CN107130120B - A kind of non-rare earth impurity and rare earth element extraction separating method - Google Patents
A kind of non-rare earth impurity and rare earth element extraction separating method Download PDFInfo
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- CN107130120B CN107130120B CN201710295025.2A CN201710295025A CN107130120B CN 107130120 B CN107130120 B CN 107130120B CN 201710295025 A CN201710295025 A CN 201710295025A CN 107130120 B CN107130120 B CN 107130120B
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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
- C22B59/00—Obtaining rare earth metals
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/28—Amines
- C22B3/282—Aliphatic amines
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/40—Mixtures
- C22B3/402—Mixtures of acyclic or carbocyclic compounds of different types
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/40—Mixtures
- C22B3/409—Mixtures at least one compound being an organo-metallic compound
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a kind of non-rare earth impurities and rare earth element extraction separating method, the method uses the iron in N235 extracting and separating rear earth feed liquids first, it removes that iron processes is further cleared by the iron in rare earth feed liquid with precipitation again, then uses the aluminium in non-saponified aphthenic acids extraction and separation feed liquid;Rare earth feed liquid by detaching iron, aluminium carries out extraction grouping using P507 N235 extractants, heavy rare earth is detached with light, rare earth elements, to the feed liquid containing heavy rare earth element non-saponified aphthenic acids extraction and separation yttrium and other heavy rare earth elements, extraction grouping separating calcium, magnesium and light rare earth elements, other rare earth elements are carried out to the feed liquid containing light rare earth elements using P507 N235 extractants to be further continued for being detached one by one with P507 N235 extractants.The present invention realizes being kept completely separate for non-rare earth impurity iron, aluminium, calcium, magnesium and rare earth element, realize the comprehensive utilization of acid, extractant used be not necessarily to saponification process can direct reuse, for extraction process without adding acid reagent and alkaline reagent, separation costs are very low.
Description
Technical field
The present invention relates to rare earth element extraction separating method, the extraction point of specifically a kind of non-rare earth impurity and rare earth element
From method.
Background technology
Rare earth element has unique electronic structure and light, electricity, magnetism characteristic, develops and utilizes rare earth resources, for promoting
China's expanding economy has great importance.Rare Earth Mine is main rare earth resources, in the smelting process of Rare Earth Mine, from dilute
Separation of rare earth elements is a wherein important step in the leachate of Tu Kuang.Common rare earths separation method is solvent extraction
It follows the example of.China's rare-earth trade uses the extractant separation of rare earth elements based on acidic organophosphorus extractant P507 or P204 more.
Traditional is the separation method of main extractant with P507 or P204, is needed using alkaline reagents such as ammonium hydroxide to extraction
It takes agent to carry out pre- saponification process, not only consumes a large amount of alkaline reagents, also create a large amount of ammonia nitrogen waste waters, it is necessary to by processing ability
Discharge, no it will cause environmental pollutions.In recent years, have the technology report of many non-saponifiable extraction separation of rare earth elements, wherein
" a kind of non-saponification rare earth extraction separation process "(CN102766766A), also applicant " a kind of light rare earth elements without soap
Change extraction separating method "( CN104532021A), " a method of and no saponifiable extraction detaches light rare earth elements "(
CN104120258A)Etc. patents use P507-N235 system extraction and separation rare earth chloride liquids, the acidity such as P507 can be save
The pre- saponification step of extractant realizes being detached without saponifiable extraction for rare earth element, is a kind of extraction and separation technology of green.But
Be, P507-N235 systems be used for extracting and separating rear earth element when, the presence of non-rare earth impurity can interfere the progress of extraction, wherein
Iron present in rare earth feed liquid can be extracted by P507 and be extracted by N235, and the back extraction of iron is very difficult;Rare earth feed liquid
In aluminium it is susceptible to hydrolysis, the presence of hydrolysate can lead to the generation of extraction process emulsion, make organic phase and water phase can not
Separation.In addition, the extraction and separation for rare earth element yttrium, conventional method mostly uses saponification cycloalkanes acid system, the saponification of aphthenic acids
Process equally consumes ammonium hydroxide, thus the process of extraction and separation yttrium equally will produce ammonia nitrogen waste water;Though and P507-N235 is avoided that ammonia
The generation of nitrogen waste water, but to the separating capacity of yttrium, it is but far below saponification cycloalkanes acid system, thus P507-N235 systems are used for
The extraction and separation advantage of yttrium is little.
