CN109136538A - The processing method of rare earth ore concentrate - Google Patents
The processing method of rare earth ore concentrate Download PDFInfo
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- CN109136538A CN109136538A CN201810960213.7A CN201810960213A CN109136538A CN 109136538 A CN109136538 A CN 109136538A CN 201810960213 A CN201810960213 A CN 201810960213A CN 109136538 A CN109136538 A CN 109136538A
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- Prior art keywords
- rare earth
- ore concentrate
- earth ore
- magnesium
- chloride
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/08—Chloridising roasting
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- 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 invention discloses a kind of processing method of rare earth ore concentrate, includes the following steps: that (1) mixes the chloride of magnesium with rare earth ore concentrate, then roasted under air conditions, to form product of roasting；Wherein, the weight ratio of the chloride of magnesium and rare earth ore concentrate is 0.5~1.9:1, the MgCl in the chloride of magnesium2Weight ratio with rare earth ore concentrate is 0.23~0.9:1, and maturing temperature is 460~580 DEG C, and calcining time is 30~200 minutes；(2) product of roasting after cooling is directlyed adopt acid solution to leach, rare earth metal leaching rate is 95% or more.The present invention can realize higher leaching rate with lower temperature, and can form molten mass to avoid product of roasting.
Description
Technical field
The present invention relates to a kind of processing method of rare earth ore concentrate, especially a kind of side of magnesium chloride Roasting Decomposition rare earth ore concentrate
Method.
Background technique
The rare earth resources in Inner Mongol packet header are richly endowed by nature, account for the 81% of national rare earth reserves.Baotou rare earth ore concentrate accounts for China
Smelt 60% or more of rare earth ore concentrate.The technique that mischmetal is extracted from rare earth ore concentrate mainly includes that concentrated sulfuric acid roasting decomposes work
Skill.The baking tail gases of the technique contain the sour gas such as a large amount of sulphur and fluorine, are handled using the method that water spray absorbs, but discharge tail
Gas is difficult to reach national relevant emission standards.Due to the mixed acid that spray liquid is sulfuric acid, fluosilicic acid and hydrofluoric acid, still it is difficult to recycle
It utilizes, lime neutralisation treatment can only be used, it is big not only to neutralize the quantity of slag, and be easy to cause secondary pollution.The thorium element set of the technique
In leached mud, the quantity of slag is big, accounts for 50% or more of rare earth ore concentrate amount, and radioactive intensity is more than national low-activity slag standard,
It saves extremely difficult with processing.
The disclosure that rare earth ore concentrate extracts mischmetal further includes liquid alkaline decomposition technique.The technique concentration is 50~70%
Liquid alkaline solution decomposes rare earth ore concentrate, and reaction temperature is 140~160 DEG C, then washes the soluble salt of excess base and generation, last salt
Acid dissolution obtains re chloride.Acid waste gas, waste water and emissive industrial waste residue containing ammonia nitrogen are not generated in technical process.At this
In technique, slurry viscosity is big after concentrate is mixed with sodium hydroxide solution, is reacted in a kettle, since decomposition reaction disappears
The boiling point for consuming reaction system after part sodium hydroxide reduces, and reaction system is easy to cause to overheat and " bumping " accident occurs, gives birth to
It is not easy to control to produce operation, operating post has biggish security risk.For example, the China application No. is 201010145840.9 is special
Benefit application discloses a kind of technique of liquid alkali roasting decomposition rare earth ore concentrate, and concentrate and soda lye (concentration > 60%) are mixed
It closes, the Roasting Decomposition at 150~550 DEG C in Industrial Stoves, realizes continuous production.
