CN106636685A - Method for extracting rare earth element from cerium-doped yttrium lutecium silicate crystals - Google Patents
Method for extracting rare earth element from cerium-doped yttrium lutecium silicate crystals Download PDFInfo
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Abstract
The invention relates to a method for extracting rare earth elements from cerium-doped yttrium lutecium silicate crystals. The method comprises the following steps of S1, crushing and sieving the cerium-doped yttrium lutecium silicate crystals to obtain powder; S2, adding the powder into alkali solution; performing roasting to obtain roasting products; S3, performing water washing and filtering on the roasting products to obtain first filter liquid and first precipitates; S4, adding acid into the first filter liquid to regulate the pH and to precipitate silicic acid; firing the silicic acid to obtain silicon oxide; S5, performing acid addition, dissolution and oxidation on the first precipitates; regulating the pH for precipitating or extracting and separating quadrivalent cerium ions; leaving residue liquid; S6, performing yttrium and lutecium separation operation on the residue liquid. The cerium, the yttrium, the lutecium and the silicic acid are respectively purified and recovered; the obtained product has high purity; the cyclic utilization of the rare earth elements can be realized; the production cost is effectively reduced; the product market competitiveness is improved.
Description
Technical field
The present invention relates to a kind of extracting method of rare earth element, more particularly to a kind of carry from the yttrium luetcium silicate crystal for mixing cerium
The method for taking rare earth element.
Background technology
Yttrium luetcium silicate due to mixing cerium（Ce:LYSO, it is also possible to be written as (Lu1-x-yYxCey)2SiO5）Crystal has high density,
The excellent scintillation properties such as high atomic number, height output and fast die-away time.Through the research of more than ten years, in crystal growth, dodge
Bright performance study and device design all obtain greater advance, and start to obtain extensively application.Due to Ce:LYSO crystal is comprehensive
Can be excellent, its discovery causes the scientific research of the states such as the extensive concern of world's scintillation crystal circle, the U.S., Japan, Germany, Russia
Mechanism all strengthens to Ce:The research dynamics of LYSO crystal, especially to Ce:The research of LYSO Scintillation Properties and device,
Research shows：Use Ce:Ray detector made by LYSO crystal has boundless potential application, including nuclear medicine
（PET、CT、SPECT）, oil well probing, high-energy physics, nuclear physics, safety inspection, the aspect such as environmental test.The coming years, Ce:
The market prospects of LYSO crystal will be boundless.
Ce:While LYSO scale of mass production, substantial amounts of substandard product, processing leftover pieces or crucible bottom are also generated
Material.Contain substantial amounts of valuable element, particularly rare earth element in these leftover pieces.Rare earth is a kind of non-renewable resource, right
National economy and national security have important strategic importance.Therefore, the recycling to rare earth resources is particularly significant.Additionally,
By Ce:Valuable element recycling in LYSO waste materials, can also effectively reduce production cost, improve the market competition of product
Power.
Therefore, it is necessary to design a kind of method of the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium.
The content of the invention
It is an object of the invention to provide a kind of method of the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium.
To realize object defined above, the present invention is adopted the following technical scheme that：It is a kind of to extract from the yttrium luetcium silicate crystal for mix cerium
The method of rare earth element, it comprises the steps：
Step S1：The yttrium luetcium silicate crystal fracture of cerium will be mixed, sieving obtains powder；
Step S2：Above-mentioned powder is added in aqueous slkali, then carries out roasting and obtain product of roasting；
Step S3：Above-mentioned product of roasting is washed and filtered, the first filtrate and the first precipitation is obtained；
Step S4：Add acid for adjusting pH to be settled out silicic acid the first filtrate, silicic acid calcination is obtained into silica；
Step S5：First precipitation is carried out into acid adding, dissolving, oxidation, pH precipitations or extraction separation of quadravalence cerium ion is adjusted, remaining as
Extraction raffinate；
Step S6：Extraction raffinate is carried out into the operation of separating yttrium, lutetium.
As a further improvement on the present invention, crystal fracture mode is first Mechanical Crushing in step S1, then uses ball milling
Machine is levigate.
