these embodiments are all Belong to the protection scope of the present invention.
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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 |
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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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