Invention content
For the deficiency of P507-N235 systems, the present invention provides the extractions of a kind of non-rare earth impurity and rare earth element point
From method, it is therefore an objective to avoid interference of the non-rare earth impurity to P507-N235 system extracting and separating rear earth elements, while realize yttrium
The separation of no saponifiable extraction and 14 kinds of rare earth elements in addition to yttrium are detached without saponifiable extraction.
Realizing the technical solution of the object of the invention is:
A kind of extraction separating method of non-rare earth impurity and rare earth element, includes the following steps:
(1)N235, kerosene are sent into after mixing in acidification slot, with hydrochloric acid solution mixing 10min, wait for two-phase laminated flow
Afterwards, upper organic phase is separated, is sent into extraction tank, is extracted, obtained with the rare-earth chlorination leachate containing iron, aluminium, calcium, magnesium
Raffinate and load organic phases, are stripped load organic phases, obtain strip liquor;
(2)By step(1)The strip liquor of gained is sent into the first stirred tank, is heated to 60-100 DEG C, stirs 1-7h, to production
Object is filtered separation, obtains filter residue and filtrate, and filtrate cycle is sent into acidification slot, is used as the acidulant of N235 acidifications;
(3)By step(1)The raffinate of gained is sent into the second stirred tank, is heated to 60-100 DEG C, stirs 1-7h, to production
Object is filtered separation, obtains filter residue and filtrate;By filter residue and step(2)The filter residue of gained, which merges, to be collected, and is obtained iron-containing solid
Body product;
(4)By step(3)The filtrate of gained is sent into fractional extraction separation process one, becomes aphthenic acids 5-20%, N235 with group
The extractant extraction and separation of 5-20%, sec-octyl alcohol 5-40%, kerosene 10-60% obtain not iron content, aluminium in the outlet of extraction section water phase
Raffinate exports in stripping section water phase and obtains the strip liquor containing aluminium, and the organic phase that stripping section organic phase outlet obtains is after washing
Extraction section is returned to recycle;
(5)By step(4)The raffinate of gained is sent into fractional extraction separation process two, to the extraction based on P507, N235
Agent extraction and separation are taken, is exported in extraction section water phase and obtains the raffinate containing La, Ce, Pr, Nd, Ca, Mg, Sm, Eu, Gd, Tb, Dy,
It is exported in stripping section water phase and obtains the strip liquor containing Y, Ho, Er, Tm, Yb, Lu, the organic phase warp that stripping section organic phase outlet obtains
Extraction section is returned after washing to recycle;
(6)By step(5)The raffinate of gained is sent into fractional extraction separation process three, to the extraction based on P507, N235
Agent extraction and separation are taken, is exported in extraction section water phase and obtains the raffinate containing Ca, Mg, La, Ce, Pr, Nd, are exported in stripping section water phase
Obtain the strip liquor containing Sm, Eu, Gd, Tb, Dy;
(7)By step(6)The raffinate of gained is sent into fractional extraction separation process four, to the extraction based on P507, N235
Take agent extraction and separation, extraction section water phase export obtain the raffinate containing Ca, Mg, stripping section water phase outlet obtain containing La,
The strip liquor of Ce, Pr, Nd;
(8) by step(5)The strip liquor of gained is sent into fractional extraction separation process five, becomes aphthenic acids 10-20% with group,
The extractant extraction and separation of N235 5-30%, sec-octyl alcohol 5-50%, kerosene 10-60% export in extraction section water phase and obtain the extraction containing Y
Extraction raffinate exports in stripping section water phase and obtains the strip liquor containing Ho, Er, Tm, Yb, Lu;
(9)To step(6)、(7)、(8)The strip liquor of gained is further divided to the extractant based on P507, N235
From making La, Ce therein, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu are separated into single rare earth element step by step.
