CN106702165B - A method of leaching niobium scandium from tailing - Google Patents
A method of leaching niobium scandium from tailing Download PDFInfo
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- CN106702165B CN106702165B CN201710030923.5A CN201710030923A CN106702165B CN 106702165 B CN106702165 B CN 106702165B CN 201710030923 A CN201710030923 A CN 201710030923A CN 106702165 B CN106702165 B CN 106702165B
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- tailing
- scandium
- niobium
- magnetic separation
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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
- 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
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- 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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
-
- 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
- C22B59/00—Obtaining rare earth metals
-
- 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
Abstract
The present invention discloses a kind of method that niobium scandium is leached from tailing, is related to technical field of wet metallurgy.It includes the following steps：S1, calcium hydroxide and coal dust are added in the tailing for selecting iron, rare earth and fluorite, obtain mixture, obtain roasted ore after mixture is roasted；S2, ball-milling treatment is carried out to roasted ore, and by low intensity magnetic separation, obtain weak magnetic separation iron concentrate and low intensity magnetic separation tailing；S3, low intensity magnetic separation tailing is mixed with the concentrated sulfuric acid, leaching obtains sulfuric acid leaching object, after filtration washing, obtains leachate and the leached mud containing niobium and scandium.Method of the invention is easy to operate, and low energy consumption, has good environmental benefit, and process costs are low, can effectively leach and select iron, rare earth and niobium, scandium in fluorite tailing, and niobium, scandium leaching rate are high, moreover it is possible to recycle the iron of high-grade, high yield.
Description
Technical field
The method that the present invention relates to a kind of to leach niobium scandium from tailing, is related to technical field of wet metallurgy.
Background technique
Due in the tailing that baiyuneboite selects iron, rare earth and fluorite, niobium, scandium content be respectively 0.36% and
0.03%, reach 3 times of raw ore or more, niobium, scandium are effectively enriched with, and therefore, baiyuneboite selects the tail of iron, rare earth and fluorite
Mine is to extract the high-quality mineral resources of niobium, scandium element.In addition, during high intensity magnetic separation iron, ratio of the iron not recycled in tailing
Example about 15.74%, the form that is primarily present is silicate.The valuable metals such as niobium, scandium and the iron in tailing have been made full use of, for
Realize that the comprehensive utilization of Bayan Obo mineral products resource is of great significance.
Currently, niobium, scandium are tentatively enriched with by selecting iron, rare earth and fluorite, then pass through the method for flotation by dressing plant of Baogang
Obtaining grade is 4%, the niobium concentrate that yield is 30% or so.On this basis, scandium concentrate is obtained using high intensity magnetic separation process.In height
It presses and uses concentrated sulfuric acid pressure leaching niobium and scandium in reaction kettle.This method can make niobium leaching rate reach 65%, and scandium leaching rate reaches 90%
More than.
The advantages of above-mentioned recovery method is to carry out wet-leaching using niobium, scandium concentrate, and impurity content is relatively in leachate
It is few, the removal of impurities workload in subsequent extraction process can be reduced.The disadvantage is that the rate of recovery of niobium, scandium physical separation is too low, it is very one big
Niobium, scandium mineral is divided to be stranded in tailing, it is relatively fewer into the mineral quantity for leaching process, and then can be to the final recycling of niobium, scandium
Rate has an impact, and pressure leaching is higher to equipment intensity requirement, increases process costs to a certain extent.
In addition, can effectively leach niobium, scandium mineral there are also many methods.For example, the method that sulfuric acid low temperature decomposes niobium mineral,
It is only used for labile niobium mineral, and acid consumption is larger；The method that hydrogen fluoride decomposes niobium mineral, can generate toxic gas
HF；The method that chloridising decomposes niobium mineral, heavier to equipment corrosion and environmental pollution, operating environment is poor；Sodium hydroxide solution
The method of scandium is leached, so that filter process is separated by solid-liquid separation difficulty, it is at high cost；The method that concentrated hydrochloric acid soaks scandium, the reaction time is long, leaches
Rate is lower.
In conclusion urgent need provides, one kind is easy to operate, and low energy consumption, has good environmental benefit, process costs are low, can
It effectively leaches and selects iron, rare earth and niobium, scandium in fluorite tailing, niobium, scandium leaching rate are high, moreover it is possible to recycle high-grade, high yield iron
The method of niobium scandium is leached from tailing.
