CN109055776A - The extracting method of Zn-ef ficiency in low-grade lead zinc ore - Google Patents
The extracting method of Zn-ef ficiency in low-grade lead zinc ore Download PDFInfo
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- CN109055776A CN109055776A CN201811052106.0A CN201811052106A CN109055776A CN 109055776 A CN109055776 A CN 109055776A CN 201811052106 A CN201811052106 A CN 201811052106A CN 109055776 A CN109055776 A CN 109055776A
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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
- C22B19/00—Obtaining zinc or zinc oxide
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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
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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Abstract
The present invention provides a kind of extracting methods of Zn-ef ficiency in low-grade lead zinc ore.Device used in the extracting method includes vacuum reduction smelting device, the total content of lead element and Zn-ef ficiency in low-grade lead zinc ore is lower than 20wt%, and Zn-ef ficiency and lead element exist in the form of zinc silicate, zinc carbonate, zinc sulphide, ceruse and vulcanized lead symbiosis, extracting method includes: in vacuum reduction smelting device, low-grade lead zinc ore, reproducibility fuel and cerussite are subjected to reducing and smelting, obtain metallic zinc and containing lead skim.Metallic zinc and metallic lead are prepared compared to other raw materials, the present invention uses low-grade lead-zinc to prepare metallic zinc and metallic lead for raw material, this is conducive to that preparation cost is greatly reduced.And by said extracted method, by the Zn-ef ficiency in low-grade lead-zinc, concentration and separation is come out in the form of zinc simple substance, and the reduction volatilization rate of Zn-ef ficiency can reach 99% or so in raw material.
Description
Technical field
The present invention relates to metal smelt fields, in particular to a kind of extraction side of Zn-ef ficiency in low-grade lead zinc ore
Method.
Background technique
Lead, zinc are two important specieses in ten kinds of common non-ferrous metals, and application field is extensive, and interrelationship between industries is high,
There is importance status, significance level is only second to copper and aluminium in national economy and social development.From the point of view of endowment of resources, lead zinc
Mine is typically all lead zinc symbiosis, can respectively obtain lead concentrate and zinc concentrate by ore dressing.With lead concentrate and zinc concentrate resource
Continually develop utilization and consumption, the development and utilization of low-grade lead-zinc resource receives more and more attention.For
Superior resources Transformation Strategies are increased, excavate the market value of resource energetically, realizes that resource value maximizes, studies low-grade oxidation
The comprehensive resource of Pb-Zn deposits, which recycles, has very major and immediate significance.
The reserves of low-grade lead-zinc at home and abroad are very rich, and ore main feature has following two points:
(1) due to the deep oxidation of ore, primary slime is more, and particle is thinner, is handled with general beneficiation method, and ore dressing is returned
Yield is lower, will cause the loss and waste of resource；
(2) in ore it is leaded, zinc is lower, and valuable metals such as richer germanium, cadmium of association.
Currently, both at home and abroad for low-grade lead-zinc pyrometallurgical smelting process research it is less, mostly use floatation or
The hydrometallurgical method of person separates and is enriched with lead Zn-ef ficiency therein.In above-mentioned treatment process, it is desirable that low-grade lead-zinc
Degree of oxidation with higher, and zinc silicate, zinc carbonate, zinc sulphide, ceruse and the low-grade lead oxide zinc of vulcanized lead symbiosis
Mine is often difficult to be effectively separated lead element and Zn-ef ficiency by floatation or hydrometallurgy.
Summary of the invention
It is existing to solve the main purpose of the present invention is to provide a kind of extracting method of Zn-ef ficiency in low-grade lead zinc ore
Separation method can not be in the low-grade lead oxide zinc with zinc silicate, zinc carbonate, zinc sulphide, ceruse and vulcanized lead symbiosis
The problem of lead element and Zn-ef ficiency are effectively separated.
To achieve the goals above, a kind of extracting method of Zn-ef ficiency in low-grade lead zinc ore is provided according to the present invention,
Device used in extracting method includes vacuum reduction smelting device, and the lead element and Zn-ef ficiency in low-grade lead zinc ore always contain
Amount is lower than 20wt%, and Zn-ef ficiency and lead element are in the form of zinc silicate, zinc carbonate, zinc sulphide, ceruse and vulcanized lead symbiosis
In the presence of extracting method includes: to carry out low-grade lead zinc ore, reproducibility fuel and cerussite in vacuum reduction smelting device
Reducing and smelting obtains metallic zinc and containing lead skim.