Wherein, step(1)Described in rare-earth chlorination leachate in contain La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy,
15 kinds of rare earth elements of Ho, Er, Tm, Yb, Lu, Y, and contain 4 kinds of non-rare earth impurity elements of Fe, Al, Ca, Mg, middle rare earth
Total concentration is 1 ~ 1.8mol/L, a concentration of 0.05-15g/ of wherein Fe a concentration of 0.01-7g/L, Al a concentration of 0.01-8g/L, Ca
A concentration of 0.05-6g/L of L, Mg.
Wherein, step(2)In, be added in a stirring kettle before stirring air or hydrogenperoxide steam generator, addition air
Molal quantity is Fe in solution2+0.25-3 times of molal quantity.
Wherein, step(2)With(3)In, bloodstone or goethite is added in whipping process or before stirring in a stirring kettle,
The bloodstone of addition or the quality of goethite are Fe in solution3+0.1-20 times of quality;Particularly, work as step(3)Middle gained
Filter residue(Iron-containing solid product)For bloodstone(Or goethite)When, take part filter residue to be added in stirred tank.
Wherein, step(1)Described in extractant be made of 10-40%N235 and 30-80% kerosene or n-hexane, be added acid
The concentration of hydrochloric acid changed in slot is 0.3-2mol/L, and organic phase and water phase is comparably 2 ~ 1 in extraction section:1 ~ 10, stripping section with 0 ~
The hydrochloric acid of 0.1mol/L is as strip liquor, and organic phase and water phase is comparably 2 ~ 1 in stripping section:1~6.
Wherein, step(5)、(6)、(7)、(9)Described in extractant by 10-50%P507,10-40%N235 and 20-60%
Kerosene forms, and washing section uses the hydrochloric acid of 0 ~ 2mol/L as cleaning solution, organic phase:Feed liquid:It is 8 ~ 1 that the stream of washing lotion, which compares,:1~10:1~
5, stripping section uses the hydrochloric acid of 0.01 ~ 3mol/L as strip liquor, and organic phase and water phase is comparably 2 ~ 1 in stripping section:1~6.
Wherein, step(4)With(8)In, washing section uses the hydrochloric acid of 0 ~ 1mol/L as cleaning solution, organic phase:Feed liquid:Washing lotion
Stream to compare be 5 ~ 1:1~4:1 ~ 3, stripping section uses the hydrochloric acid of 0.01 ~ 2mol/L as strip liquor, organic phase and water phase in stripping section
Be comparably 2 ~ 1:1~3.
Compared with the prior art, the advantages of the present invention are as follows:
(1)Either use P507 system extracting and separating rear earth elements, or using cycloalkanes acid system extraction and separation aluminium and
Yttrium, extractant are all not necessarily to saponification process, avoid the consumption of alkaline reagent, the generation of ammonia nitrogen waste water is also eliminated from source.
(2)By N235 extraction and separation iron and subsequent except iron this two steps process, it ensure that the iron in rare earth feed liquid is complete
Full removing, the interference so as to avoid iron to follow-up P507-N235 systems extracting and separating rear earth elementary process.Iron removal step discharges
Acidification of the acid cycle for N235, not only reduced the acid consumption of N235 acidification processes, but also realize the comprehensive profit of acid
With.
(3)Aphthenic acids need to be in higher acidity except aluminium(Usually require that pH<2)Lower progress, and the acidity of rare earth feed liquid is relatively low
(Usual pH>3), therefore, traditional aphthenic acids needs first acid adding to adjust the acidity of rare earth feed liquid to pH except aluminium process<2;And it is of the invention
The method, rare earth feed liquid remove aluminium process after iron removal, and the acid of iron removal release can make the acid of rare earth feed liquid
Degree is increased to pH<2, the acid adding operation before being operated except aluminium is not only eliminated, the acid consumption except aluminium operation has been greatly reduced.