Summary of the invention
(1) technical problems to be solved
In order to solve the above problem of the prior art, the present invention provides a kind of method that niobium scandium is leached from tailing, the party
Method is easy to operate, and low energy consumption, has good environmental benefit, process costs are low, can effectively leach and select iron, rare earth and fluorite tailing
In niobium, scandium, niobium, scandium leaching rate are high, moreover it is possible to recycle the iron of high-grade, high yield.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include：
A method of it leaching niobium scandium from tailing, includes the following steps：
S1, calcium hydroxide and coal dust are added in the tailing for selecting iron, rare earth and fluorite, obtain mixture, mixture is roasted
Roasted ore is obtained after burning；
S2, ball-milling treatment is carried out to the roasted ore in step S1, and by low intensity magnetic separation, obtain weak magnetic separation iron concentrate and weak magnetic
Select tailing；
S3, the low intensity magnetic separation tailing in step S2 is mixed with the concentrated sulfuric acid, leaching obtains sulfuric acid leaching object, through filtering
After washing, leachate and the leached mud containing niobium and scandium are obtained.
A kind of improvement of the method for niobium scandium is leached from tailing as the present invention, the weight of the calcium hydroxide in the S1 is
The 18%-90% of tailing weight, the weight of coal dust are the 3%-8% of tailing weight；
Preferably, the weight of the calcium hydroxide in the S1 is the 20% of tailing weight, and the weight of coal dust is tailing weight
5%.
A kind of improvement of the method for niobium scandium is leached from tailing as the present invention, the maturing temperature in the S1 is 1000
DEG C -1400 DEG C, calcining time 90min-150min；
Preferably, the maturing temperature in the S1 is 1200 DEG C, calcining time 120min.
A kind of improvement of the method for niobium scandium is leached from tailing as the present invention, the mixture in the S1 uses graphite earthenware
Crucible is held；
Or,
Mixture in the S1 is held using corundum crucible, and is passed through isolation air when using corundum crucible roasting
Protective gas.
A kind of improvement for leaching the method for niobium scandium from tailing as the present invention roasts after ball-milling treatment in the S2
Mine amount of the grinding particle size less than or equal to 75 μm is not less than the 95% of total mine amount in mine.
A kind of improvement of the method for niobium scandium is leached from tailing as the present invention, the magnetic field that the low intensity magnetic separation in the S2 uses
Intensity is 200mT-300mT；
Preferably, the magnetic field strength that the low intensity magnetic separation in the S2 uses is 270mT.
A kind of improvement of the method for niobium scandium, the mass fraction of the concentrated sulfuric acid in the S3 are leached from tailing as the present invention
It is 98% or 93%.
A kind of improvement of the method for niobium scandium is leached from tailing as the present invention, the concentrated sulfuric acid in the S3 and low intensity magnetic separation tail
The mass ratio of mine is 7.36:1-14.72:1；
Preferably, the mass ratio of the concentrated sulfuric acid in the S3 and low intensity magnetic separation tailing is 11.04:1.
A kind of improvement of the method for niobium scandium is leached from tailing as the present invention, the extraction temperature in the S3 be 245 DEG C-
300 DEG C, extraction time 50min-90min；
Preferably, the extraction temperature in the S3 is 270 DEG C, extraction time 60min.
(3) beneficial effect
The beneficial effects of the invention are as follows：
Contain fixed carbon in coal dust of the invention, can be used as reducing agent, the iron compound at high temperature containing tailing is (such as
Di-iron trioxide, ferrosilite, ferroso-ferric oxide etc.) in ferric ion be reduced to metallic iron, later pass through ball milling and weak magnetic
Ferro element in choosing separation and recovery tailing, while the mineral treating capacity of subsequent extract technology is reduced, it reduces miscellaneous in niobium, scandium pickle liquor
The amount of matter.Calcium hydroxide plays activation and decomposition, and it is easy that calcium hydroxide can react generation with niobium mineral in a heated condition
In by the compound of Ore Leaching, and calcium hydroxide reacts with scandium contained mineral, damages to the structure of mineral, is conducive to acid
Leaching to scandium, to improve the leaching rate of niobium in tailing, scandium.
Compared with prior art, method of the invention is easy to operate, and low energy consumption, have good environmental benefit, technique at
This is low, can effectively leach and select iron, select rare earth and select niobium, the scandium in fluorite tailing, and niobium, scandium leaching rate are high, and (niobium, scandium leaching rate are not
Lower than 90%), moreover it is possible to recycle the iron of high-grade (90% or more), high yield (85% or more).
Detailed description of the invention
Fig. 1 is a kind of flow diagram of method that niobium scandium is leached from tailing of the invention.
Specific embodiment
In order to preferably explain the present invention, in order to understand, with reference to the accompanying drawing, by specific embodiment, to this hair
It is bright to be described in detail.
