CN105618777A - Method for preparing metal lead powder through vacuum carbothermal reduction - Google Patents
Method for preparing metal lead powder through vacuum carbothermal reduction Download PDFInfo
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- CN105618777A CN105618777A CN201610000219.0A CN201610000219A CN105618777A CN 105618777 A CN105618777 A CN 105618777A CN 201610000219 A CN201610000219 A CN 201610000219A CN 105618777 A CN105618777 A CN 105618777A
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- vacuum
- lead powder
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- carbothermal reduction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material
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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
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The method relates to a method for preparing metal lead powder through vacuum carbothermal reduction. The method comprises the following steps: blending zinc smelting leaching residue with a reducing agent in a mass ratio of (5-20): 1, and breaking and evenly mixing the materials to obtain a mixture; pressing the mixture on a tablet press into lump materials; loading the lump materials into a high temperature-resistant crucible of which a upper opening is open, and then placing the crucible into a vacuum furnace; arranging a furnace cover with a condensation disc above the crucible in the furnace, starting the vacuum furnace after the furnace cover is closed, heating to the range of 500-1000 DEG C at a temperature rise rate of 5-20 DEG C per minute, preserving heat for 1-8 hours, and controlling the pressure in the vacuum furnace to be less than or equal to 100Pa; and after the reduction reaction is finished, carrying out cooling, and opening the furnace to take out materials, thereby obtaining the product metal lead powder on the condensation disc, and obtaining reducing slag in the high temperature-resistant crucible. The method for preparing the metal lead powder through the vacuum carbothermal reduction is capable of obtaining the metal lead powder through one-step vacuum reduction smelting; the method has the advantages of short process flow, relatively low reaction temperature, easy heating, convenient operation and control, no production of lead oxide smoke dust, no environmental pollution, stable and reliable lead powder quality, satisfaction of quality standard, high lead recovery, low cost, and high comprehensive utilization level of resources.
Description
Technical field
The present invention relates to a kind of method that vacuum carbothermal reduction prepares metal lead powder, belong to the technical field of zinc abstraction leached mud synthetical recovery.
Background technology
At present, the leached mud of zinc abstraction factory output, main sulfur-bearing lead plumbate, the industrialized preparing process of this slag is: send pyrometallurgical smelting of lead system, after adding slag former, flux and the reducing agent such as substantial amounts of troilite or ferrum oxide, quartz, limestone, coal, under blasting compression air or excess oxygen, carry out aoxidizing and reducing two sections of meltings, output lead bullion, lead oxide flue dust and a large amount of slag (abandoning slag). Lead pig product is obtained after the refining of lead bullion.
Adopting the leached mud of this conventional process zinc abstraction factory output, Problems existing is: 1, need to add a large amount of slag former, flux, reducing agent and compression air and oxygen, consuming cost; 2, the oxidation of lead sulfate and reduction melting are the endothermic reaction, need to consume substantial amounts of fuel, and energy consumption index is much larger than the pyrometallurgical smelting of concentrate of lead sulfide ore; 3, the lead oxide flue dust of output also needs return to process, and the quantity of slag of output slag is big, and in slag, valuable metal grade is by dilution, can only abandon, and causes valuable metal to lose.
At present, the product that the plumbous smelting enterprise of more than 95% produces is lead pig, it is impossible to directly output metal lead powder. But in fields such as ceramic metal, chemical products, low-melting alloy goods, radiation shielding coating, erosion shield, powder metallurgy oil-free lubricating agent, traditional Chinese Painting sole pigment, lead battery and organic synthesiss, it is necessary to use metal lead powder. Therefore, the metal lead powder that these industries use again melts post-treatment and becomes metal lead powder, repeat consumption processing cost mainly through lead pig.
Summary of the invention
It is an object of the invention to for above-mentioned existing industrial technology Problems existing, it is proposed to a kind of vacuum carbothermal reduction prepares the method for metal lead powder, the method only needs a step vacuum reduction melting can obtain metal lead powder, technological process is short, product quality is high, and production cost is low, free from environmental pollution.