(4)Iron, aluminium in rare earth feed liquid are just detached before rare earth element extraction and separation, avoid aphthenic acids extraction and separation
Emulsion during yttrium caused by iron, aluminum water solution.In addition, before aphthenic acids extraction and separation yttrium, use
P507-N235 extraction systems are grouped rare earth element, the non-rare earth impurities such as calcium, magnesium not in the heavy rare earth containing yttrium, because
And impurity content is lower in the raffinate after aphthenic acids extraction and separation yttrium, prepared yttrium oxide product purity higher.
(5)Iron, aluminium, yttrium and other rare earth elements extraction separation process used in extractant be all without saponification process
Ke Xunhuanliyong, production process adjusts the acidity of solution without adding alkaline reagent without additional addition acid solution;Cause
This, the production cost of the method for the invention is very low.
Description of the drawings
Fig. 1 is the separation process figure of embodiment 1 rare earth feed liquid iron and other elements.
Fig. 2 is the separation process of embodiment 2 rare earth feed liquid aluminium and other elements(Fractional extraction process one)Figure.
Fig. 3 is 3 rare earth feed liquid heavy rare earth of embodiment and light, rare earth elements separation process(Fractional extraction process two)
Figure.
Fig. 4 is the separation process of 4 rare earth feed liquid calcium of embodiment, magnesium and other rare earth elements(Fractional extraction process three, four)
Flow chart.
Fig. 5 is the separation process of embodiment 5 rare earth feed liquid yttrium and other rare earth elements(Fractional extraction process five)Figure.
Specific implementation mode
With reference to embodiment and attached drawing, the present invention is described in further detail, to more fully understand present disclosure,
But the present invention is not limited to following embodiments.
Embodiment 1:
30%N235 and 70% kerosene are sent into after mixing in acidification slot, with 1mol/L hydrochloric acid solution mixing 10min, are waited for
After two-phase laminated flow, upper organic phase is separated, is sent into extraction tank, with the rare-earth chlorination leachate containing iron, aluminium, calcium, magnesium(Wherein
Rare earth concentration is 1.5mol/L, concentration of iron 1.35g/L, aluminum concentration 3g/L, calcium concentration 4g/L, magnesium density 1.1g/L)
According to compared to(Organic phase:Water phase)It is 1:1 ratio mixes 15min, after two-phase laminated flow, measures the material of extraction tank water phase outlet
Concentration of iron is down to 0.07g/L in liquid, from extraction tank organic phase outlet flow out organic phase be sent into back extraction slot, according to compared to(It is organic
Phase:Water phase)It is 1:5 ratio is added water and is stirred 15min with organic phase, after two-phase laminated flow, has from what back extraction slot flowed out
Machine mutually returns to acidification slot and recycles.
It is sent into the first stirred tank from the liquid of back extraction slot water phase outlet outflow, hydrogenperoxide steam generator is added(Wherein peroxide
The molal quantity for changing hydrogen is to be stripped Fe in the liquid of slot water phase outlet outflow2+1.5 times of molal quantity), 95 DEG C are warming up to, is stirred to react
It is filtered after 2h, collects filter residue, filtrate returns to acidification slot and recycles.
2g bloodstone is added in the second stirred tank, the feed liquid of extraction tank water phase outlet outflow is sent into the second stirred tank
In, 80 DEG C are warming up to, is filtered after being stirred to react 5h, collects filter residue and filtrate, after measured, concentration of iron is less than in filtrate
2ppm.Filter residue merges collection with the filter residue obtained from the first stirred tank.Flow is as shown in Figure 1.