As a further improvement on the present invention, powder is added in step S2 and is mixed and stirred in aqueous slkali uniformly,
The solute of aqueous slkali is 1 with the mass ratio of powder:1～1:5, then roasting, 100～300 DEG C of sintering temperature, roasting time 1～5
Hour.
As a further improvement on the present invention, water temperature is 30～100 DEG C when washing in step S3, washing time 1～4
Hour, water-washing method is to wash while stirring.
As a further improvement on the present invention, acid for adjusting pH is added to precipitate between 4～5 to the first filtrate in step S4
Go out silicic acid, afterwards calcination obtains silica under the conditions of 600～1000 DEG C by silicic acid.
As a further improvement on the present invention, after control is aoxidized in step S5 between the pH to 3～4 of solution, quadrivalent cerium is then
It is precipitated out in the form of cerium hydroxide, is filtrated to get cerium hydroxide precipitation and extraction raffinate, cerium hydroxide precipitation roasting is obtained
The oxide of cerium.
As a further improvement on the present invention, tetravalence is extracted in solution from after oxidation with extractant P204 in step S5
Cerium ion, washes down tetravalence cerium ion from organic phase again plus oxalic acid precipitation with hydrochloric acid, and then calcination obtains the oxide of cerium.
As a further improvement on the present invention, step S6 is according to following steps separating yttrium lutetium：Using two step extractor bodies
It is separating yttrium：With N263- heavy solvent-RE (NO3)3-LiNO3System and N263- heavy solvent-RECl3-NH4CNS system fractional extractions
Yttrium, obtains the raffinate containing yttrium again Jing after oxalic acid precipitation, and calcining obtains yittrium oxide, is the extract containing lutetium in organic phase, uses
After sour back extraction, simultaneously ignition precipitate obtains luteium oxide to reprecipitation.
As a further improvement on the present invention, step S6 is according to following steps separating yttrium lutetium：With extractant extraction point
From yttrium：Allotment feed liquid to rare earth ion total concentration be 0.5～2.5mol/L, pH between 1.5～3.5, the extractant for adopting for
Aphthenic acids-mixed alcohol-kerosene, and saponification is carried out with alkali lye, saponification degree is 60～90%, uses VHaveRepresent organic extractant, VMaterialRepresent
Material liquid volume, VWashWashing lotion volume is represented, stream is than being VHave：VMaterial：VWash=4～10:1:1～3, the organic phase concentration after separating and extracting
For 1～5mol/L salt acid elutions, after multitple extraction and washing, go out saliva and mutually obtain yttrium chloride solution, be in organic phase containing
The extract of lutetium, then back extraction is carried out with acid, the strip liquor of lutetium is obtained, then oxalic acid precipitation is used respectively, 700～1000 DEG C of precipitation Jing burns
Burning obtains yittrium oxide and luteium oxide.
As a further improvement on the present invention, step S6 is according to following steps separating yttrium lutetium：Extraction raffinate is handed over using ion
Change chromatography and carry out separating yttrium lutetium, first adsorb rare earth ion on adsorption column, then using the connection of drip washing under different temperatures
With method, different using eluent drip washing sequencing with eluent drip washing on adsorption column and splitter, drip washing is respectively obtained
Solution containing yttrium and the solution containing lutetium, respectively with oxalic acid precipitation after, in 700～1000 DEG C of calcinations, respectively obtain yittrium oxide and oxygen
Change lutetium.
The present invention from Extraction of rare earth element in the yttrium luetcium silicate crystal for mix cerium, cerium, yttrium, lutetium and silicic acid are purified respectively,
Reclaim, resulting product purity is high, realizes recycling for rare earth element, effectively reduces production cost, improves product
The market competitiveness.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described enforcement
Example is only a part of embodiment of the invention, rather than the embodiment of whole.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.