The purpose of the present invention realizes by the following means:
A kind of vacuum carbothermal reduction prepares the method for metal lead powder, it is characterised in that it has the following steps:
(1) by zinc abstraction leached mud and reducing agent 5 ~ 20:1 dispensing in mass ratio, broken mix homogeneously obtains batch mixing;
(2) batch mixing is pressed on tablet machine block;
(3) block is loaded in high-temperature crucible, crucible is suitable for reading to be opened wide, then put it in vacuum drying oven, crucible in stove is arranged over the bell with condensate pans, vacuum drying oven is started after covering bell, heating to 500 ~ 1000 DEG C with the heating rate of 5 ~ 20 DEG C/min, temperature retention time is 1 ~ 8 hour, vacuum furnace pressure control��100Pa;
(4) after reduction reaction terminates, cooling, blow-on feeding, condensate pans obtains resultant metal Hydrocerussitum (Ceruse), in high-temperature crucible, obtains reducing slag.
Zinc abstraction leached mud described in step (1) be mainly composed of lead sulfate. Lead content is be more than or equal to 45%.
Reducing agent described in step (1) is the one in activated carbon, Linesless charcoal, coal and petroleum coke.
Block described in step (2) is cylindrically shaped.
The purity of the resultant metal Hydrocerussitum (Ceruse) described in step (4), more than 99.5%, reaches Hydrocerussitum (Ceruse) quality standard, and described reducing slag is rich in there being the valuable metals such as silver, bismuth, copper, antimony.
The feature of the present invention: the method only needs a step vacuum reduction melting to can be obtained by metal lead powder, and technological process is greatly shortened, and techno-economic effect is obvious. There is reduction reaction in zinc abstraction leached mud (furnace pressure control��100Pa) under vacuum, reduce reaction temperature, and the thermal source of heating is mainly electric energy, also without adding slag former, flux, compression air and oxygen in course of reaction, not output lead oxide flue dust, non-environmental-pollution, Hydrocerussitum (Ceruse) steady quality is reliable, meet relevant quality standard, lead recovery is high, and less costly, the reducing slag of output is rich in there being the valuable metals such as silver, bismuth, copper, antimony, precious metal smelting system can be fed directly to and carry out synthetical recovery, improve waste and old level of resource utilization.
Accompanying drawing explanation
Fig. 1 is the principle process chart of the present invention.
Fig. 2 is crucible and the condenser location diagram in vacuum drying oven of the present invention.
In Fig. 2, the label of each several part is as follows:
1--is crucible, and 2-is condenser, and 3-is insulation asbestos.
Detailed description of the invention
Next in conjunction with example, the present invention is described in further detail, but the invention is not restricted to these embodiments.
Embodiment one:
(1) 5:1 in mass ratio, takes zinc abstraction leached mud 100g, is mainly composed of lead sulfate, and leaded 50.73%, reducing agent is activated carbon 20g, mixs homogeneously with activated carbon and obtain batch mixing after leached mud is broken.
(2) batch mixing is pressed on tablet machine cylindrical block.
(3) loading in high-temperature crucible by block, crucible is suitable for reading to be opened wide, and then puts it in vacuum drying oven, and the crucible in stove is arranged over the bell with condensate pans. Starting vacuum drying oven after covering bell, heat to 500 DEG C with the heating rate of 5 DEG C/min, temperature retention time is 8 hours, and vacuum furnace pressure controls at 1 ~ 5Pa.
(4) after reduction reaction terminates, cooling, blow-on feeding, condensate pans obtains resultant metal Hydrocerussitum (Ceruse), purity is 99.98%, and composition is in Table 1; Reducing slag is obtained in high-temperature crucible, leaded 3.03%, argentiferous 0.15%, bismuth 2.72%, copper 3.91%, antimony 4.57%. The lead recovery of Hydrocerussitum (Ceruse) is 95.5%.
Table 1 Hydrocerussitum (Ceruse) composition (%)
Embodiment two:
(1) 20:1 in mass ratio, takes zinc abstraction leached mud 100g, is mainly composed of lead sulfate, and leaded 55.36%, reducing agent Linesless charcoal 5g, powder will be mixed homogeneously after broken for leached mud with charcoal powder.