Further, before carrying out reducing and smelting, extracting method further include: by low-grade lead zinc ore, reproducibility fuel
It is successively ground with the mixture of cerussite, compression process, obtains blank；Blank is subjected to reducing and smelting reaction, obtains gold
Belong to zinc and contains lead skim；Preferably, process of lapping includes the steps that grinding mixture using ball mill, more preferable ball mill
Revolving speed be 100~600rpm, milling time be 2~10h.
Further, pressing process includes the steps that suppressing said mixture with the pressure of 150~250Mpa.
Further, device used in extracting method further includes cooling device, after carrying out reducing and smelting, extraction side
Method further include: the gaseous products generated in reducing and smelting reaction are cooled down using above-mentioned cooling device, obtain metallic zinc；It is excellent
Selection of land, device used in the extracting method further includes waste-heat recovery device, and the waste-heat recovery device setting is described true
On flow path between empty reducing and smelting device and the cooling device, the extracting method further include: recycled using the waste heat
Device carries out waste heat recycling to the gaseous products generated in reducing and smelting reaction, then using the cooling device to process
The gaseous products of the waste heat recycling step carry out the cooling procedure, obtain the metallic zinc.
Further, the vacuum degree of reducing and smelting process is 1~200Pa, and reaction temperature is 900~1200 DEG C, when reaction
Between be 0.5~2h；Preferably, the vacuum degree of reducing and smelting process is 1~100Pa, and reaction temperature is 1100~1200 DEG C, reaction
Time is 1~2h.
Further, reducing and smelting process is Temperature Programmed Processes, and the process of temperature programming includes: with 5~15 DEG C/min
Rate, by reducing and smelting react reaction system be warming up to reducing and smelting temperature；By reaction system reducing and smelting temperature into
Row heat preservation, the time of insulating process are 0.5~2h；With the rate of 5~15 DEG C/min, reaction system is down to room temperature.
Further, zinc sulphide and ceruse rub in the mixture of low-grade lead zinc ore, reproducibility fuel and cerussite
You are than being 1:0.5~2；Preferably, zinc sulphide and ceruse in the mixture of low-grade lead zinc ore, reproducibility fuel and cerussite
Molar ratio be 1:0.8~1.2.
Further, reproducibility fuel is in the group that charcoal, active carbon, graphite, petroleum coke, coal and carbon black form
It is one or more of.
Further, in low-grade lead zinc ore the Zn-ef ficiency of 90wt% or more with the shape of zinc silicate, zinc carbonate or zinc sulphide
Formula exists, and the lead element of 90wt% or more exists in the form of ceruse and/or vulcanized lead.
It applies the technical scheme of the present invention, prepares metallic zinc and metallic lead compared to other raw materials, the present invention uses low product
Position lead-zinc is that preparation cost is cheaper when raw material prepares metallic zinc and metallic lead, is conducive to the low-grade lead oxide in China
Utilization and the exploitation of zinc ore.By the said extracted method, by the Zn-ef ficiency in low-grade lead-zinc with the shape of zinc simple substance
Formula concentration and separation comes out, and wherein the reduction volatilization rate of Zn-ef ficiency can reach 99% or so in raw material, while also obtaining containing vulcanization
The clinker of lead.In conclusion Zn-ef ficiency and lead member in above-mentioned low-grade lead zinc ore can be efficiently separated using said extracted method
Element, and then improve its economic benefit.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 shows the Zn-ef ficiency of the low-grade lead zinc ore provided in a kind of typical embodiment according to the present invention
The structural schematic diagram of extraction system.
Wherein, the above drawings include the following reference numerals:
10, unit is smelted in vacuum reduction；11, reducing and smelting device；12, vacuum evacuation device；101, feed opening；102, zinc steams
Gas outlet；20, cerussite feeding mechanism；30, low-grade lead zinc ore feeding mechanism；40, crushing and screening device；50, pressure setting；
13, cooling device；14, waste-heat recovery device；60, reproducibility fuel supply device.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.Below in conjunction with embodiment, the present invention will be described in detail.
As described in background technique, some separation methods can not be to zinc silicate, zinc carbonate, zinc sulphide, ceruse
With in the low-grade lead oxide zinc of vulcanized lead symbiosis lead element and Zn-ef ficiency be effectively separated.It is asked to solve above-mentioned technology
Topic, this application provides a kind of extracting method of Zn-ef ficiency in low-grade lead zinc ore, device used in the extracting method includes
Vacuum reduction smelting device, the total content of lead element and Zn-ef ficiency in low-grade lead zinc ore are lower than 20wt%, and Zn-ef ficiency and
Lead element exists in the form of zinc silicate, zinc carbonate, zinc sulphide, ceruse and vulcanized lead symbiosis, and extracting method includes: in vacuum
In reducing and smelting device, low-grade lead zinc ore, reproducibility fuel and cerussite are subjected to reducing and smelting, obtain metallic zinc and leaded
Slag.
