CN110372027A - A kind of method that chloride system precipitates low chlorine root luteium oxide - Google Patents
A kind of method that chloride system precipitates low chlorine root luteium oxide Download PDFInfo
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- CN110372027A CN110372027A CN201910768391.4A CN201910768391A CN110372027A CN 110372027 A CN110372027 A CN 110372027A CN 201910768391 A CN201910768391 A CN 201910768391A CN 110372027 A CN110372027 A CN 110372027A
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 52
- 239000000460 chlorine Substances 0.000 title claims abstract description 34
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000002244 precipitate Substances 0.000 title claims abstract description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 150
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 50
- 239000007788 liquid Substances 0.000 claims abstract description 41
- 230000001376 precipitating effect Effects 0.000 claims abstract description 33
- 238000005406 washing Methods 0.000 claims abstract description 31
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims abstract description 26
- YQAQUOLVUCJCHH-UHFFFAOYSA-N lutetium;oxalic acid Chemical compound [Lu].OC(=O)C(O)=O YQAQUOLVUCJCHH-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 21
- 239000013049 sediment Substances 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 14
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 13
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000047 product Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000006298 dechlorination reaction Methods 0.000 claims abstract description 12
- 238000001556 precipitation Methods 0.000 claims abstract description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 9
- 239000012498 ultrapure water Substances 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 3
- 210000003298 dental enamel Anatomy 0.000 description 13
- 239000013078 crystal Substances 0.000 description 12
- 238000000746 purification Methods 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- -1 oxonium ion Chemical class 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 229910052765 Lutetium Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000002591 computed tomography Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- NIDNOXCRFUCAKQ-UMRXKNAASA-N (1s,2r,3s,4r)-bicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1[C@H]2C=C[C@@H]1[C@H](C(=O)O)[C@@H]2C(O)=O NIDNOXCRFUCAKQ-UMRXKNAASA-N 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009509 drug development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002547 new drug Substances 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- AHKZTVQIVOEVFO-UHFFFAOYSA-N oxide(2-) Chemical compound [O-2] AHKZTVQIVOEVFO-UHFFFAOYSA-N 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000026676 system process Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
- C01F17/271—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of methods that chloride system precipitates low chlorine root luteium oxide, comprising the following steps: (1) feed liquid is prepared: the LuCl for being 0.1 ~ 0.8 mol/L by concentration3Solution and concentrated nitric acid solution mix to form the stable feed liquid of concentration, and the nitrate concentration in feed liquid is 0.3 ~ 2.0mol/L；(2) precipitating reagent is prepared: being used concentration for the oxalic acid solution of 120 ~ 150g/L, is heated to solid oxalic acid in oxalic acid solution and is completely dissolved, so that precipitating reagent be made；(3) precipitating dechlorination root: parallel-flow precipitation mode is used, bottom water, above-mentioned feed liquid and above-mentioned precipitating reagent are precipitated in temperature in 35 ~ 60 DEG C of hybrid reactions, stoichiometric ratio n (lutecium chloride): n (oxalic acid)=1:(1.65 ~ 1.95 of the lutecium chloride and oxalic acid that put into reaction)；(4) washing dechlorination root: sediment oxalic acid lutetium is washed；(5) calcination: obtaining low chlorine root luteium oxide product for the sediment oxalic acid lutetium calcination after washing, and preventing from occurring in oxalic acid lutetium precipitation process chloride ion package and powder reuniting causes impurity higher.
Description
Technical field
The invention belongs to rare earth material fields, are related to a kind of method that chloride system precipitates low chlorine root luteium oxide, are one
The preparation method of kind rare earth oxide.