The present invention provides a kind of method of the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium, and it includes following step
Suddenly：
Step S1：The yttrium luetcium silicate crystal fracture of cerium will be mixed, sieving obtains powder；
Step S2：Step S1 gained powder is added in aqueous slkali, then carries out roasting and obtain product of roasting；
Step S3：Above-mentioned product of roasting is washed and filtered, the first filtrate and the first precipitation is obtained；
Step S4：Add acid for adjusting pH to be settled out silicic acid the first filtrate, silicic acid calcination is obtained into silica；
Step S5：First precipitation is carried out into acid adding, dissolving, oxidation, pH precipitations or extraction separation of quadravalence cerium ion is adjusted, remaining as
Extraction raffinate；
Step S6：Extraction raffinate is carried out into the operation of separating yttrium, lutetium.
The raw material that step S1 is adopted is the discarded yttrium luetcium silicate crystal for mixing cerium, in certain embodiments of the present invention
In, the crumbling method for mixing the yttrium luetcium silicate crystal of cerium is preferably：Mechanical Crushing is first carried out, then it is levigate with ball mill.
In the step S2 powder is added uniform, the solute of aqueous slkali and the quality of powder will be mixed and stirred in aqueous slkali
Than being preferably 1:1～1:5, then roasting, sintering temperature is preferably 100～300 DEG C, and roasting time is preferably 1～5 hour,
In certain embodiments of the present invention, the solute of aqueous slkali is 1 with the mass ratio of powder:1、1:2、1:3、1:5；In certain of the invention
In a little embodiments, sintering temperature is 100 DEG C, 250 DEG C, 300 DEG C；In certain embodiments of the present invention, roasting time is 1 little
When, 3 hours, 5 hours.The solute of the aqueous slkali in step S2, in certain embodiments of the present invention, preferably in NaOH, KOH
One or more.
Water temperature is 30～100 DEG C when washing in step S3, washing time 1～4 hour, and water-washing method is for while stirring
Washing, in certain embodiments of the present invention, water temperature is 30 DEG C, 70 DEG C, 100 DEG C；In certain embodiments of the present invention, wash
Time is 1 hour, 2 hours, 4 hours.
Add acid for adjusting pH to silicic acid is settled out between 4～5 to the first filtrate in step S4, afterwards by silicic acid 600
Calcination under the conditions of～1000 DEG C obtains silica.In certain embodiments of the present invention, the acid of addition is hydrochloric acid；The present invention's
In some embodiments, plus acid for adjusting pH is to 4,4.5 or 5；In certain embodiments of the present invention, calcination temperature be 700 DEG C, 850
℃、1000℃。
For step S5：Specifically there is two methods separation of quadravalence cerium ion, first method is：Solution after control oxidation
Between pH to 3～4, quadrivalent cerium is then precipitated out in the form of cerium hydroxide, is filtrated to get cerium hydroxide precipitation and extraction raffinate, will
Cerium hydroxide precipitation roasting obtains the oxide of cerium；Second method is：Use extractant P204（It is double（2- ethylhexyls）Phosphoric acid
Ester）Tetravalence cerium ion is extracted in solution from after oxidation, tetravalence cerium ion is washed down from organic phase with hydrochloric acid add again oxalic acid precipitation,
Then calcination obtains the oxide of cerium.
For step S6, specifically there are three kinds of method separating yttrium lutetiums：First method is：Separated using two step extraction systems
Yttrium：With N263- heavy solvent-RE (NO3)3-LiNO3System and N263- heavy solvent-RECl3-NH4CNS systems（RE3+Represent rare earth
Ion）Fractional extraction yttrium, obtains the raffinate containing yttrium again Jing after oxalic acid precipitation, and calcining obtains yittrium oxide, be in organic phase containing
The extract of lutetium, after sour back extraction, simultaneously ignition precipitate obtains luteium oxide to reprecipitation.
Second method is：With extractant extract and separate yttrium：Allotment extraction raffinate to rare earth ion total concentration be 0.2～
Between 1.5～3.5, the extractant for adopting is aphthenic acids-mixed alcohol-kerosene, and carries out saponification with alkali lye for 2.5mol/L, pH,
Saponification degree is 60～90%, uses VHaveRepresent organic extractant, VMaterialRepresent material liquid volume, VWashWashing lotion volume is represented, stream is than being VHave：VMaterial：
VWash=4～10:1:1～3, the yttrium solution that saliva mutually obtains purity 4N is gone out after separating and extracting, organic phase concentration is 1～5mol/L
Hydrochloric acid, after multitple extraction and washing, the yttrium in organic phase is washed the purity of lutetium in the yield and organic phase of lower raising yttrium, extraction
Taking liquid acid carries out back extraction, obtains the strip liquor of lutetium, then with oxalic acid precipitation, precipitates 700～1000 DEG C of calcinations of Jing and obtain yittrium oxide
And luteium oxide.