In above-mentioned vacuum reduction smelting process, zinc carbonate and ceruse in raw material are decomposed into first in temperature-rise period
With reproducibility fuel reduction reaction can occur for zinc oxide and lead oxide, subsequent zinc oxide and zinc silicate, by low-grade lead oxide zinc
Zn-ef ficiency in mine is separated, and metal zinc fume is obtained.Since atmosphere belongs to strong reducing property gas in vacuum reduction smelting device
Atmosphere, thus vulcanized lead in raw material and zinc sulphide can't reduction volatilizations.Non-volatile zinc sulphide can be sent out with lead oxide in raw material
Raw redox reaction generates vulcanized lead and zinc oxide, and it is anti-that further with reproducibility raw material redox occurs for the zinc oxide of generation
It answers, the Zn-ef ficiency in final zinc sulphide can be also separated in the form of zinc fume.
Metallic zinc and metallic lead are prepared compared to other raw materials, the present invention uses low-grade lead-zinc for raw material preparation
Preparation cost is cheaper when metallic zinc and metallic lead, is conducive to the utilization and exploitation of the low-grade lead-zinc in China.Pass through
The said extracted method, by the Zn-ef ficiency in low-grade lead-zinc, concentration and separation is come out in the form of zinc simple substance, Central Plains
The reduction volatilization rate of Zn-ef ficiency can reach 99% or so in material, while also obtain leaded clinker.In conclusion using said extracted
Method can efficiently separate Zn-ef ficiency and lead element in above-mentioned low-grade lead zinc ore, and then improve its economic benefit.
In order to make the metallic zinc simple substance generated convenient for collecting, it is preferable that device used in said extracted method further includes
Cooling device, after carry out reducing and smelting, extracting method further include: using cooling device to being generated in reducing and smelting reaction
Gaseous products are cooled down, and metallic zinc is obtained；Preferably, device used in said extracted method further includes waste heat recycling dress
It sets, which is arranged on the flow path between vacuum reduction smelting device and cooling device, and said extracted method is also
It include: that waste heat recycling is carried out to the gaseous products generated in reducing and smelting reaction using waste-heat recovery device, then using cooling
Device carries out cooling procedure to by the gaseous products of waste heat recycling step, obtains metallic zinc.
Zn-ef ficiency and lead element in low-grade lead zinc ore can be efficiently separated using said extracted method.A kind of preferred
Embodiment in, before carrying out reducing and smelting, extracting method further include: by low-grade lead zinc ore, reproducibility fuel and white
The mixture of lead ore successively ground, compression process, obtains blank；Blank is subjected to reducing and smelting reaction, obtains metallic zinc
With contain lead skim.
Before reducing and smelting, first raw material is successively ground, is pressed into blank, this not only contributes to improve reduction smelting
The efficiency of refining also helps the generation for reducing fugitive dust, not only contributes to improve entire extraction process so that above-mentioned steps be added
Economy also advantageously improves its feature of environmental protection.
Preferably, process of lapping includes the steps that grinding mixture using ball mill, and more preferable ball mill turns
Speed is 100~600rpm, and milling time is 2~10h.In process of lapping, the revolving speed and milling time of ball mill include but unlimited
In above range, and is limited and advantageously reduce compacting difficulty within the above range.Preferably, pressing process includes with 150
The step of pressure of~250Mpa suppresses said mixture.The pressure of pressing process includes but is not limited to above range,
And limited within the above range, this aspect can make above-mentioned raw materials be pressed into required shape, reduce dust emission, another party
Face also advantageously improves the extent of reaction of blank during reducing and smelting.
In a preferred embodiment, reducing and smelting process carries out under conditions of vacuum degree is 1~200Pa.Also
Former smelting temperature and vacuum degree include but is not limited to above range, and are limited and be conducive to improve Zn-ef ficiency within the above range
Volatilization efficiency and vulcanized lead production rate.
In a preferred embodiment, the vacuum degree of reducing and smelting process is 1~200Pa, and reaction temperature is 900
~1200 DEG C, the reaction time is 0.5~2h.Reaction time, reducing and smelting temperature and the vacuum degree of reducing and smelting process include but
It is not limited to above range, and is limited the life of the volatilization efficiency and vulcanized lead that are conducive to improve Zn-ef ficiency within the above range
At rate.Preferably, the vacuum degree of reducing and smelting process is 1~100Pa, and reaction temperature is 1100~1200 DEG C, the reaction time 1
~2h.