Embodiment 2:
The filtrate that 1 second stirred tank of embodiment is isolated is sent into the 4th grade of extraction section in fractional extraction process one, is extracting
The 1st grade of addition group of section is taken to become aphthenic acids 10%, N235 10%, sec-octyl alcohol 40%, the organic phase of kerosene 35%, in washing section
0.04mol/L hydrochloric acid solutions, organic phase is added in 3rd level:Feed liquid:It is 4 that the stream of washing lotion, which compares,:1:1, it is added in the 3rd level of stripping section
It is 1 that the stream of 1.1mol/L hydrochloric acid solutions, wherein organic phase and water phase, which compares,:2.The organic phase of stripping section outlet outflow is washed through 2 grades
The 1st grade of recycling of extraction section is returned afterwards.After measured, main component is chlorine from the strip liquor of stripping section water phase outlet outflow
Change aluminium, other elements content in addition to aluminum is less than 100ppm, and main component is from the raffinate of extraction section water phase outlet outflow
Rare earth-iron-boron and calcium chloride, magnesium chloride, aluminium ion concentration are less than 50ppm.Flow is as shown in Figure 2.
Embodiment 3:
The raffinate of 2 gained of embodiment is sent into the 5th grade of extraction section in fractional extraction separation process two, group is become
P507 50%, N235 20%, organic be added to extraction section the 1st grade of kerosene 30%, the 5th grade in washing section is added 1.1mol/
L hydrochloric acid solutions, organic phase:Feed liquid:It is 5 that the stream of washing lotion, which compares,:1:0.5,3mol/L hydrochloric acid solutions are added in the 3rd level of stripping section,
It is 1 that wherein the stream of organic phase and water phase, which compares,:3.After measured, extraction section water phase export obtain with La, Ce, Pr, Nd, Ca, Mg,
Raffinate based on Sm, Eu, Gd, Tb, Dy, the wherein total concentration of Y, Ho, Er, Tm, Yb, Lu are less than 310ppm, in stripping section water
Mutually outlet obtains the strip liquor based on Y, Ho, Er, Tm, Yb, Lu, wherein La, Ce, Pr, Nd, Ca, Mg, Sm, Eu, Gd, Tb, Dy
Total concentration be less than 200ppm.The organic phase that stripping section organic phase outlet obtains returns to the 1st grade of cycle of extraction section after 4 grades of washings
It uses.Flow is as shown in Figure 3.
Embodiment 4:
The raffinate of 3 gained of embodiment is sent into the 9th grade of extraction section in fractional extraction separation process three, group is become
P507 40%, N235 25%, organic be added to extraction section the 1st grade of kerosene 35%, in the 10th grade of addition of washing section
0.8mol/L hydrochloric acid solutions, organic phase:Feed liquid:It is 6 that the stream of washing lotion, which compares,:1:1,2.5mol/L salt is added in the 3rd level of stripping section
It is 1 that the stream of acid solution, wherein organic phase and water phase, which compares,:4.After measured, extraction section water phase export obtain with Ca, Mg, La, Ce,
Raffinate based on Pr, Nd, the wherein total concentration of Sm, Eu, Gd, Tb, Dy be less than 250ppm, stripping section water phase export obtain with
Strip liquor based on Sm, Eu, Gd, Tb, Dy, the wherein total concentration of Ca, Mg, La, Ce, Pr, Nd are less than 320ppm.Stripping section is organic
It mutually exports obtained organic phase and returns to the 1st grade of recycling of extraction section after 2 grades of washings.
Raffinate is sent into the 6th grade of four extraction section of fractional extraction separation process, group is become into P507 55%, N235
35%, organic be added to extraction section the 1st grade of kerosene 25%, the 7th grade in washing section is added 0.05mol/L hydrochloric acid solutions, has
Machine phase:Feed liquid:It is 6 that the stream of washing lotion, which compares,:1:2,2mol/L hydrochloric acid solutions, wherein organic phase and water is added in the 3rd level of stripping section
It is 2 that the stream of phase, which compares,:1.After measured, the raffinate based on Ca, Mg, wherein La, Ce, Pr, Nd are obtained in the outlet of extraction section water phase
Total concentration be less than 180ppm, in the outlet of stripping section water phase obtain strip liquor based on La, Ce, Pr, Nd, wherein Ca, Mg
Total concentration is less than 360ppm.The organic phase that stripping section organic phase outlet obtains returns to the 1st grade of cycle of extraction section after 2 grades of washings to be made
With.Flow is as shown in Figure 4.