Background technique
Positron e mission computed tomography (Positron Emission Computed Tomography, PET)
System is widely used in the Diagnosis and differential diaggnosis of a variety of diseases, state of an illness judgement, therapeutic evaluation, organ function research and new drug development
Etc..In PET system, scintillation crystal spontaneous radiation reasons for its use event, non-genuine random coincidence event and scattering symbol
Ambient noise caused by conjunction event is likely to cause large effect to signal noise ratio (snr) of image.Therefore, PET system would generally adopt
Guarantee signal noise ratio (snr) of image with the following method: reduce spontaneous radiation and improve system capacity resolution ratio etc..In these methods, improve
The quality index of scintillation crystal is that a kind of approach is solved the problems, such as from source.
Most commonly used rare earth scintillating crystals are Lu in PET system2SiO5: Ce (LSO:Ce) and (LuxY1–x)2SiO5:Ce
(LYSO:Ce).In both crystal, luteium oxide is main host material component part, and occupy crystal weight 80% is left
It is right.For LSO the or LYSO scintillation crystal for obtaining higher performance, manufacturing enterprise requires also increasingly the quality index of luteium oxide
Strictly.Influence of the foreign ion to crystal property in luteium oxide product is also especially important, according to pertinent literature, impurity from
Son will have a direct impact on the light output of rare earth scintillating crystals LSO or LYSO, influence PET testing efficiency, and major impurity in luteium oxide
Ion is chloride ion, and chloride ion is minus 1 valence, and oxonium ion is negative divalent in rare earth scintillating crystals LSO or LYSO, and luteium oxide is used
During making scintillation crystal, chloride ion can substitute oxonium ion, cause crystal defect, influence crystal property.
Currently, luteium oxide precipitated using chloride content in the luteium oxide of precipitation method preparation all in 100 ~ 200ug/g or so
Easily occur the case where chlorine root package in journey, leads to after burning that chlorine root is higher in luteium oxide.And use luteium oxide through nitric acid weight molten two
Secondary precipitating, will lead to product yield reduce, increased costs the problems such as.Therefore, how to realize that luteium oxide material quality index becomes
Many rare earths material producers wish the significant technology issues solved.
Summary of the invention
The purpose of the present invention is to provide a kind of methods that chloride system precipitates low chlorine root luteium oxide, can effectively prevent
The problem of will appear chloride ion package in oxalic acid lutetium precipitation process and powder reuniting lead to the higher problem of impurity.
To achieve the above object, the invention adopts the following technical scheme:
A kind of method that chloride system precipitates low chlorine root luteium oxide, comprising the following steps: (1) feed liquid is prepared: being 0.1 by concentration
The LuCl of ~ 0.8 mol/L3Solution and concentrated nitric acid solution mix to form the stable feed liquid of concentration, wherein the nitre in feed liquid
Acid group concentration is 0.3 ~ 2.0mol/L；(2) precipitating reagent is prepared: being used concentration for the oxalic acid solution of 120 ~ 150g/L, is heated to grass
Solid oxalic acid is completely dissolved in acid solution, so that required precipitating reagent be made；(3) precipitating dechlorination root: using parallel-flow precipitation mode, will
Bottom water, above-mentioned feed liquid and above-mentioned precipitating reagent are precipitated in temperature in 35 ~ 60 DEG C of hybrid reactions, the lutecium chloride and oxalic acid for putting into reaction
Stoichiometric ratio be n (lutecium chloride): n (oxalic acid)=1:(1.65 ~ 1.95)；(4) washing dechlorination root: by sediment oxalic acid lutetium into
Row washing；(5) the sediment oxalic acid lutetium calcination after washing calcination: is obtained into low chlorine root luteium oxide product.
Mass ratio < 20ug/g of the quality of impurity and oxalic acid solution in oxalic acid solution.
The volume of the bottom water is 2 ~ 3 times of material liquid volume.
Sediment oxalic acid lutetium in step (5) after the washing calcination 3h under 950 ~ 1100 DEG C of environment.
5min is aged before the washing of sediment oxalic acid lutetium in step (4).
Sediment oxalic acid lutetium uses 50 ~ 65 DEG C of high-purity water washing in step (4), until detection washs oxalic acid lutetium through lautertuns
Filtrate pH > 6 after stop washing.