In order to further increase the reduction efficiency of reducing and smelting process, it is preferable that reducing and smelting process uses temperature programming
Mode heat up.It can make above-mentioned reducing and smelting process under more stable elevated temp by the way of temperature programming
It carries out, to be conducive to improve the conversion ratio of reaction raw materials, and then improves the separative efficiency of Zn-ef ficiency and lead element.
In a preferred embodiment, the process of temperature programming is included: and will be restored with the rate of 5~15 DEG C/min
The reaction system for smelting reaction is warming up to reducing and smelting temperature；Reaction system is kept the temperature in reducing and smelting temperature, was kept the temperature
The time of journey is 0.5~2h；With the rate of 5~15 DEG C/min, the reaction system of reducing and smelting is down to room temperature.
Temperature and heating or rate of temperature fall in Temperature Programmed Processes in each temperature control section include but is not limited to above range, and
The separative efficiency and conversion ratio for being conducive to further increase Zn-ef ficiency and lead element within the above range are limited, and then advantageous
In the economic benefit for improving said extracted process.
Preferably, above-mentioned vacuum reduction smelting device is vacuum drying oven.
In a preferred embodiment, vulcanize in the mixture of low-grade lead zinc ore, reproducibility fuel and cerussite
The molar ratio of zinc and ceruse is 1:0.5~2.The molar ratio of zinc sulphide and ceruse includes but is not limited to above range, and incite somebody to action
It limits the rate of recovery and separative efficiency that can be conducive to improve Zn-ef ficiency and lead element within the above range.Preferably, low product
The molar ratio of zinc sulphide and ceruse is 1:0.8~1.2 in the mixture of position Pb-Zn deposits, reproducibility fuel and cerussite.
During above-mentioned reducing and smelting, the reproducibility raw material of this field routine can choose.In a kind of preferred embodiment party
In formula, reproducibility fuel includes but is not limited to one of charcoal, active carbon, graphite, petroleum coke, coal and group of carbon black composition
Or it is several.
Preferably, in low-grade lead zinc ore the Zn-ef ficiency of 90wt% or more in the form of zinc silicate, zinc carbonate or zinc sulphide
In the presence of the lead element of 90wt% or more exists in the form of ceruse and/or vulcanized lead.Had using the raw material with above-mentioned composition
Conducive to the rate of recovery for further increasing Zn-ef ficiency and lead element.
Another invention of the application additionally provides a kind of extraction system of the Zn-ef ficiency of low-grade lead zinc ore, as shown in Figure 1,
Said extracted system includes: that unit 10 and cerussite feeding mechanism 20 are smelted in vacuum reduction, and vacuum reduction is smelted unit 10 and is arranged
There are feed opening 101 and zinc fume outlet 102, feed opening 101 is used to add the Zn-ef ficiency of cerussite and low-grade lead zinc ore；Zinc powder
Mine feeding mechanism 20 is provided with cerussite supply opening, and cerussite supply opening is connected to feed opening 101.
In said extracted system, is smelted in unit 10 by cerussite feeding mechanism 20 to vacuum reduction and supply cerussite.
In vacuum reduction smelting process, zinc carbonate and ceruse in raw material are decomposed into zinc oxide and oxidation in temperature-rise period first
With reproducibility fuel reduction reaction can occur for lead, subsequent zinc oxide and zinc silicate, by the Zn-ef ficiency in low-grade lead-zinc
It separates, obtains metal zinc fume.Since atmosphere belongs to strong reducing property atmosphere in vacuum reduction smelting device, thus in raw material
Vulcanized lead and zinc sulphide can't reduction volatilization.With lead oxide in raw material redox reaction can occur for non-volatile zinc sulphide
Vulcanized lead and zinc oxide are generated, further with reproducibility raw material redox reaction, final zinc sulphide occur for the zinc oxide of generation
In Zn-ef ficiency can be also separated in the form of zinc fume.
The device that metallic zincs and metallic lead are extracted compared to other, in processing system provided by the invention, use is low-grade
Lead-zinc is that preparation cost is cheaper when raw material prepares metallic zinc and metallic lead, is conducive to the low-grade lead oxide zinc in China
Utilization and the exploitation of mine.Through the said extracted system, by the Zn-ef ficiency in low-grade lead-zinc in the form of zinc simple substance
Concentration and separation comes out, and wherein the reduction volatilization rate of Zn-ef ficiency while also obtaining leaded clinker 99% or so in raw material.To sum up institute
It states, Zn-ef ficiency and lead element in above-mentioned low-grade lead zinc ore can be efficiently separated using said extracted system, and then improve its warp
Ji benefit.