In general, above-mentioned technique carries out in dense strong acid (concentrated sulfuric acid) or dense highly basic (strong caustic) system,
Equipment seriously corroded, operating condition is poor, and security risk is big.Therefore, it is necessary to develop the rare earth ore concentrate point avoided using strong acid and strong base
Solution technique.Rare earth essence is decomposed with calcium oxide and sodium chloride for example, disclosing application No. is 01128097.2 Chinese patent application
The method of mine, roasting rare earth concentrate at a high temperature of 700 DEG C or more.For another example, CN102653820A discloses a kind of from white clouds Hubei Province
The method of scandium is extracted in rich tailing, comprising the following steps: (1) the activators such as tailing and calcium chloride by weight 1:0.3~1.3
Ratio mixing；The mixture of step (1) is roasted 0.5~4 hour, 700 DEG C~1200 DEG C of maturing temperature；Roast obtained roasting
Mining hot water washing is burnt, roasted ore and water lotion are formed；The activator of recycling is back to use step by water lotion concentration and recovery activator
Suddenly (1)；The mining inorganic acid solution of roasting after washing, obtains solution containing scandium.The above method is mentioned only for single scandium element
It takes.For another example, CN102643992A discloses a kind of recovery method of rare earth waste, method includes the following steps: (1) is to rare earth
Precipitation additive and fluxing agent powder are added in waste material, obtains mixture after mixing, wherein the dosage of precipitation additive is rare earth
20~200wt% of waste material total weight, the dosage of fluxing agent are 1~20wt% of rare earth waste total weight；The rare earth waste
Predominantly rare earth phosphor waste material and/or rare earth aluminic acid waste salt；The precipitation additive is selected from magnesite, shepardite or magnesia
One of or it is a variety of；The fluxing agent is selected from boric acid, lithium metaborate, lithium tetraborate, sodium tetraborate, lithium carbonate, lithium chloride, chlorine
Change one of magnesium, sodium fluoride, magnesium fluoride or aluminum fluoride or a variety of；(2) mixture for obtaining step (1) is 600~1400
DEG C roasting temperature 1~6 hour；(3) to step (2) obtain in product of roasting be added acid solution carry out acid it is molten, be separated by filtration
To mainly containing rare earth element pickle liquor and acid leaching residue；(4) rare earth element and other metallic elements in pickle liquor are separated.On
The maturing temperature for stating method is excessively high, roasted ore hard molten mass easy to form, needs ball mill crushing just so as to cause roasted ore
It can be carried out subsequent leaching operation, otherwise leaching rate caused to reduce.
Summary of the invention
In view of this, it is an object of the present invention to provide a kind of processing method of rare earth ore concentrate, it can be with lower
Temperature realize higher leaching rate, and molten mass can be formed to avoid product of roasting.It is a discovery of the invention that passing through control magnesium
The proportion of chloride and rare earth ore concentrate, and maturing temperature is adjusted, rare earth metal leaching rate can be improved, and can be to avoid roasting
Product forms molten mass, thereby completing the present invention.
The present invention provides a kind of processing method of rare earth ore concentrate, includes the following steps:
(1) chloride of magnesium is mixed with rare earth ore concentrate, is then roasted under air conditions, to form product of roasting；
Wherein, the weight ratio of the chloride of magnesium and rare earth ore concentrate is 0.5~1.9:1, the MgCl in the chloride of magnesium2With rare earth ore concentrate
Weight ratio is 0.23~0.9:1, and maturing temperature is 460~580 DEG C, and calcining time is 30~200 minutes；
(2) by the product of roasting after cooling directly adopt acid solution leach, rare earth metal leaching rate be 95% with
On.
Method in accordance with the invention it is preferred that the chloride of magnesium and the weight ratio of rare earth ore concentrate are 1.0~1.8:1, magnesium
MgCl in chloride2Weight ratio with rare earth ore concentrate is 0.6~0.9:1, and maturing temperature is 500~580 DEG C.
Method in accordance with the invention it is preferred that the chloride of magnesium and the weight ratio of rare earth ore concentrate are 1.5~1.8:1, magnesium
MgCl in chloride2Weight ratio with rare earth ore concentrate is 0.7~0.85:1, and maturing temperature is 560~580 DEG C.
Method in accordance with the invention it is preferred that the chloride of magnesium is magnesium chloride hexahydrate.
Method in accordance with the invention it is preferred that the rare earth ore concentrate is selected from mengite rare-earth concentrate, fluorine carbon cerium mischmetal essence
One of mine, monazite and fluorine carbon cerium mixed rare earth concentrate are a variety of.
Method in accordance with the invention it is preferred that the rare earth ore concentrate is monazite and fluorine carbon cerium mixed rare earth concentrate.
Method in accordance with the invention it is preferred that the content of the rare earth oxide REO in the rare earth ore concentrate be 60~
68wt%.
Method in accordance with the invention it is preferred that the product of roasting after cooling does not carry out pulverization process, directly adopt acid molten
Liquid leaches.
Method in accordance with the invention it is preferred that the acid solution is water-soluble selected from the sulfuric acid that concentration is 0.5~10mol/L
Liquid.
Method in accordance with the invention it is preferred that the product of roasting after cooling is dissolved in the acid solution, from
And form the rare earth metal salt solutions that pH is 4~5.