Embodiment 5:
The strip liquor of 3 gained of embodiment is sent into the 11st grade of extraction section in fractional extraction separation process five, group is become
Aphthenic acids 20%, N235 20%, sec-octyl alcohol 30%, the organic of kerosene 30% are added to the 1st grade of extraction section, and the 9th grade in washing section adds
Enter 1.8mol/L hydrochloric acid solutions, organic phase:Feed liquid:It is 3 that the stream of washing lotion, which compares,:1:1, the 4th grade in stripping section is added 2.8mol/L
It is 3 that the stream of hydrochloric acid solution, wherein organic phase and water phase, which compares,:2.It is exported in extraction section water phase and obtains the raffinate containing Y, wherein Ho,
The concentration of Er, Tm, Yb, Lu are less than 100ppm, are exported in stripping section water phase and obtain the strip liquor containing Ho, Er, Tm, Yb, Lu,
The concentration of middle Y is less than 90ppm.The organic phase that stripping section organic phase outlet obtains returns to the 1st grade of cycle of extraction section after 3 grades of washings
It uses.Flow is as shown in Figure 5.
Claims (8)
1. a kind of non-rare earth impurity and rare earth element extraction separating method, it is characterised in that include the following steps:
(1)N235, kerosene are sent into after mixing in acidification slot, are divided after two-phase laminated flow with hydrochloric acid solution mixing 10min
Go out upper organic phase, is sent into extraction tank, is extracted with the rare-earth chlorination leachate containing iron, aluminium, calcium, magnesium, obtain raffinate
Liquid and load organic phases, are stripped load organic phases, obtain strip liquor;
(2)By step(1)The strip liquor of gained is sent into the first stirred tank, is heated to 60-100 DEG C, stirs 1-7h, is carried out to product
It is separated by filtration, obtains filter residue and filtrate, filtrate cycle is sent into acidification slot, is used as the acidulant of N235 acidifications;
(3)By step(1)The raffinate of gained is sent into the second stirred tank, is heated to 60-100 DEG C, stirs 1-7h, to product into
Row is separated by filtration, and obtains filter residue and filtrate;By filter residue and step(2)The filter residue of gained, which merges, to be collected, and iron-containing solid production is obtained
Product;
(4)By step(3)The filtrate of gained is sent into fractional extraction separation process one, becomes aphthenic acids 5-20%, N235 5- with group
The extractant extraction and separation of 20%, sec-octyl alcohol 5-40%, kerosene 10-60% obtain not iron content, the extraction of aluminium in the outlet of extraction section water phase
Extraction raffinate, exports in stripping section water phase and obtains the strip liquor containing aluminium, and the organic phase that stripping section organic phase outlet obtains is returned after washing
Extraction section is returned to recycle;
(5)By step(4)The raffinate of gained is sent into fractional extraction separation process two, to the extractant based on P507, N235
Extraction and separation export in extraction section water phase and obtain the raffinate containing La, Ce, Pr, Nd, Ca, Mg, Sm, Eu, Gd, Tb, Dy, anti-
Extract the outlet of section water phase and obtain the strip liquor containing Y, Ho, Er, Tm, Yb, Lu, the organic phase that stripping section organic phase outlet obtains is through washing
Extraction section is returned afterwards to recycle;
(6)By step(5)The raffinate of gained is sent into fractional extraction separation process three, to the extractant based on P507, N235
Extraction and separation export in extraction section water phase and obtain the raffinate containing Ca, Mg, La, Ce, Pr, Nd, export and obtain in stripping section water phase
Strip liquor containing Sm, Eu, Gd, Tb, Dy;
(7)By step(6)The raffinate of gained is sent into fractional extraction separation process four, to the extractant based on P507, N235
Extraction and separation, extraction section water phase export obtain the raffinate containing Ca, Mg, stripping section water phase outlet obtain containing La, Ce, Pr,
The strip liquor of Nd;
(8)By step(5)The strip liquor of gained is sent into fractional extraction separation process five, becomes aphthenic acids 10-20%, N235 with group
The extractant extraction and separation of 5-30%, sec-octyl alcohol 5-50%, kerosene 10-60% export in extraction section water phase and obtain the raffinate containing Y,
It is exported in stripping section water phase and obtains the strip liquor containing Ho, Er, Tm, Yb, Lu;
(9)To step(6)、(7)、(8)The strip liquor of gained is further detached to the extractant based on P507, N235,
Make La, Ce therein, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu are separated into single rare earth element step by step.