In a preferred embodiment, as shown in Figure 1, it includes: reducing and smelting that unit 10 is smelted in above-mentioned vacuum reduction
Device 11 and vacuum evacuation device 12, reducing and smelting device 11 are provided with feed opening 101 and zinc fume outlet 102, vacuum evacuation device
12 for making have vacuum environment in reducing and smelting device 11.The structure that unit 10 is smelted in vacuum reduction is including but not limited to above-mentioned
A kind of structure, as long as can be to produce vacuum environment in reducing and smelting device 11.By above-mentioned smelting process in vacuum ring
It is not oxidized that the zinc simple substance for enabling to extract is smelted under border, to obtain the higher metal zinc product of purity.
In a preferred embodiment, as shown in Figure 1, said extracted system further includes low-grade lead zinc ore supply dress
30 and reproducibility fuel supply device 60 are set, low-grade lead zinc ore feeding mechanism 30 is provided with low-grade lead zinc ore supply opening, also
Originality fuel supply device 60 is provided with reproducibility fuel supply opening, low-grade lead zinc ore supply opening and reproducibility fuel supply opening
It is connected to feed opening 101.Setting low-grade lead zinc ore feeding mechanism 30 and with reproducibility fuel supply device 60 be conducive into
One step improves the degree of automation of said extracted system, and then advantageously reduces the labor intensity of operator.
In a preferred embodiment, it as shown in Figure 1, said extracted system further includes crushing and screening device 40, breaks
Broken screening plant 40 be provided with screening materials carrying entrance and screening materials carrying outlet, screening materials carrying entrance respectively with cerussite supply opening,
Low-grade lead zinc ore supply opening and reproducibility fuel supply opening are connected, and screening materials carrying outlet is defeated by raw material with feed opening 101
Send pipeline connection.Crushing and screening device 40, which is arranged, to be crushed and be sieved before raw material carries out reducing and smelting, this is advantageous
In the contact area for improving reaction raw materials, and then improve the extent of reaction of reducing and smelting.
In a preferred embodiment, as shown in Figure 1, said extracted system further includes pressure setting 50, compacting dress
It sets on the feed line road that 50 are arranged between crushing and screening device 40 and reducing and smelting device 11.Before reducing and smelting,
The raw material being discharged in crushing and screening device 40 is first passed through pressure setting 50, to be compressed into blank, this not only contributes to mention
The efficiency of high reducing and smelting also helps the generation for reducing fugitive dust, entirely mentions so that above-mentioned steps be added and not only contribute to improve
The economy of taking technique also advantageously improves its feature of environmental protection.
In order to make the metallic zinc simple substance generated convenient for collecting, in a preferred embodiment, as shown in Figure 1, above-mentioned
Extraction system further includes cooling device 13, and the zinc between zinc fume outlet 102 and vacuum evacuation device 12 is arranged in cooling device 13
Vapor pipe road, cooling device 13 is for making the zinc fume being discharged from reducing and smelting device 11 be converted into solid-state.
In a preferred embodiment, remaining as shown in Figure 1, said extracted system further includes waste-heat recovery device 14
Heat recovery apparatus 14 is arranged on the zinc fume transfer pipeline between zinc fume outlet 102 and cooling device 13.In off-gas recovery
Waste-heat recovery device 14 is set on pipeline and is conducive to improve the energy utilization rate of entire extraction process, while being conducive to improve containing zinc
Steam is converted to the efficiency of zinc oxide dust.
In a preferred embodiment, said extracted system further includes temperature monitoring device, and temperature monitoring device is used
Temperature in real-time monitoring reducing and smelting device 11.Temperature monitoring device is arranged can be to the temperature in reducing and smelting device 11
Real-time monitoring is carried out, so as to more accurately control the temperature of reducing and smelting process, improves the reduction efficiency of Zn-ef ficiency.
The application is described in further detail below in conjunction with specific embodiment, these embodiments should not be understood as limitation originally
Apply for range claimed.
The Zn-ef ficiency of low-grade lead zinc ore is extracted using extraction element shown in FIG. 1 in embodiment 1 to 7.