The present invention carries out decomposition reaction using the chloride and rare earth ore concentrate of properly mixed magnesium at a lower temperature, intermediate
Product chlorinated rare earth, which further decomposes, generates rare earth oxide, can promote the generation of concentrate decomposition reaction.Rare Earth Concentrate Decomposition
Obtained final product is the rare earth oxide for being soluble in acid, can leach rare earth in Low acid reaction condition, leaching rate is higher.
Roasting process does not form molten mass, will not ring formation, product of roasting is powder, good fluidity, it is easy to accomplish continuous production.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, but protection scope of the present invention is not limited to
This.
" being selected from " or " being selected from " used herein refer to independent component selection or two kinds (or more) group of component
It closes.
The processing method of rare earth ore concentrate of the invention includes calcination steps and leaching step, but does not include pulverising step.
Calcination steps of the invention include: to mix the chloride of magnesium with rare earth ore concentrate, are then roasted under air conditions,
To form product of roasting；Wherein, the weight ratio of the chloride of magnesium and rare earth ore concentrate is 0.5~1.9:1, in the chloride of magnesium
MgCl2Weight ratio with rare earth ore concentrate is 0.23~0.9:1, and maturing temperature is 460~580 DEG C, and calcining time is 30~200 points
Clock.
In the present invention, the chloride of magnesium includes but is not limited to MgCl2, MgCl2·6H2O etc..Control magnesium chloride with
The weight ratio of rare earth ore concentrate is very important, it is especially desirable to control MgCl2With the weight ratio of rare earth ore concentrate.The chloride of magnesium with
The weight ratio of rare earth ore concentrate should be 0.5~1.9:1, the MgCl in the chloride of magnesium2Weight ratio with rare earth ore concentrate is 0.23
~0.9:1.When their ratio exceeds above range, lead to the reduction of rare earth metal leaching rate.Especially when the chloride of magnesium
It is greater than 1.9:1, and MgCl with the ratio of the weight ratio of rare earth ore concentrate2When weight ratio with rare earth ore concentrate is 0.23~0.9:1, need
Higher maturing temperature is wanted, so as to cause the formation of molten mass, product of roasting mobility is deteriorated, and is unable to continuous production.At certain
In a little embodiments, the chloride of magnesium and the weight ratio of rare earth ore concentrate are 1.0~1.8:1；Preferably 1.5~1.8:1.Work as the two
Ratio be in above range, rare earth leaching rate is very high, and maturing temperature do not need it is too high.In certain embodiments, magnesium
Chloride in MgCl2Weight ratio with rare earth ore concentrate is 0.6~0.9:1, preferably 0.7~0.85:1.When the ratio of the two
Example be in above range, rare earth leaching rate is very high, and maturing temperature do not need it is too high.
In the present invention, control maturing temperature is also very important.Maturing temperature should be 460~580 DEG C.Roasting temperature
Degree is lower than 460 DEG C, leads to roast insufficient, leaching rate reduction；Maturing temperature is higher than 580 DEG C, results in molten mass, generates knot
Circle, product of roasting mobility are deteriorated.In certain embodiments, maturing temperature is 500~580 DEG C；Preferably 560~580 DEG C.
When maturing temperature is in above range, rare earth leaching rate is very high, and can avoid the formation of molten mass, to be conducive to realize continuous
Metaplasia produces.Calcining time can be 30~200 minutes, preferably 60~150 minutes, more preferably 60~90 minutes.It roasts in this way
It burns sufficiently, and improves production efficiency.
In the present invention, the chloride of magnesium indicates that magnesium reacts the compound to be formed with hydrochloric acid, and specific example includes but not
It is limited to magnesium chloride hexahydrate.The raw ore rock of rare earth after ore dressing to the product of high rare earth grade be known as rare earth ore concentrate.This hair
Bright rare earth ore concentrate can be selected from mengite rare-earth concentrate, fluorine carbon cerium mischmetal concentrate, monazite and fluorine carbon cerium mixed type rare earth essence
One of mine is a variety of.According to embodiment of the present invention, rare earth ore concentrate is monazite and fluorine carbon cerium mixed type rare earth
Concentrate.It is an unexpected discovery of the invention that rare earth metal leaches when rare earth ore concentrate is monazite and fluorine carbon cerium mixed rare earth concentrate
Rate is higher.
Rare earth ore concentrate of the invention mainly includes monazite and bastnaesite two types.