The third method is：Extraction raffinate, come separating yttrium lutetium, is first being adsorbed rare earth ion using ion exchange chromatography
Adsorb on post, then using the method for combined use of drip washing under different temperatures, with eluent drip washing on adsorption column and splitter, utilize
Eluent drip washing sequencing is different, and drip washing respectively obtains the solution containing yttrium and the solution containing lutetium, respectively with oxalic acid precipitation after,
700～1000 DEG C of calcinations, respectively obtain yittrium oxide and luteium oxide.
In order to further illustrate the present invention, describe the present invention with reference to embodiments, but can not be managed
Solve as limiting the scope of the present invention.
Embodiment 1.
First, the yttrium luetcium silicate crystal for mixing cerium is taken, Mechanical Crushing is first carried out, then it is levigate with ball mill, with the sieve of 325 mesh
Carry out screening the crystal powder for obtaining that average grain diameter is 0.045mm.
Then by concentration in the above-mentioned crystal powders of sodium hydroxide solution mixing 100g of 5mol/L, NaOH and crystal
The mass ratio of powder is 1:2, then carry out roasting and obtain product of roasting, sintering temperature is 200-300 DEG C, roasting time 4 hours.
Product of roasting is washed with 70 DEG C of warm water, is stirred 2 hours in washing, is filtrated to get the first filtrate and first and is sunk
Form sediment, containing soluble silicate in the first filtrate, the first precipitation is then rare-earth precipitation.
By the first filtrate under 80 DEG C, stirring condition, the pH of the first filtrate is adjusted to 4.5 with the hydrochloric acid of concentration 3mol/L,
So that silicic acid precipitates, then calcination is carried out under the conditions of silicic acid is deposited in into 800 DEG C obtain silica.
Rare-earth precipitation is adjusted into pH with the hydrochloric acid solution of 2.5mol/L to be allowed to be completely dissolved to 2.0, reaction temperature is 75 DEG C,
Reaction is filled with sufficient amount of oxygen in 2 hours in backward solution, then reacts 3 hours, it is ensured that the Ce in solution3+It is completely oxidized to Ce4+, so
It is 4 to add sodium hydroxide solution to be adjusted to pH afterwards, Ce4+The Precipitation in the form of cerium hydroxide, then carry out being filtrated to get extraction raffinate
With cerium hydroxide precipitation, cerium hydroxide precipitation 850 DEG C of calcinations of Jing, obtain ceria, the extraction raffinate after filtration again extract and separate yttrium,
Lutetium.
The total concentration of allotment extraction raffinate to rare earth ion is 0.5-1.5mol/L, and pH is adjusted to 3.5 formation feed liquids, adds organic phase
Extract and separate is carried out in separating and extracting system for the kerosene of+20% mixed alcohol of 20% aphthenic acids+60%, uses the NaOH saponification, saponification degree to be
80%, use VHaveRepresent organic extractant, VMaterialRepresent material liquid volume, VWashWashing lotion volume is represented, stream is than being VHave：VMaterial：VWash=7～10:1:2
～3, through 72 grades of extraction, 13 grades of washing, cleaning solution is the HCl of concentration 2.5mol/L, in water acquisition high-purity is mutually exported
Yttrium chloride solution, the oxalic acid precipitation of the yttrium chloride solution high-quality is filtrated to get yttrium oxalate precipitation, then carries out 900 DEG C of calcinations,
The yittrium oxide that purity is 4N is obtained with, in organic phase outlet highly purified lutetium extract is just obtained, after sour back extraction, Jing is careless
Again 900 DEG C of calcinations can obtain high-purity luteium oxide to acid precipitation, and product purity is up to more than 4N.
Embodiment 2.