The main object phase constituent of 1 middle-low grade lead-zinc of embodiment 1 to 7 and comparative example has dolomite (CaMg
(CO3)2), zincblende (Zn0.776Fe0.224S), calcite (CaCO3), cerussite (PbCO3) and smithsonite (Zn4Si2O7(OH)2·
H2O) etc..The sample that p- 0.074mm accounts for 100% respectively has carried out the chemical phase analysis of lead, zinc.In ore, the chemicals of lead
It is mainly mutually ceruse and vulcanized lead, accounts for the 74.10wt% and 15.47wt% of lead object phase total amount respectively；The chemical and physical phase master of zinc
If zinc carbonate, zinc silicate and zinc sulphide, 28.14wt%, 43.36wt% and 25.24wt% of zinc object phase total amount are accounted for respectively.Sample
Gangue mineral in product is mainly calcite and dolomite, separately there is a small amount of quartz, feldspar, barite, mica and apatite etc..It is former
Mineral composition and content in mine are shown in Table 1 to 3.
Table 1
| It is separate | Lead sulfate | Ceruse | Vulcanized lead | Limonite | Total lead |
| Lead content/wt% | 0.026 | 3.88 | 0.81 | 0.52 | 5.236 |
| Lead occupation rate/% | 0.5 | 74.1 | 15.47 | 9.93 | 100 |
Table 2
| It is separate | Zinc carbonate | Zinc silicate | Zinc sulphide | Limonite | Total zinc |
| Zn content/wt% | 3.2 | 4.93 | 2.87 | 0.37 | 11.37 |
| Zinc occupation rate/% | 28.14 | 43.36 | 25.24 | 3.25 | 100 |
Table 3
Embodiment 1
Low-grade lead-zinc, active carbon and cerussite are subjected to ingredient according to weight ratio 100:5:3 and are uniformly mixed,
Its middle-low grade lead-zinc includes 4.95wt%S, 5.28wt%P, 11.4wt%Zn, 14.50wt%Fe, 13.14wt%
Ca, 3.60wt%Mg, 0.17wt%Na, 0.14wt%K, 0.42wt%Al, 0.0045wt%Ge；Activated carbon purity is
97wt%, lead content 71.11wt% in cerussite.ZnS and PbCO in reaction raw materials3Molar ratio be 1:0.91.
Raw material is put into ball milling 2h in ball mill, drum's speed of rotation 350rpm mixes well raw material.After ball milling
Raw material is pressed into the cylindric block of Φ 1.8cm × 0.5cm with pressure-like machine under 230Mpa pressure.
Block is put into vacuum reduction smelting device (vacuum drying oven), is heated to 1200 DEG C with the heating rate of 5 DEG C/min,
1h is kept the temperature, room temperature is then down to the rate of temperature fall of 5 DEG C/min, during which the pressure in vacuum reduction smelting device (vacuum drying oven) is protected
It holds in 100Pa.
In experimentation, it is anti-that with the lead oxide in raw material redox can occur for the zinc sulphide in low-grade lead-zinc
Vulcanized lead and zinc oxide should be generated, the zinc silicate and zinc oxide in raw material further with the anti-former volatiling reaction of surviving of coal dust, zinc steam
Gas is collected by condensing unit.After separating treatment, the volatility of Zn-ef ficiency and lead element in raw ore is respectively
99.5% and 5.3%, a small amount of lead and germanium are contained in obtained metallic zinc, wherein Zn-ef ficiency content is 93.4wt%, zinc in kiln slag
Element and lead element content are respectively 0.22wt% and 7.38wt%.The higher metallic zinc of obtained purity and kiln slag can be into one
Step is for producing metallic zinc and metallic lead.
Embodiment 2
Low-grade lead-zinc, coal dust and cerussite are subjected to ingredient according to weight ratio 100:10:5 and are uniformly mixed,
Its middle-low grade lead-zinc includes 4.95wt%S, 5.28wt%P, 11.4wt%Zn, 14.50wt%Fe, 13.14wt%
Ca, 3.60wt%Mg, 0.17wt%Na, 0.14wt%K, 0.42wt%Al, 0.0045wt%Ge；Activated carbon purity is
97wt%, lead content 71.11wt% in cerussite.ZnS and PbCO in reaction raw materials3Molar ratio be 1:1.15.
Raw material is put into ball milling 5h in ball mill, drum's speed of rotation 600rpm mixes well raw material.After ball milling
Raw material is pressed into the cylindric block of Φ 1.8cm × 0.5cm with pressure-like machine under 230Mpa pressure.