(1) bastnaesite roasts reaction of decomposing at 450 DEG C, specific as follows:
3RE(CO3)2F=RE2O3+REF3+6CO2
3Ce(CO3)F+1/2O2=2CeO2+CeF3+3CO2
Bastnaesite, which decomposes the fluoride generated, to be continued to generate rare earth chloride with magnesium chloride, specific as follows:
2REF3+3MgCl3=2RECl3+3MgF2
2CeF3+3MgCl3=2CeCl3+3MgF2
Monazite is as follows with magnesium chloride:
2REPO4+3MgCl2=2RECl3+Mg3(PO4)2
The rare earth chloride that reaction generates continues to be decomposed to form the rare earth oxide for being soluble in acid, specific as follows
CeCl3+H2O+1/2O2=CeO2+2HCl
2RECl3+3H2O=RE2O3+6HCl
In the present invention, the content of the rare earth oxide REO in the rare earth ore concentrate be 38~68wt%, preferably 50
~68wt%, more preferably 60~68wt%.The content of suitable rare earth oxide REO advantageously reduces maturing temperature, improves
Leaching rate.In certain embodiments, the rare earth ore concentrate be the monazite containing 60~68wt% rare earth oxide REO with
Fluorine carbon cerium mixed rare earth concentrate.It can be further improved leaching rate in this way.
Leaching step of the invention includes: that the product of roasting after cooling is directlyed adopt acid solution to leach, rare earth
Metal leaching rate is 95% or more.Product of roasting temperature is too high, cools down, and can also can control drop with Temperature fall
Temperature.Product of roasting is cooled to room temperature.The product of roasting after so-called " direct " expression cooling is not changed material attribute
Physical or chemical treatment, but do not limit change of the product of roasting spatially or on monnolithic case.According to the present invention one
A embodiment, the product of roasting after cooling do not carry out pulverization process, directly adopt acid solution leaching.The example of pulverization process
Including but not limited to grinding etc..
In the present invention, the acid solution can be selected from aqueous sulfuric acid, aqueous hydrochloric acid solution etc.；Preferably 0.5~
The aqueous sulfuric acid of 10mol/L.The concentration of aqueous sulfuric acid can be 1~8mol/L, preferably 3~5mol/L.It is advantageous in this way
In improvement rare earth metal leaching rate.
In the present invention, the product of roasting after cooling is dissolved in the acid solution, thus formed pH be 4~
5 rare earth metal salt solutions.Pure rare-earth salt solution available in this way.
Embodiment 1
By 100kg monazite and fluorine carbon cerium mixed rare earth concentrates (REO content is 65wt%) and 150kg magnesium chloride hexahydrate
(MgCl2: rare earth ore concentrate=0.70:1) mixing, it is heated to 580 DEG C in Muffle furnace, obtains within insulation reaction 1.0 hours roasting and produces
Object cools to room temperature, with the sulfuric acid leaching of 3mol/L, rare earth leaching rate 98.8%.Product of roasting be it is powdered, roasting process does not have
There are generation melting behaviors.
Embodiment 2
By 100kg monazite and fluorine carbon cerium mixed rare earth concentrate (REO content is 60wt%) and 180kg magnesium chloride hexahydrate
Mix (MgCl2: rare earth ore concentrate=0.84:1), it is heated to 580 DEG C in Muffle furnace, obtains within insulation reaction 1.5 hours roasting and produces
Object cools to room temperature, with the sulfuric acid leaching of 3mol/L, rare earth leaching rate 95.6%.Product of roasting be it is powdered, roasting process does not have
There are generation melting behaviors.
Embodiment 3
100kg fluorine carbon cerium mischmetal concentrate (REO content is 42wt%) is mixed into (MgCl with 50kg magnesium chloride hexahydrate2: rare earth
Concentrate=0.23:1), it is heated to 480 DEG C in Muffle furnace, obtains product of roasting within insulation reaction 1.5 hours, cools to room temperature, uses
The sulfuric acid leaching of 3mol/L, rare earth leaching rate 95.5%.Product of roasting be it is powdered, roasting process does not generate melting behaviors.
Comparative example 1
By 100kg monazite and fluorine carbon cerium mixed rare earth concentrate (REO content is 50wt%) and 200kg magnesium chloride hexahydrate
Mix (MgCl2: rare earth ore concentrate=0.936:1), it is heated to 680 DEG C in Muffle furnace, obtains within insulation reaction 1.5 hours roasting and produces
Object cools to room temperature, with the sulfuric acid leaching of 3mol/L, rare earth leaching rate 92.6%.
Comparative example 2
100kg mengite rare-earth concentrate (REO content is 50wt%) is mixed into (MgCl with 260kg magnesium chloride hexahydrate2: it is dilute
Native concentrate=1.2:1), it is heated to 700 DEG C in Muffle furnace, obtains product of roasting within insulation reaction 1.5 hours, cools to room temperature,
With the sulfuric acid leaching of 3mol/L, rare earth leaching rate 88.3%.