First, the yttrium luetcium silicate crystal for mixing cerium is taken, Mechanical Crushing is first carried out, then it is levigate with ball mill, finally use 325 purposes
Sieve carries out sieving the crystal powder for obtaining that average grain diameter is 0.045mm.
Then by concentration in the above-mentioned crystal powders of sodium hydroxide solution mixing 100g of 6mol/L, NaOH and powder
Mass mixing ratio be 1:1, then roasting is carried out, sintering temperature is 250 DEG C, roasting time 3 hours.
Material after roasting 30 DEG C of hot wash, agitator treating 4 hours, are filtrated to get the first filtrate and first heavy
Form sediment.Contain silicate in first filtrate, rare earth element is then contained in the first precipitation.
By the first filtrate under 80 DEG C of stirring conditions, with the salt acid for adjusting pH of concentration 3mol/L to 4 so that under silicic acid precipitation
Come, then carry out 600 DEG C of calcinations to obtain silica.
Containing rare earth element first precipitation is allowed to be completely dissolved with the hydrochloric acid solution of 2.5mol/L, and while in solution
Enough air is filled with, is reacted 3 hours, the Ce in solution3+It is completely oxidized to Ce4+, using quadrivalent cerium and P204 extractants have compared with
Strong complexing power, with P204 by tetravalence cerium ion from solution with other ion isolations out, remaining as extraction raffinate, use
The hydrochloric acid of 0.8mol/L is Ce4+Wash down from organic phase again plus oxalic acid precipitation, then under conditions of 900 DEG C calcination into titanium dioxide
Cerium.
It is 1.5-2.5mol/L that allotment extraction raffinate causes the total concentration of rare earth ion, and pH is adjusted to 3.5 formation feed liquids, molten with NaOH
Liquid saponification, saponification degree 85%, in being subsequently adding the separating and extracting system that organic phase is the kerosene of+20% mixed alcohol of 20% aphthenic acids+60%
Extract and separate is carried out, V is usedHaveRepresent organic extractant, VMaterialRepresent material liquid volume, VWashWashing lotion volume is represented, stream is than being VHave：VMaterial：VWash=
4～7:1:1～2, through 70 grades of extraction, 10 grades of washing, cleaning solution is the HCl of concentration 3.0mol/L, mutually exports in water and obtain
Yttrium chloride solution is obtained, the oxalic acid precipitation of the solution high-quality is filtered, then carries out 800 DEG C of calcinations, it is possible to obtain the oxygen of purity 4N
Change yttrium, in organic phase outlet high-purity extract containing lutetium is just obtained, after sour back extraction, again 800 DEG C of calcinations can be obtained Jing oxalic acid precipitations
High-purity luteium oxide, product purity is up to more than 4N.
Embodiment 3.
The yttrium luetcium silicate crystal for mixing cerium is taken, Mechanical Crushing is first carried out, then, final sieve with 325 mesh levigate with ball mill
Carry out sieving the powder for obtaining that average grain diameter is 0.045mm.
Then the above-mentioned powder of 80g is mixed into the sodium hydroxide solution that concentration is 6mol/L, the matter of NaOH and powder
Amount mixing ratio is 1:5, then roasting is carried out, sintering temperature is 100-200 DEG C, roasting time 5 hours.
Material after roasting 100 DEG C of hot wash, agitator treating 1 hour, are filtrated to get the first filtrate and first heavy
Form sediment.Contain silicate in first filtrate, rare earth element is then contained in the first precipitation.
By the first filtrate under 80 DEG C of stirring conditions, with the salt acid for adjusting pH of concentration 3mol/L to 5 so that silicon precipitates
800 DEG C of calcinations are carried out again obtains silica.
The containing rare earth element first precipitation is adjusted into pH with the hydrochloric acid solution of 2.5mol/L to be allowed to be completely dissolved to 1, is reacted
Temperature is 75 DEG C, in 2 hours reaction time, enough air is then filled with solution, is reacted 1.5 hours, the Ce in solution3+It is complete
Total oxygen is melted into Ce4+, it is subsequently adding sodium hydroxide solution regulation pH to 3.5 and allows cerium hydroxide to precipitate, with the yttrium lutetium in extraction raffinate
Ion isolation.The cerium hydroxide of precipitation is filtered, is dried, being heated to 850 DEG C is carried out calcination, obtains ceria.