Embodiment 1
As shown in Figure 1, embodiment 1 provides a kind of method for leaching niobium scandium from tailing, wherein raw material is selected from white clouds Hubei Province
Bo Kuang selects the tailing of iron, rare earth and fluorite, wherein mainly containing the mineral of valuable metal, including the not recoverable iron ore of high intensity magnetic separation
The niobium of object and high intensity magnetic separation and floatation process preliminary concentration, scandium mineral.Wherein, the iron in tailing, niobium, scandium content respectively such as
Under：W (TFe)=15.74%, w (Nb2O5)=0.36%, w (Sc2O3)=0.03%.
S1, above-mentioned tailing 100g is taken, (wherein, fixed carbon content is 20g calcium hydroxide and 5g coal dust is added
83.66%) it, is mixed, obtains mixture, mixture is roasted into 120min at 1200 DEG C, obtains roasted ore.
S2, ball-milling treatment is carried out to roasted ore by ball-grinding machine, and guarantees after ball-milling treatment grinding particle size in roasted ore
Mine amount less than or equal to 75 μm is not less than the 95% of total mine amount, and the low intensity magnetic separation in the case where magnetic field strength is the magnetic field of 270mT, can obtain later
Obtaining grade is 91.92%, the Iron concentrate and low intensity magnetic separation tailing that yield is 88.39%.
S3, low intensity magnetic separation tailing in 20g step S2 is taken, compares the concentrated sulfuric acid according to quality：Low intensity magnetic separation tailing=7.36:1 is added
The concentrated sulfuric acid that mass fraction is 98%, mineral aggregate is stirred evenly, leaches 60min at 245 DEG C, obtains sulfuric acid leaching object, later
It is filtered with funnel, leached mud and leachate is separated, and wash slag repeatedly with clear water, to ensure leached ion energy
It can smoothly enter into leachate.
Embodiment 1 is using inductive coupling plasma emission spectrograph (abbreviation ICP spectrometer) to obtained in step S3
Leached mud and leachate carry out elemental analysis, and the leaching rate by can be calculated niobium, scandium is respectively 95.96%, 95.72%.
The step of with embodiment 1, is similar, embodiment 2-9 be by adjusting the maturing temperature and calcining time in step S1,
The weight of calcium hydroxide, the weight of coal dust, the magnetic field strength in step S2, the mass fraction of the concentrated sulfuric acid in step S3, dense sulphur
Acid and the mass ratio of low intensity magnetic separation tailing, the Parameter Conditions such as extraction temperature and extraction time are realized.The technique item of embodiment 2-9
The leaching rate situation of part, grade, yield and the niobium, scandium that obtain iron is specifically as shown in table 1.
Table 1：The leaching rate situation of grade, yield and the niobium of the process conditions of embodiment 2-9 and iron, scandium.
In above-mentioned each embodiment, calcium hydroxide plays activation and decomposition, and calcium hydroxide is in a heated condition
Generation can be reacted with niobium mineral to be easy to by the compound of Ore Leaching.Calcium hydroxide reacts with scandium contained mineral, to the knot of mineral
It is configured to destroy, is conducive to leaching of the acid to scandium.(weight of calcium hydroxide is the 18%- of tailing weight to the weight of calcium hydroxide
It 90%) is determined according to the leaching rate of niobium, scandium.Guarantee niobium, scandium leaching rate 90% or more under the premise of, in order to
Process costs are reduced as far as possible, and the weight of calcium hydroxide is selected in line with the principle of few additive, and the weight of calcium hydroxide is preferred
It is the 20% of tailing weight.
Due to containing fixed carbon in coal dust, reducing agent can be used as, iron compound (such as three oxygen at high temperature containing tailing
Change two iron, ferrosilite, ferroso-ferric oxide etc.) in ferric ion be reduced to ferrous metal, and then realize the recycling of iron in tailing.
The weight (3%-8% that the weight of coal dust is tailing weight) of coal dust is determined according to the leaching rate of niobium, scandium.Guaranteeing
Niobium, scandium leaching rate under the premise of 90% or more, in order to reduce process costs as far as possible, the weight of coal dust is in line with low addition
The principle of amount selects, and the weight of coal dust is preferably the 5% of tailing weight.
