WO2019223559A1 - 一种用于再生粗铅精炼的选择性除锑砷保锡剂及使用方法 - Google Patents
一种用于再生粗铅精炼的选择性除锑砷保锡剂及使用方法 Download PDFInfo
- Publication number
- WO2019223559A1 WO2019223559A1 PCT/CN2019/086506 CN2019086506W WO2019223559A1 WO 2019223559 A1 WO2019223559 A1 WO 2019223559A1 CN 2019086506 W CN2019086506 W CN 2019086506W WO 2019223559 A1 WO2019223559 A1 WO 2019223559A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- antimony
- arsenic
- lead
- tin
- retaining agent
- Prior art date
Links
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
- C22B13/00—Obtaining lead
- C22B13/06—Refining
- C22B13/08—Separating metals from lead by precipitating, e.g. Parkes process
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/06—Refining
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C24/00—Alloys based on an alkali or an alkaline earth metal
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
-
- 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
Definitions
- the invention relates to the field of refining and impurity removal of regenerated crude lead, and in particular to a selective antimony, arsenic and tin retaining agent used for refining regenerated crude lead and a method for using the same.
- crude lead contains impurities such as antimony, tin, arsenic, iron, cadmium, and copper, and impurities in the crude lead must be refined to remove impurities.
- Traditional lead refining removes impurities such as antimony, arsenic, and tin.
- Oxidative refining removes impurities by oxidizing slag with oxygen in the air.
- Basic refining uses sodium nitrate as an oxidant The impurities are oxidized and slag is removed.
- the purpose of the present invention is to provide a selective antimony and arsenic tin retaining agent for regenerating crude lead refining and a method for using the same, to solve the problem that a large amount of tin resources are wasted in the prior art oxidation refining and alkaline refining methods.
- antimony and arsenic tin retaining agents are composed of 10-30 wt% aluminum, 65-85 wt% calcium, 1-10 wt% coke powder, and 1-2 wt%.
- Composition of lead powder; calcium, aluminum, coke powder, and lead powder are thoroughly mixed according to the above-mentioned mass ratio to prepare an antimony and arsenic tin retaining agent.
- the selective antimony arsenic tin retaining agent is composed of 10% by weight of aluminum, 80% by weight of calcium, 8% by weight of coke powder, and 2% by weight of lead powder based on its total mass of 100.
- the selective antimony arsenic tin retaining agent is composed of 25% by weight of aluminum, 72% by weight of calcium, 2% by weight of coke powder, and 1% by weight of lead powder based on its total mass of 100.
- the selective antimony arsenic tin retaining agent is composed of 30 wt% aluminum, 67 wt% calcium 2 wt% coke powder, and 1 wt% lead powder based on its total mass of 100.
- the selective antimony and arsenic tin remover of the present invention is applied to the production of antimony and arsenic by refining primary lead and the production of antimony and arsenic by refining crude lead.
- the method for removing the antimony and arsenic in crude lead by using the selective antimony arsenic and tin retaining agent refining the regenerated crude lead includes the following steps:
- Step (1) Weigh the components according to the mass ratio, and mix the components uniformly to form an antimony and arsenic removing composition
- Step (2) The antimony and arsenic-removed crude lead is heated and melted to a temperature of 340-500 ° C, a sample is taken, and the sample is subjected to spectral analysis to obtain the total antimony-arsenic content in the pot, which is heated to 580-650 ° C, and then the antimony is removed.
- the amount of antimony arsenic tin retaining agent is calculated based on 1-1.5 times of the total antimony arsenic content. Turn on the mixer and stir the lead solution to generate a vortex. Does not affect the normal existence of the vortex.
- the antimony arsenic remover is melted into the lead solution to form antimony compound with antimony arsenide and floats on the liquid surface of the lead solution. After adding the antimony remover, the arsenic remover is continued to stir for 10 to 60 minutes;
- Step (3) Allow to cool down, reduce the temperature of the lead solution after the reaction to below 480 ° C, add coal powder or sawdust and stir to remove the remaining calcium and aluminum until the white paste-like residue becomes a loose black powder. The slag was removed, and the antimony and arsenic in the lead solution dropped to less than 0.0005%, and the tin content remained basically unchanged.
- the coke powder in the antimony, arsenic and tin removal agent described in the invention can avoid the slag formation of lead liquid at high temperature, which is beneficial to prevent the oxidation of lead.
- the agent is fully and rapidly dissolved in the lead solution; the calcium and aluminum in the antimony, arsenic, and tin retention agent can react with antimony and arsenic at high temperatures to form antimonides and arsenides; during the process of removing antimony and arsenic, the antimonides, Arsenide has a high melting point, low solubility in lead solution, and its density is less than that of lead. It can be precipitated from the lead solution and float on top of the lead solution to become scum.
- the antimony compound is stirred by the mixer.