By adopting the above technical scheme, the present invention is mixed with lutecium chloride by a certain concentration as feed liquid by nitric acid, reduces chlorine
Ion and lutetium ion match, and by lutecium chloride concentration, concentration of oxalic acid configuration in a certain range, at the same by control feed liquid temperature,
Oxalic acid temperature and bottom water temperature are stablized with reaching the entire precipitation system process temperature of control, effectively prevent in oxalic acid lutetium precipitation process
In the problem of will appear chloride ion package, via detecting Cl content < 20ppm in low chlorine root luteium oxide product produced by the present invention,
To illustrate the present invention can solve can occur in rare earth chloride precipitation process chlorine root package and powder reuniting cause impurity higher
Problem simplifies process.The present invention has technology controlling and process simple, and at low cost, yield is big, and product impurity is low, and easily industrialization etc. is excellent
Point.
Specific embodiment
Below with reference to embodiment, invention is further described in detail.
Embodiment 1
Present invention discloses a kind of methods that chloride system precipitates low chlorine root luteium oxide, comprising the following steps:
(1) feed liquid is prepared: concentration is 0.5mol/L and volume is 0.5m3LuCl32m is added in solution3In container, add
The concentrated nitric acid solution of the concentration 65% ~ 68% of 51.7L mixes to form the stable feed liquid of concentration, that is, after mixing 1 hour, inspection
The calculated value deviation for surveying the concentration of the concentration and lutecium chloride of lutecium chloride in feed liquid is no more than 0.02mol/L, just steady to form concentration
Fixed feed liquid, in this present embodiment, the calculated value of the concentration of lutecium chloride are that 0.437mol/L detects the dense of solution after stirring 1h
Degree is 0.417 ~ 0.457mol/L, that is, is judged to being uniformly mixed.Wherein the nitrate concentration in feed liquid is 1.359mol/L, n
(Lu3+): n(NO3 -)=1:3, in this present embodiment, 65% ~ 68% concentrated nitric acid molar concentration is about 14.5mol/L.Wherein, n (Lu3 +)=0.5mol/L* 500L=250mol, n(NO3 -)=51.7L*14.5mol/L=750mol。
(2) precipitating reagent is prepared: using concentration for the purification oxalic acid solution of 135g/L, the volume for refining oxalic acid solution is
0.42m3, wherein Fe, Ca, SO4 2-The quality of equal impurity and mass ratio < 20ug/g of purification oxalic acid solution, temperature are heated to 40 DEG C
Left and right is completely dissolved the solid oxalic acid in oxalic acid solution, so that required precipitating reagent be made.
(3) precipitating dechlorination root: can be toward 5m31.2m is added in enamel clarifying kettle3High purity water, temperature are controlled at 40 DEG C or so,
Bottom water is made, above-mentioned feed liquid and precipitating reagent are added simultaneously in enamel clarifying kettle using parallel-flow precipitation mode, using Electromagnetic Flow
It is 16.67L/min that meter, which controls to adjust feed liquid flow, and precipitating agent flux is 23L/min, and above-mentioned configuration honest material liquid, precipitating reagent is complete
Portion is transferred in enamel clarifying kettle, the stoichiometric ratio of the lutecium chloride and oxalic acid that put into reaction are as follows: n (lutecium chloride): n (oxalic acid)=
1:1.8, wherein the oxalic acid molar concentration of 135g/L is 135/126.06=1.07mol/L, n (lutecium chloride)=0.5mol/L *
500L=250mol, n (oxalic acid)=1.07mol/L*420L=449mol, n (lutecium chloride): n (oxalic acid)=250/449=1:1.8.
(4) washing dechlorination root: after the reaction was completed, it is aged 5min, sediment oxalic acid lutetium in enamel clarifying kettle is put to filtering
Trough washery.Using 55 DEG C of high-purity water washings, until detection stops washing behind filtrate pH > 6 of lautertuns washing oxalic acid lutetium.