Block is put into vacuum reduction smelting device (vacuum drying oven), is heated to 1200 DEG C with the heating rate of 5 DEG C/min,
1h is kept the temperature, room temperature is then down to the rate of temperature fall of 5 DEG C/min, during which the pressure in vacuum reduction smelting device (vacuum drying oven) is protected
It holds in 50Pa.
In experimentation, it is anti-that with the lead oxide in raw material redox can occur for the zinc sulphide in low-grade lead-zinc
Vulcanized lead and zinc oxide should be generated, the zinc silicate and zinc oxide in raw material further with the anti-former volatiling reaction of surviving of coal dust, zinc steam
Gas is collected by condensing unit.After separating treatment, the volatility of Zn-ef ficiency and lead element in raw ore is respectively
99.8% and 5.6%, a small amount of lead and germanium are contained in obtained metallic zinc, wherein Zn-ef ficiency content is 92.7wt%, zinc in kiln slag
Element and lead element content are respectively 0.12wt% and 7.78wt%.The higher metallic zinc of obtained purity and kiln slag can be into one
Step is for producing metallic zinc and metallic lead.
Embodiment 3
With the difference of embodiment 1 are as follows: the molar ratio of zinc sulphide and ceruse is 1:2 in reaction raw materials.
After reduction volatilization, the volatility of zinc and lead in raw ore is respectively 99.7% and 7.4%, obtained metallic zinc
Middle Zn-ef ficiency content is 92.9wt%, and Zn-ef ficiency and lead element content are respectively 0.08wt% and 8.12wt% in kiln slag.
Embodiment 4
With the difference of embodiment 1 are as follows: the molar ratio of zinc sulphide and ceruse is 1:0.5 in reaction raw materials.
After reduction, the volatility of Zn-ef ficiency and lead element in raw ore is respectively 90.03% and 6.7%, is obtained
Zn content is 93.5wt% in metallic zinc, and Zn-ef ficiency and lead element content are respectively 0.56wt% and 9.1wt% in kiln slag.
Embodiment 5
With the difference of embodiment 1 are as follows: the process of temperature programming includes: with the rate of 20 DEG C/min, by the anti-of reducing and smelting
System is answered to be warming up to the reducing and smelting temperature；The reaction system of reducing and smelting is subjected to constant temperature, constant temperature in reducing and smelting temperature
The time of process is 1h；With the rate of 10 DEG C/min, the reaction system of reducing and smelting is down to room temperature.
After reduction, the volatility of Zn-ef ficiency and lead element in raw ore is respectively 99.1% and 6.2%, obtained gold
Belonging to Zn-ef ficiency content in zinc is 92.0wt%, and Zn-ef ficiency and lead element content are respectively 0.31wt% and 7.89wt% in kiln slag.
Embodiment 6
With the difference of embodiment 1 are as follows: reducing and smelting process does not use Temperature Programmed Processes, but is directly heated.
After reduction, the volatility of Zn-ef ficiency and lead element in raw ore is respectively 98.3% and 6.4%, obtained gold
Belonging to Zn-ef ficiency content in zinc is 90.7wt%, and Zn-ef ficiency and lead element content are respectively 0.38wt% and 8.02wt% in kiln slag.
Embodiment 7
With the difference of embodiment 1 are as follows: the temperature of reducing and smelting process is 1000 DEG C, reaction time 1h.
After reduction, the volatility of Zn-ef ficiency and lead element in raw ore is respectively 93.88% and 5.0%, is obtained
Zn-ef ficiency content is 91.74wt% in metallic zinc, in kiln slag Zn-ef ficiency and lead element content be respectively 0.36wt% and
8.20wt%.
Comparative example 1
With the difference of embodiment 1 are as follows: be added without cerussite and carry out reduction volatilization using rotary kiln.
After rotary kiln reduction volatilization, the volatility of Zn-ef ficiency and lead element in raw ore is respectively 60% and 2.1%,
Zn content is 39wt% in obtained zinc oxide fumes, in kiln slag Zn-ef ficiency and lead element content be respectively 8.20wt% and
3.11wt%.
It can be seen from the above description that the above embodiments of the present invention realized the following chievements:
Comparing embodiment 1 and comparative example 1 using method provided by the present application it is found that be conducive to improve low-grade lead oxide zinc
The separation rate and the rate of recovery of Zn-ef ficiency and lead element in mine.
Comparing embodiment 1 to 4 is it is found that the molar ratio of zinc sulphide in reaction raw materials and ceruse is limited to the application is preferred
In the range of be conducive to improve the separation rate and the rate of recovery of Zn-ef ficiency and lead element in low-grade lead-zinc.