The determination method of above-mentioned each maturing temperature is to select minal (without other gangues, pure niobium mineral), is added
Calcium hydroxide does differential thermal analysis to mixture after mixing, primarily determines the temperature that minal and calcium hydroxide react,
Then it is tested near this temperature, that is, can determine the temperature range that tailing and calcium hydroxide of the invention react.Contain
The determination of scandium mineral reaction temperature is also to be selected scandium contained mineral using above-mentioned similar approach and be uniformly mixed with calcium hydroxide, it
Differential thermal analysis is done to mixture afterwards, primarily determines the probable ranges for the temperature that scandium contained mineral and calcium hydroxide react, then
By testing the temperature range for further determining that tailing and calcium hydroxide of the invention react.In summary experimental result,
Finally available maturing temperature range is 1000 DEG C -1400 DEG C.In the leaching rate for guaranteeing niobium, scandium, as far as possible reduction process costs
In the case where, lower 1200 DEG C of maturing temperature preferable temperature.
The range 90min-150min of calcining time can be determined according to the leaching rate of final niobium, scandium.Guaranteeing niobium, scandium
Leaching rate, as far as possible in the case where reduction process costs, the shorter 120min of the preferred duration of calcining time.
In order to avoid reduction gained metallic iron is oxidized, implementation process holds reaction mass using graphite crucible.Specifically,
Since graphite can generate carbon monoxide with air, there is protective effect, therefore, graphite crucible can manufacture reducing atmosphere, avoid also
The ferrous metal obtained after original is iron oxide by the dioxygen oxidation in air.It is, of course, also possible to hold reaction using corundum crucible
Material, but the protective gas for needing to be passed through isolation air when corundum crucible roasting is used, it is same to can avoid such as nitrogen or argon gas
Metallic iron is oxidized by oxygen as iron oxide.
The purpose of ball-milling treatment is conducive to niobium, scandium by Ore Leaching, and leaching velocity is fast and leaches thorough.Ball milling particle size range is
It is determined according to the grade of the iron of concentrate obtained by magnetic separation and yield.In order to guarantee the leaching rate of high niobium, scandium, roasted after ball-milling treatment
The 95% of total mine amount should be not less than by burning mine amount of the grinding particle size less than or equal to 75 μm in mine.But above-mentioned ball milling granularity cannot
It is too small, in this way, magnetic relatively weak；Ball milling granularity can not be excessive, in this way, iron is with other impurity, solution is not left, when magnetic separation
Impurity can be brought into concentrate together with iron, to influence the grade and yield of iron.
Due to metallic iron be it is ferromagnetic, tapping can be separated and recovered in the mineral roasted by low intensity magnetic separation.Pass through magnetic
Choosing can not only reduce the mineral treating capacity of subsequent extract technology, but can reduce impurity in niobium, scandium pickle liquor amount (this is because
Iron is also dissolved in acid).The size of magnetic field strength is determined according to the yield of the grade of magnetic concentrate and iron.Magnetic field mistake
Greatly, impurity is taken away together, to reduce the grade of concentrate；If magnetic field is too small, then the yield of iron is reduced.Therefore, it is
Guarantee that the grade of concentrate and the yield of iron, the magnetic field strength range that low intensity magnetic separation uses select 200mT-300mT.In order to guarantee essence
The grade of mine and the yield of iron, as far as possible in the case where reduction process costs, the preferred 270mT of the magnetic field strength of low intensity magnetic separation.
The concentrated sulfuric acid that above-mentioned mass fraction is 98% is that scientific research institution laboratory generally uses, and mass fraction is 93%
The concentrated sulfuric acid is generally used in industrial enterprise.(mass ratio of the concentrated sulfuric acid and low intensity magnetic separation tailing is 7.36 to the quality of the concentrated sulfuric acid:1-
14.72:1), extraction temperature (245 DEG C -300 DEG C) and extraction time (50min-90min) are according to the leaching rate of niobium, scandium come really
Fixed.Guarantee niobium, scandium leaching rate 90% or more under the premise of, in order to reduce process costs as far as possible, the concentrated sulfuric acid
Quality, extraction temperature and extraction time are selected in line with few additive, low temperature and the principle of short time respectively.The concentrated sulfuric acid and weak magnetic
Select the mass ratio preferably 11.04 of tailing:1, preferably 270 DEG C of extraction temperature, the preferred 60min of extraction time.
In conclusion method of the invention is easy to operate, low energy consumption, has good environmental benefit, process costs are low, can
It effectively leaching and selects iron, rare earth and niobium, scandium in fluorite tailing, niobium, scandium leaching rate are high (niobium, scandium leaching rate are not less than 90%),
The iron of high-grade (90% or more), high yield (85% or more) can also be recycled.
The technical principle that detailed description of the preferred embodimentsthe present invention has been described is combined above.These descriptions are intended merely to explain the present invention
Principle, and shall not be construed in any way as a limitation of the scope of protection of the invention.Based on the explanation herein, art technology
Personnel, which do not need to make the creative labor, can associate other specific embodiments of the invention, these modes fall within this
Within the protection scope of invention.