Extraction raffinate extract and separate yttrium lutetium again：Using two step extraction system separating yttriums, with N263- heavy solvent-RE (NO3)3-LiNO3
System and N263- heavy solvent-RECl3-NH4CNS systems, fractional extraction yttrium, obtain the raffinate containing yttrium, Jing oxalic acid precipitations
Afterwards, then by 1000 DEG C of calcinings yittrium oxide is obtained, the extract containing lutetium is arrived in organic phase, is precipitated with after sour back extraction, then Jing
1000 DEG C of calcinations obtain luteium oxide, and yittrium oxide, luteium oxide purity are up to 4N.
Embodiment 4.
First, the yttrium luetcium silicate crystal for mixing cerium is taken, Mechanical Crushing is first carried out, then it is levigate with ball mill, finally use 325 purposes
Sieve carries out sieving the crystal powder for obtaining that average grain diameter is 0.045mm.
Then the above-mentioned powder of 50g is added into concentration for mixing, NaOH and powder in the sodium hydroxide solution of 6mol/L
Mass ratio be 1:3, then roasting is carried out, sintering temperature is 200-300 DEG C, roasting time 2 hours.
Material after roasting 60 DEG C of hot wash, agitator treating 1 hour, are filtrated to get the first filtrate and first heavy
Form sediment.Contain silicate in first filtrate, rare earth element is then contained in the first precipitation.
By the first filtrate under 80 DEG C of stirring conditions, with the salt acid for adjusting pH of concentration 3mol/L to 4.5 so that silicic acid is precipitated
Get off, being again heated to 750 DEG C carries out the oxide that calcination obtains silicon.
Containing rare earth element first precipitation is allowed to be completely dissolved with the hydrochloric acid solution of 2.5mol/L, reaction temperature is 70
DEG C, 1 hour reaction time, and while enough air is filled with solution, reaction 1 hour is subsequently adding sodium hydroxide solution tune
Section pH to 3.5, the Ce in solution3+It is oxidized to Ce4+After become cerium hydroxide precipitation, be filtrated to get extraction raffinate and cerium hydroxide heavy
Form sediment, cerium hydroxide drying is heated into 850 DEG C of calcinations, obtain ceria.
Extraction raffinate extract and separate yttrium lutetium again.Extraction raffinate using ion exchange chromatography come separating yttrium lutetium, first by rare earth ion
Adsorb on adsorption column, then using 200 DEG C of high temperature and the method for combined use of 25 DEG C of normal temperature drip washing, with eluent is in adsorption column and divides
The drip washing on post, it is different using eluent drip washing sequencing, the effect of separating yttrium and lutetium is reached, drip washing is respectively obtained containing yttrium
Solution and the solution containing lutetium, respectively with oxalic acid precipitation after, in 950 DEG C of calcinations, respectively obtain yittrium oxide and luteium oxide, yittrium oxide,
Luteium oxide purity is up to 4N.
Cerium, yttrium, lutetium and silicic acid are separately recovered and are carried by the present invention from Extraction of rare earth element in the yttrium luetcium silicate crystal for mix cerium
Pure, resulting product purity is high, realizes recycling for rare earth element, effectively reduces production cost, improves the city of product
Field competitiveness.
Although being example purpose, the preferred embodiment of the present invention, the ordinary skill people of this area are had been disclosed for
Member will be various to change, it is realized that disclosed in without departing from by appending claims in the case of scope and spirit of the present invention
It is possible for entering, increasing and replacing.
Claims (10)
1. a kind of method of the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium, it is characterised in that：It comprises the steps：
Step S1：The yttrium luetcium silicate crystal fracture of cerium will be mixed, sieving obtains powder；
Step S2：Above-mentioned powder is added in aqueous slkali, then carries out roasting and obtain product of roasting；
Step S3：Above-mentioned product of roasting is washed and filtered, the first filtrate and the first precipitation is obtained；
Step S4：Add acid for adjusting pH to be settled out silicic acid the first filtrate, silicic acid calcination is obtained into silica；
Step S5：First precipitation is carried out into acid adding, dissolving, oxidation, pH precipitations or extraction separation of quadravalence cerium ion is adjusted, obtains remaining
Liquid；
Step S6：Extraction raffinate is carried out into the operation of separating yttrium, lutetium.