Present invention is not limited to the embodiments described above, without departing from the essence of the present invention, this field skill
Any deformation, improvement, the replacement that art personnel are contemplated that each fall within the scope of the present invention.
Claims (10)
1. a kind of processing method of rare earth ore concentrate, which comprises the steps of:
(1) chloride of magnesium is mixed with rare earth ore concentrate, is then roasted under air conditions, to form product of roasting；Wherein,
The chloride of magnesium and the weight ratio of rare earth ore concentrate are 0.5~1.9:1, the MgCl in the chloride of magnesium2With the weight of rare earth ore concentrate
Than for 0.23~0.9:1, maturing temperature is 460~580 DEG C, calcining time is 30~200 minutes；
(2) product of roasting after cooling is directlyed adopt acid solution to leach, rare earth metal leaching rate is 95% or more.
2. the method according to claim 1, wherein magnesium chloride and rare earth ore concentrate weight ratio be 1.0~
1.8:1, the MgCl in the chloride of magnesium2Weight ratio with rare earth ore concentrate is 0.6~0.9:1, and maturing temperature is 500~580 DEG C.
3. the method according to claim 1, wherein magnesium chloride and rare earth ore concentrate weight ratio be 1.5~
1.8:1, the MgCl in the chloride of magnesium2Weight ratio with rare earth ore concentrate is 0.7~0.85:1, and maturing temperature is 560~580
℃。
4. the method according to claim 1, wherein the chloride of magnesium is magnesium chloride hexahydrate.
5. the method according to claim 1, wherein the rare earth ore concentrate is selected from mengite rare-earth concentrate, fluorine
One of carbon cerium mischmetal concentrate, monazite and fluorine carbon cerium mixed rare earth concentrate are a variety of.
6. the method according to claim 1, wherein the rare earth ore concentrate is monazite and fluorine carbon cerium mixed type
Rare earth ore concentrate.
7. according to the method described in claim 6, it is characterized in that, rare earth oxide REO's in the rare earth ore concentrate contains
Amount is 60~68wt%.
8. described in any item methods according to claim 1~7, which is characterized in that the product of roasting after cooling is not crushed
Processing directlys adopt acid solution leaching.
9. according to the method described in claim 8, it is characterized in that, it is 0.5~10mol/L's that the acid solution, which is selected from concentration,
Aqueous sulfuric acid.
10. according to the method described in claim 8, it is characterized in that, the product of roasting after cooling is dissolved in the acid
Property solution in, thus formed pH be 4~5 rare earth metal salt solutions.
Priority Applications (1)
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| CN201810960213.7A CN109136538B (en) | 2018-08-22 | 2018-08-22 | Method for treating rare earth concentrate |
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| CN201810960213.7A CN109136538B (en) | 2018-08-22 | 2018-08-22 | Method for treating rare earth concentrate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114480888A (en) * | 2022-01-28 | 2022-05-13 | 包头稀土研究院 | Method for improving rare earth recovery rate of bastnaesite |
| CN114480835A (en) * | 2022-01-28 | 2022-05-13 | 包头稀土研究院 | Method for decomposing mixed rare earth concentrate and use of composition |
| CN114836637A (en) * | 2022-05-20 | 2022-08-02 | 全南县新资源稀土有限责任公司 | Acid dissolution grouping method for rare earth oxide |
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| CN1348997A (en) * | 2001-08-28 | 2002-05-15 | 东北大学 | Roasting decomposition process of mengite-RE concentrate and mengite-mixed bastnaesite RE concentrate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114480888A (en) * | 2022-01-28 | 2022-05-13 | 包头稀土研究院 | Method for improving rare earth recovery rate of bastnaesite |
| CN114480835A (en) * | 2022-01-28 | 2022-05-13 | 包头稀土研究院 | Method for decomposing mixed rare earth concentrate and use of composition |
| CN114480835B (en) * | 2022-01-28 | 2023-12-12 | 包头稀土研究院 | Method for decomposing mixed rare earth concentrate and use of composition |
| CN114836637A (en) * | 2022-05-20 | 2022-08-02 | 全南县新资源稀土有限责任公司 | Acid dissolution grouping method for rare earth oxide |
| CN114836637B (en) * | 2022-05-20 | 2023-11-24 | 全南县新资源稀土有限责任公司 | Rare earth oxide acid-soluble grouping method |
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| CN109136538B (en) | 2020-03-10 |
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