Claims (7)
1. a kind of method for leaching niobium scandium from tailing, which is characterized in that include the following steps：
S1, calcium hydroxide and coal dust are added in the tailing for selecting iron, rare earth and fluorite, mixture is obtained, after mixture is roasted
Obtain roasted ore；
S2, ball-milling treatment is carried out to the roasted ore in step S1, and by low intensity magnetic separation, obtain weak magnetic separation iron concentrate and low intensity magnetic separation tail
Mine；
S3, the low intensity magnetic separation tailing in step S2 is mixed with the concentrated sulfuric acid, leaching obtains sulfuric acid leaching object, through filtration washing
Afterwards, leachate and leached mud containing niobium and scandium are obtained；
The weight of calcium hydroxide in the S1 is the 18%-20% of tailing weight, and the weight of coal dust is the 4%- of tailing weight
8%；
In the S2, mine amount of the grinding particle size less than or equal to 75 μm is not less than total mine amount in roasted ore after ball-milling treatment
95%；
The magnetic field strength that low intensity magnetic separation in the S2 uses is 200mT-300mT；
Maturing temperature in the S1 is 1000 DEG C -1400 DEG C, calcining time 90min-150min；
The mass fraction of the concentrated sulfuric acid in the S3 is 98% or 93%, the quality of the concentrated sulfuric acid and low intensity magnetic separation tailing in the S3
Than being 7.36:1-14.72:1；
Extraction temperature in the S3 is 255 DEG C -300 DEG C, extraction time 55min-90min.
2. the method for niobium scandium is leached from tailing as described in claim 1, it is characterised in that：Calcium hydroxide in the S1
Weight is the 20% of tailing weight, and the weight of coal dust is the 5% of tailing weight.
3. the method for niobium scandium is leached from tailing as described in claim 1, it is characterised in that：Maturing temperature in the S1 is
1200 DEG C, calcining time 120min.
4. the method for niobium scandium is leached from tailing as described in claim 1, it is characterised in that：Mixture in the S1 uses
Graphite crucible is held；
Or,
Mixture in the S1 is held using corundum crucible, and the guarantor of isolation air is passed through when using corundum crucible roasting
Protect gas.
5. the method for niobium scandium is leached from tailing as described in claim 1, it is characterised in that：Low intensity magnetic separation in the S2 uses
Magnetic field strength be 270mT.
6. the method for niobium scandium is leached from tailing as described in claim 1, it is characterised in that：The concentrated sulfuric acid in the S3 with it is weak
The mass ratio of magnetic tailing is 11.04:1.
7. the method for niobium scandium is leached from tailing as described in claim 1, it is characterised in that：Extraction temperature in the S3 is
270 DEG C, extraction time 60min.
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| CN111363912B (en) * | 2020-04-17 | 2022-02-18 | 包头稀土研究院 | Method for treating rare earth tailings |
| CN111482264B (en) * | 2020-04-17 | 2021-12-28 | 包头稀土研究院 | Method for treating medium lean oxidized ore |
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| CN102168173A (en) * | 2011-03-29 | 2011-08-31 | 内蒙古科技大学 | Method for extracting niobium from tailings |
| CN102653820A (en) * | 2012-04-24 | 2012-09-05 | 包头稀土研究院 | Method for extracting scandium from baiyuneboite tailings |
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| CN103361495A (en) * | 2013-07-17 | 2013-10-23 | 内蒙古科技大学 | Method for extracting niobium from Bayan Obo mine tailing |
| CN105568003A (en) * | 2015-12-31 | 2016-05-11 | 包头稀土研究院 | Method for enriching niobium from Bayan obo tailings |
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2017
- 2017-01-17 CN CN201710030923.5A patent/CN106702165B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102168173A (en) * | 2011-03-29 | 2011-08-31 | 内蒙古科技大学 | Method for extracting niobium from tailings |
| CN102653820A (en) * | 2012-04-24 | 2012-09-05 | 包头稀土研究院 | Method for extracting scandium from baiyuneboite tailings |
| CN102925668A (en) * | 2012-11-20 | 2013-02-13 | 湖南稀土金属材料研究院 | Method for leaching out scandium from niobium tailing dressing |
| CN103352118A (en) * | 2013-07-17 | 2013-10-16 | 内蒙古科技大学 | Method for extracting Nb from bayan obo tailings |
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| CN105568003A (en) * | 2015-12-31 | 2016-05-11 | 包头稀土研究院 | Method for enriching niobium from Bayan obo tailings |
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