(2) batch mixing is pressed on tablet machine cylindrical block.
(3) loading in high-temperature crucible by block, crucible is suitable for reading to be opened wide, and then puts it in vacuum drying oven, and the crucible in stove is arranged over the bell with condensate pans. Starting vacuum drying oven after covering bell, heat to 650 DEG C with the heating rate of 10 DEG C/min, temperature retention time is 5 hours, and vacuum furnace pressure controls at 5 ~ 10Pa.
(4) after reduction reaction terminates, cooling, blow-on feeding, condensate pans obtains resultant metal Hydrocerussitum (Ceruse), purity is that 99.991% composition is in Table 2; Reducing slag is obtained in high-temperature crucible, leaded 0.64%, argentiferous 0.22%, bismuth 3.51%, copper 4.23%, antimony 5.36%. The lead recovery of Hydrocerussitum (Ceruse) is 98.9%.
Table 2 Hydrocerussitum (Ceruse) composition (%)
Embodiment three:
(1) 10:1 in mass ratio, takes zinc abstraction leached mud 100g, is mainly composed of lead sulfate, and leaded 64.83%, reducing agent is coal 10g, and both obtain batch mixing by broken mix homogeneously.
(2) batch mixing is pressed on tablet machine cylindrical block.
(3) loading in high-temperature crucible by block, crucible is suitable for reading to be opened wide, and then puts it in vacuum drying oven, and the crucible in stove is arranged over the bell with condensate pans. Starting vacuum drying oven after covering bell, heat to 1000 DEG C with the heating rate of 20 DEG C/min, temperature retention time is 1 hour, and vacuum furnace pressure controls at 60 ~ 100Pa.
(4) after reduction reaction terminates, cooling, blow-on feeding, condensate pans obtains resultant metal Hydrocerussitum (Ceruse), purity is 99.995%, and composition is in Table 3; Reducing slag is obtained in high-temperature crucible, leaded 0.15%, argentiferous 0.46%, bismuth 6.24%, copper 9.18%, antimony 12.53%. The lead recovery of Hydrocerussitum (Ceruse) is 99.5%.
Table 3 Hydrocerussitum (Ceruse) composition (%)
In above-mentioned each example, technical process is as shown in Figure 1. After block enters vacuum drying oven, it is positioned in crucible 1, crucible is not added a cover, suitable for reading unlimited, arranging condenser 2 on crucible, this condenser is actual is a plate-like, is fixed on the bell of vacuum drying oven, lead in block is reduced to metallic vapour, and condensation of catching a cold when rising to this condenser is Hydrocerussitum (Ceruse) and comes together in dish. The surrounding of crucible adds insulation asbestos 3. All the other are identical with general vacuum drying oven.
Claims (5)
1. the method that a vacuum carbothermal reduction prepares metal lead powder, it is characterised in that it has the following steps:
(1) by zinc abstraction leached mud and reducing agent 5 ~ 20:1 dispensing in mass ratio, broken mix homogeneously obtains batch mixing;
(2) batch mixing is pressed on tablet machine block;
(3) block is loaded in high-temperature crucible, crucible is suitable for reading to be opened wide, then put it in vacuum drying oven, crucible in stove is arranged over the bell with condensate pans, vacuum drying oven is started after covering bell, heating to 500 ~ 1000 DEG C with the heating rate of 5 ~ 20 DEG C/min, temperature retention time is 1 ~ 8 hour, vacuum furnace pressure control��100Pa;
(4) after reduction reaction terminates, cooling, blow-on feeding, condensate pans obtains resultant metal Hydrocerussitum (Ceruse), in high-temperature crucible, obtains reducing slag.
2. the method that vacuum carbothermal reduction prepares metal lead powder according to claim 1, it is characterised in that the zinc abstraction leached mud described in step (1) be mainly composed of lead sulfate, lead content is be more than or equal to 45%.