2. non-rare earth impurity according to claim 1 and rare earth element extraction separating method, it is characterised in that:Step(1)
Described in rare-earth chlorination leachate in contain La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, 15 kinds of Ho, Er, Tm, Yb, Lu, Y
Rare earth element, and contain 4 kinds of non-rare earth impurity elements of Fe, Al, Ca, Mg, middle rare earth total concentration is 1 ~ 1.8mol/L,
A concentration of 0.05-6g/L of middle a concentration of 0.01-7g/L of Fe, Al a concentration of 0.01-8g/L, Ca a concentration of 0.05-15g/L, Mg.
3. non-rare earth impurity according to claim 1 and rare earth element extraction separating method, it is characterised in that:Step(2)
In, air or hydrogenperoxide steam generator, the air or hydrogen peroxide of addition is added in whipping process or before stirring in a stirring kettle
Molal quantity be solution in Fe2+0.25-3 times of molal quantity.
4. non-rare earth impurity according to claim 1 and rare earth element extraction separating method, it is characterised in that:Step(2)
With(3)In, bloodstone or goethite, the bloodstone or needle of addition is added before stirring in the first stirred tank and the second stirred tank
The quality of iron ore is Fe in solution3+0.1-20 times of quality.
5. non-rare earth impurity according to claim 1 and rare earth element extraction separating method, it is characterised in that:Step(3)
When the iron content solid product of middle gained is bloodstone or goethite, portioned product is taken to be separately added into the first stirred tank and the second stirring
In kettle.
6. non-rare earth impurity according to claim 1 and rare earth element extraction separating method, it is characterised in that:Step(1)
Described in extractant be made of 10-40%N235 and 30-80% kerosene or n-hexane, be added acidification slot in concentration of hydrochloric acid be
0.3-2mol/L, organic phase and water phase is comparably 2 ~ 1 in extraction section:1 ~ 10, stripping section use the hydrochloric acid of 0 ~ 0.1mol/L as
Strip liquor, organic phase and water phase is comparably 2 ~ 1 in stripping section:1~6.
7. non-rare earth impurity according to claim 1 and rare earth element extraction separating method, it is characterised in that:Step(5)、
(6)、(7)、(9)Described in extractant by 10-50%P507,10-40%N235 and 20-60% kerosene composition, washing section with 0 ~
The hydrochloric acid of 2mol/L is as cleaning solution, organic phase:Feed liquid:It is 8 ~ 1 that the stream of washing lotion, which compares,:1~10:1 ~ 5, stripping section with 0.01 ~
The hydrochloric acid of 3mol/L is as strip liquor, and organic phase and water phase is comparably 2 ~ 1 in stripping section:1~6.
8. non-rare earth impurity according to claim 1 and rare earth element extraction separating method, it is characterised in that:Step(4)
With(8)In, washing section uses the hydrochloric acid of 0 ~ 1mol/L as cleaning solution, organic phase:Feed liquid:It is 5 ~ 1 that the stream of washing lotion, which compares,:1~4:1 ~ 3,
Stripping section uses the hydrochloric acid of 0.01 ~ 2mol/L as strip liquor, and organic phase and water phase is comparably 2 ~ 1 in stripping section:1~3.
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