Comparing embodiment 1,5,6 is it is found that excellent by the application is limited to using the parameter of temperature programming and Temperature Programmed Processes
Be conducive to improve the separation rate and the rate of recovery of Zn-ef ficiency and lead element in low-grade lead-zinc in the range of choosing.
Comparing embodiment 1 and 7 is it is found that the temperature and time of reducing and smelting is limited in the preferred range of the application favorably
In the separation rate and the rate of recovery that improve Zn-ef ficiency and lead element in low-grade lead-zinc.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. the extracting method of Zn-ef ficiency in a kind of low-grade lead zinc ore, which is characterized in that device used in the extracting method
Including vacuum reduction smelting device, the total content of lead element and Zn-ef ficiency in the low-grade lead zinc ore is lower than 20wt%, and
The Zn-ef ficiency and the lead element exist in the form of zinc silicate, zinc carbonate, zinc sulphide, ceruse and vulcanized lead symbiosis, institute
Stating extracting method includes:
In the vacuum reduction smelting device, the low-grade lead zinc ore, reproducibility fuel and cerussite are subjected to reduction smelting
Refining obtains metallic zinc and containing lead skim.
2. extracting method according to claim 1, which is characterized in that before carrying out the reducing and smelting, the extraction
Method further include:
The mixture of the low-grade lead zinc ore, the reproducibility fuel and the cerussite is successively ground, at compacting
Reason, obtains blank；The blank is subjected to the reducing and smelting reaction, obtains the metallic zinc and described containing lead skim；
Preferably, the process of lapping includes the steps that grinding the mixture using ball mill, the more preferable ball
The revolving speed of grinding machine is 100~600rpm, and milling time is 2~10h.
3. extracting method according to claim 2, which is characterized in that the pressing process includes with 150~250Mpa's
The step of pressure suppresses the mixture.
4. extracting method according to claim 1 or 2, which is characterized in that device used in the extracting method also wraps
Cooling device is included, after carrying out the reducing and smelting, the extracting method further include: gone back using the cooling device to described
Original is smelted the gaseous products generated in reaction and is cooled down, and the metallic zinc is obtained；
Preferably, device used in the extracting method further includes waste-heat recovery device, and the waste-heat recovery device setting exists
On flow path between the vacuum reduction smelting device and the cooling device, the extracting method further include: using described remaining
Heat recovery apparatus carries out waste heat recycling to the gaseous products generated in reducing and smelting reaction, then uses the cooling device
The cooling procedure is carried out to by the gaseous products of the waste heat recycling step, obtains the metallic zinc.
5. extracting method according to any one of claim 1 to 3, which is characterized in that the reducing and smelting process it is true
Reciprocal of duty cycle is 1~200Pa, and reaction temperature is 900~1200 DEG C, and the reaction time is 0.5~2h；
Preferably, the vacuum degree of the reducing and smelting process is 1~100Pa, and the reaction temperature is 1100~1200 DEG C, described
Reaction time is 1~2h.
6. extracting method according to claim 5, which is characterized in that the reducing and smelting process is Temperature Programmed Processes,
Described program heating process include:
With the rate of 5~15 DEG C/min, the reaction system that the reducing and smelting reacts is warming up to reducing and smelting temperature；
The reaction system is kept the temperature in the reducing and smelting temperature, the time of the insulating process is 0.5~2h；
With the rate of 5~15 DEG C/min, the reaction system is down to room temperature.
7. extracting method according to any one of claim 1 to 3, which is characterized in that the low-grade lead zinc ore, described
The molar ratio of zinc sulphide and ceruse is 1:0.5~2 in the mixture of reproducibility fuel and the cerussite；
Preferably, zinc sulphide and carbonic acid in the mixture of the low-grade lead zinc ore, the reproducibility fuel and the cerussite
The molar ratio of lead is 1:0.8~1.2.
8. extracting method according to any one of claim 1 to 3, which is characterized in that the reproducibility fuel is selected from wood
One or more of charcoal, active carbon, graphite, petroleum coke, coal and group of carbon black composition.
9. extracting method according to claim 1, which is characterized in that the zinc of 90wt% or more in the low-grade lead zinc ore
Element exists in the form of zinc silicate, zinc carbonate or zinc sulphide, and the lead element of 90wt% or more is with ceruse and/or vulcanized lead
Form exists.
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| CN111270085A (en) * | 2020-04-08 | 2020-06-12 | 中国恩菲工程技术有限公司 | Smelting system and smelting method for low-grade lead-zinc oxide ore |
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