3. the method that vacuum carbothermal reduction prepares metal lead powder according to claim 1, it is characterised in that the reducing agent described in step (1) is the one in activated carbon, Linesless charcoal, coal and petroleum coke.
4. the method that vacuum carbothermal reduction prepares metal lead powder according to claim 1, it is characterised in that the block described in step (2) is cylindrically shaped.
5. the method that vacuum carbothermal reduction prepares metal lead powder according to claim 1, it is characterised in that the purity of the resultant metal Hydrocerussitum (Ceruse) described in step (4), more than 99.5%, reaches Hydrocerussitum (Ceruse) quality standard.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610000219.0A CN105618777A (en) | 2016-01-02 | 2016-01-02 | Method for preparing metal lead powder through vacuum carbothermal reduction |
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| CN201610000219.0A CN105618777A (en) | 2016-01-02 | 2016-01-02 | Method for preparing metal lead powder through vacuum carbothermal reduction |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107419109A (en) * | 2017-08-05 | 2017-12-01 | 重庆科技学院 | A kind of method that metallic lead is reclaimed from lead chloride |
| CN114737057A (en) * | 2022-03-24 | 2022-07-12 | 东北大学 | Method for preparing high vapor pressure metal by carbothermic reduction |
| CN115478169A (en) * | 2022-09-13 | 2022-12-16 | 六盘水中联工贸实业有限公司 | Microwave vacuum smelting method for lead sulfate slag |
Citations (5)
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| JPS5579842A (en) * | 1978-12-13 | 1980-06-16 | Dowa Mining Co Ltd | Lead concentrate treating method |
| CN1147021A (en) * | 1995-05-31 | 1997-04-09 | 爱知制钢株式会社 | Method and apparatus of treating dusts containing oxides |
| CN101709373A (en) * | 2009-11-18 | 2010-05-19 | 云南冶金集团股份有限公司技术中心 | Method and system for treating lead-zinc sulfide ores |
| CN202705427U (en) * | 2012-01-05 | 2013-01-30 | 中国科学院生态环境研究中心 | Vacuum furnace using waste leaded glass to synthesize nanometer lead |
| CN103100719A (en) * | 2012-11-12 | 2013-05-15 | 柳州百韧特先进材料有限公司 | Technological process for producing zinc powder |
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2016
- 2016-01-02 CN CN201610000219.0A patent/CN105618777A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5579842A (en) * | 1978-12-13 | 1980-06-16 | Dowa Mining Co Ltd | Lead concentrate treating method |
| CN1147021A (en) * | 1995-05-31 | 1997-04-09 | 爱知制钢株式会社 | Method and apparatus of treating dusts containing oxides |
| CN101709373A (en) * | 2009-11-18 | 2010-05-19 | 云南冶金集团股份有限公司技术中心 | Method and system for treating lead-zinc sulfide ores |
| CN202705427U (en) * | 2012-01-05 | 2013-01-30 | 中国科学院生态环境研究中心 | Vacuum furnace using waste leaded glass to synthesize nanometer lead |
| CN103100719A (en) * | 2012-11-12 | 2013-05-15 | 柳州百韧特先进材料有限公司 | Technological process for producing zinc powder |
Non-Patent Citations (2)
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107419109A (en) * | 2017-08-05 | 2017-12-01 | 重庆科技学院 | A kind of method that metallic lead is reclaimed from lead chloride |
| CN114737057A (en) * | 2022-03-24 | 2022-07-12 | 东北大学 | Method for preparing high vapor pressure metal by carbothermic reduction |
| CN114737057B (en) * | 2022-03-24 | 2024-03-26 | 东北大学 | Method for preparing high vapor pressure metal by carbothermal reduction |
| CN115478169A (en) * | 2022-09-13 | 2022-12-16 | 六盘水中联工贸实业有限公司 | Microwave vacuum smelting method for lead sulfate slag |
| CN115478169B (en) * | 2022-09-13 | 2023-08-18 | 六盘水中联工贸实业有限公司 | Microwave vacuum smelting method for lead sulfate slag |
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