- the arsenic compound is further floated and removed from the lead solution to achieve the deep separation of antimony, arsenic and lead solution.
- the antimony and arsenic content in the lead solution can be below 0.0005%, while the tin content is basically unchanged.
- the invention Compared with the existing crude lead antimony and arsenic removal method, the invention has the following advantages:
- the content of antimony and arsenic in lead is as low as 0.0005%, which is far lower than the national standard, and the removal rate of antimony and arsenic is high.
- the operation method is simple and reliable, the application range is wide, the process is smokeless and tasteless, and the working environment is good.
- the antimony-removing arsenic tin retaining agent of the present invention is composed of 10-30% by weight of aluminum, 65-85% by weight of calcium, 1-10% by weight of coke powder, and 1-2% by weight of lead powder; , Aluminum, coke powder, and lead powder are thoroughly mixed according to the above-mentioned mass ratio to prepare an antimony, arsenic and tin retaining agent.
- the selective antimony arsenic tin retaining agent is composed of 10% by weight of aluminum, 80% by weight of calcium, 8% by weight of coke powder, and 2% by weight of lead powder based on its total mass of 100.
- the selective antimony arsenic tin retaining agent is composed of 25% by weight of aluminum, 72% by weight of calcium, 2% by weight of coke powder, and 1% by weight of lead powder based on its total mass of 100.
- the selective antimony arsenic tin retaining agent is composed of 30 wt% aluminum, 67 wt% calcium 2 wt% coke powder, and 1 wt% lead powder based on its total mass of 100.
- the selective antimony and arsenic tin remover of the present invention is applied to the production of antimony and arsenic by refining primary lead and the production of antimony and arsenic by refining crude lead.
- the method for removing the antimony and arsenic in crude lead by using the selective antimony arsenic and tin retaining agent refining the regenerated crude lead includes the following steps:
- Step (1) Weigh the components according to the mass ratio, and mix the components uniformly to form an antimony and arsenic removing composition
- Step (2) Take a sample and perform spectral analysis on the sample to obtain the total antimony and arsenic content in the pot.
- the temperature is raised to 580-650 ° C, and then the antimony and arsenic removal tin retaining agent is added to the refining pot.
- the amount is calculated according to 1-1.5 times of the total antimony and arsenic content.
- the speed of adding the antimony arsenic tin retaining agent should not affect the normal existence of the vortex.
- the antimony arsenic tin retaining agent melts quickly.
- Antimony and arsenic are synthesized in the lead solution to form antimony compounds and float on the liquid surface of the lead solution. After adding the antimony and arsenic removing agent, continue stirring for 10 to 60 minutes;
- Step (3) Allow to cool down, reduce the temperature of the lead solution after the reaction to below 480 ° C, add coal powder or sawdust and stir to remove the remaining calcium and aluminum until the white paste-like residue becomes a loose black powder. Remove the antimony and arsenic in the lead solution to less than 0.0005%, and the tin content is basically unchanged.
- Example 1 A selective antimony, arsenic, and tin retention agent, based on its total mass of 100, is composed of 10% by weight of aluminum, 80% by weight of calcium, 8% by weight of coke powder, and 2% by weight of lead powder.
- the slag is weighed and sampled for direct reading spectrum analysis.
- the composition is as follows: Cu0.0007%, Sb 0.25%, As 0.0051%, Sn 0.615%, Bi 0.003% Ag 0.0008%, continue to heat up to 635 ° C to obtain the total antimony and arsenic content of the pot. Add 1.3 times the total antimony and arsenic content to remove the antimony and arsenic composition.
- the ingredients are: 10 wt% Al, 80 wt% Ca, 8 wt% coke powder, and 2 wt% lead powder.
- Example 2 A selective antimony, arsenic, and tin retention agent, based on its total mass of 100, was composed of 25 wt% aluminum, 72 wt% calcium, 2 wt% coke powder, and 1 wt% lead powder.
- the slag is weighed and sampled for direct reading spectrum analysis.
- the composition is as follows: Cu0.0005%, Sb 0.15% As 0.0031%, Sn 0.517%, Bi 0.0026% Ag0.001%, continue heating to 605 ° C to obtain the total antimony and arsenic content of the pot. Add 1.2 times the total antimony and arsenic content to remove the antimony and arsenic composition and composition.
- the ingredients are: 25 wt% Al, 72 wt% Ca, 2 wt% coke powder, and 1 wt% lead powder.
- the composition is as follows: Cu0.0005%, Sb 0.0003%, As 0.0002%, Sn 0.501%, Bi 0.0026% Ag0.00098%.
- Example 3 Selective removal of antimony, arsenic, and tin retaining agent, based on its total mass of 100, consisting of 30 wt% aluminum, 67 wt% calcium 2 wt% coke powder, and 1 wt% lead powder.