2. the method for the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium according to claim 1, it is characterised in that：
Crystal fracture mode is first Mechanical Crushing in step S1, then levigate with ball mill.
3. the method for the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium according to claim 1, it is characterised in that：
Powder is added in step S2 is mixed and stirred in aqueous slkali uniformly, the solute of aqueous slkali is 1 with the mass ratio of powder:1
～1:5, then roasting, 100～300 DEG C of sintering temperature, roasting time 1～5 hour.
4. the method for the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium according to claim 1, it is characterised in that：
Water temperature is 30～100 DEG C when washing in step S3, washing time 1～4 hour, and water-washing method is to wash while stirring.
5. the method for the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium according to claim 1, it is characterised in that：
Add acid for adjusting pH to silicic acid is settled out between 4～5 to the first filtrate in step S4, afterwards by silicic acid at 600～1000 DEG C
Under the conditions of calcination obtain silica.
6. the method for the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium according to claim 1, it is characterised in that：
In step S5 after control oxidation between the pH to 3～4 of solution, quadrivalent cerium is then precipitated out in the form of cerium hydroxide, mistake
Filter obtains cerium hydroxide precipitation and extraction raffinate, and cerium hydroxide is precipitated into the oxide that roasting obtains cerium.
7. the method for the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium according to claim 1, it is characterised in that：
Tetravalence cerium ion is extracted in solution from after oxidation with extractant P204 in step S5, with hydrochloric acid tetravalence cerium ion from organic
Oxalic acid precipitation, then calcination is added to obtain the oxide of cerium under Xiang Zhongxi again.
8. the method for the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium according to claim 1, it is characterised in that：
Step S6 is according to following steps separating yttrium lutetium：Using two step extraction system separating yttriums：Extraction raffinate adopts N263- heavy solvent-RE
(NO3)3-LiNO3System and N263- heavy solvent-RECl3-NH4CNS system fractional extraction yttriums, obtain the Jing again of the raffinate containing yttrium
After oxalic acid precipitation, calcining obtains yittrium oxide, is the extract containing lutetium in organic phase, after sour back extraction, reprecipitation simultaneously ignition precipitate
Obtain luteium oxide.
9. the method for the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium according to claim 1, it is characterised in that：
Step S6 is according to following steps separating yttrium lutetium：With extractant separating and extracting yttrium：Allocate extraction raffinate is to rare earth ion total concentration
Between 1.5～3.5, the extractant for adopting is aphthenic acids-mixed alcohol-kerosene, and is carried out with alkali lye for 0.2～2.5mol/L, pH
Saponification, saponification degree is 60～90%, uses VHaveRepresent organic extractant, VMaterialRepresent material liquid volume, VWashWashing lotion volume is represented, stream ratio is
VHave：VMaterial：VWash=4～10:1:1～3, the water after separating and extracting is mutually exported and obtains pure yttrium solution, and organic phase concentration is 1～5mol/
L salt acid elutions, after multitple extraction and washing make the yttrium in organic phase return to water phase, organic phase is then the extract containing lutetium,
Again back extraction is carried out with acid, obtain the strip liquor of lutetium, then use oxalic acid precipitation respectively, precipitation 700～1000 DEG C of calcinations of Jing are aoxidized
Yttrium and luteium oxide.
10. the method for the Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium according to claim 1, its feature exists
In：Step S6 is according to following steps separating yttrium lutetium：Extraction raffinate using ion exchange chromatography come separating yttrium lutetium, first will be dilute
Native ion adsorbs on adsorption column, then using the method for combined use of drip washing under different temperatures, with eluent in adsorption column and separation
Drip washing on post, different using eluent drip washing sequencing, drip washing respectively obtains the solution containing yttrium and the solution containing lutetium, uses respectively
After oxalic acid precipitation, in 700～1000 DEG C of calcinations, yittrium oxide and luteium oxide are respectively obtained.
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