- composition is as follows: Cu0.0003%, Sb 0.08% As 0.0041%, Sn 0.685%, Bi 0.0027% Ag0.0007%, continue heating and heating to 595 ° C to obtain the total antimony arsenic content of the pot, according to 1.4 times the total antimony arsenic content, add antimony and arsenic composition, composition
- the components are: 30 wt% Al, 67 wt% Ca, 8 wt% coke powder, and 2 wt% lead powder.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
Claims (2)
- 一种用于再生粗铅精炼的选择性除锑砷保锡剂,其特征是:除锑砷保锡剂以其总质量100为基准由10~30wt%的铝、65~85wt%的钙、1~10wt%的焦粉和1~2wt%的铅粉组成;将钙、铝、焦粉、铅粉按上述质量配比充分混合,制得除锑砷保锡剂。
- 采用权利要求1所述的一种用于再生粗铅精炼的选择性除锑砷保锡剂的使用方法,其特征是:选择性除锑砷保锡剂应用于原生铅的精炼除锑、砷生产以及再生粗铅精炼除锑、砷生产;其使用方法,包括以下步骤:步骤(1):按照质量配比称好各组分,将各组分均匀混合形成除锑、砷组合物;步骤(2):取样,对样品进行光谱分析,得到锅中的锑砷总含量,升温到580-650℃,然后将除锑砷保锡剂加入至精炼锅中,除锑砷保锡剂加入的量按锑砷总含量的1-1.5倍计算;开启搅拌机,搅拌铅液产生旋涡,投入除锑砷保锡剂的速度应不影响漩涡的正常存在,除锑砷保锡剂熔入铅液中与锑砷化合成锑化物而浮在铅液的液面,加完除锑砷保锡剂后继续搅拌10~60min;步骤(3):静置降温,将反应后的铅液温度降至480℃以下,加入造渣剂或锯末搅拌除去剩余的钙、铝,直到白色糊状渣变成疏松黑色粉状为止,将渣捞出,铅液中的锑、砷降至0.0005%以下,锡含量基本不变。
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP19806405.7A EP3805413A4 (en) | 2018-05-25 | 2019-05-12 | SELECTIVE ANTIMONY AND ARSENIC REMOVAL AND TIN RETAINING AGENT FOR REFINING SECONDARY RAW LEAD, AND METHOD OF USE |
US17/058,136 US11414724B2 (en) | 2018-05-25 | 2019-05-12 | Agent for selective antimony and arsenic removal and tin retaining for refining secondary crude lead, and use method thereof |
AU2019274901A AU2019274901A1 (en) | 2018-05-25 | 2019-05-12 | Selective antimony and arsenic removal and tin retaining agent for refining secondary crude lead, and use method |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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CN201810518994.4 | 2018-05-25 | ||
CN201810518994.4A CN108707761B (zh) | 2018-05-25 | 2018-05-25 | 一种用于再生粗铅精炼的选择性除锑砷保锡剂及使用方法 |
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WO2019223559A1 true WO2019223559A1 (zh) | 2019-11-28 |
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PCT/CN2019/086506 WO2019223559A1 (zh) | 2018-05-25 | 2019-05-12 | 一种用于再生粗铅精炼的选择性除锑砷保锡剂及使用方法 |
Country Status (5)
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US (1) | US11414724B2 (zh) |
EP (1) | EP3805413A4 (zh) |
CN (1) | CN108707761B (zh) |
AU (1) | AU2019274901A1 (zh) |
WO (1) | WO2019223559A1 (zh) |
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CN108707761B (zh) | 2018-05-25 | 2019-10-29 | 江苏新春兴再生资源有限责任公司 | 一种用于再生粗铅精炼的选择性除锑砷保锡剂及使用方法 |
CN113684386A (zh) * | 2021-08-17 | 2021-11-23 | 尤全仁 | 一种粗杂铅精炼再生铅锡基多元素合金的方法 |
CN113737020B (zh) * | 2021-09-10 | 2022-09-13 | 广西万仕智稀贵金属科技有限公司 | 一种粗锑精炼过程深度除镉的方法 |
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- 2019-05-12 AU AU2019274901A patent/AU2019274901A1/en not_active Abandoned
- 2019-05-12 WO PCT/CN2019/086506 patent/WO2019223559A1/zh unknown
- 2019-05-12 EP EP19806405.7A patent/EP3805413A4/en not_active Withdrawn
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Also Published As
Publication number | Publication date |
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CN108707761B (zh) | 2019-10-29 |
US20210198770A1 (en) | 2021-07-01 |
CN108707761A (zh) | 2018-10-26 |
AU2019274901A1 (en) | 2020-12-03 |
US11414724B2 (en) | 2022-08-16 |
EP3805413A4 (en) | 2022-03-09 |
EP3805413A1 (en) | 2021-04-14 |
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