(5) it calcination: by the sediment oxalic acid lutetium after washing after 1000 DEG C of calcination 3h of electrical kiln, obtains low chlorine root luteium oxide and produces
Product.
Cl content < 20ppm in low chlorine root luteium oxide product is detected, to illustrate to sink using chloride system of the invention
It forms sediment the method for low chlorine root luteium oxide, can prevent chloride ion package problem and powder reuniting leads to the higher problem of impurity.
Embodiment 2
(1) feed liquid is prepared: concentration is 0.35mol/L and volume is 0.8m3LuCl32m is added in solution3In container, add
The concentrated nitric acid solution of the concentration 65% ~ 68% of 57.9L mixes to form the stable feed liquid of concentration, that is, after mixing 1 hour, inspection
The calculated value deviation for surveying the concentration of the concentration and lutecium chloride of lutecium chloride in feed liquid is no more than 0.02mol/L, just steady to form concentration
Fixed feed liquid.Wherein the nitrate concentration in feed liquid is 0.978mol/L, n (Lu3+): n(NO3 -)=1:3, wherein n (Lu3+)=
0.35mol/L*800L=280mol, n(NO3 -)=14.5mol/L * 57.9L=840mol, thus n (Lu3+): n(NO3 -)=1:3.
(2) precipitating reagent is prepared: using concentration for the purification oxalic acid solution of 120g/L, the volume for refining oxalic acid solution is
0.485m3, wherein Fe, Ca, SO4 2-The quality of equal impurity and mass ratio < 20ug/g of purification oxalic acid solution, temperature are heated to 35
DEG C or so make refine oxalic acid solution in solid oxalic acid be completely dissolved, so that required precipitating reagent be made.
(3) precipitating dechlorination root: can be toward 5m32m is added in enamel clarifying kettle3High purity water, temperature are controlled at 35 DEG C or so, system
At bottom water, above-mentioned feed liquid and precipitating reagent are added simultaneously in enamel clarifying kettle using parallel-flow precipitation mode, using electromagnetic flowmeter
Control and regulation feed liquid flow is 26.67L/min, and precipitating agent flux is 16.17L/min, and above-mentioned configuration honest material liquid, precipitating reagent is complete
Portion is transferred in enamel clarifying kettle, makes the chemistry of the Chlorine in Solution lutetium for not having precipitating in the enamel clarifying kettle of reaction end and oxalic acid
Measure ratio are as follows: n (lutecium chloride): n (oxalic acid)=1:1.65, in this present embodiment, the oxalic acid molar concentration of 120g/L are 120/
126.06=0.952mol/L, n (lutecium chloride)=0.35mol/L*800L=280mol, n (oxalic acid)=0.952mol/L*485L=
462mol, n (lutecium chloride): n (oxalic acid)=280/462=1:1.65.
(4) washing dechlorination root: after the reaction was completed, it is aged 5min, sediment oxalic acid lutetium in enamel clarifying kettle is put to filtering
Trough washery.Stop washing behind filtrate pH > 6 of lautertuns washing oxalic acid lutetium using 50 DEG C of high-purity water washings to detection.
(5) it calcination: by the sediment oxalic acid lutetium after washing after 1100 DEG C of calcination 3h of electrical kiln, obtains low chlorine root luteium oxide and produces
Product.
Cl content < 20ppm in low chlorine root luteium oxide product is detected, to illustrate to sink using chloride system of the invention
It forms sediment the method for low chlorine root luteium oxide, can prevent chloride ion package problem and powder reuniting leads to the higher problem of impurity.
Embodiment 3
(1) feed liquid is prepared: concentration is 0.8mol/L and volume is 0.5m3LuCl32m is added in solution3In container, add
The concentrated nitric acid solution of the concentration 65% ~ 68% of 82.75L mixes to form the stable feed liquid of concentration, that is, after mixing 1 hour, inspection
The concentration and calculated value deviation for surveying lutecium chloride in feed liquid are no more than 0.02mol/L, just the feed liquid stable for formation concentration.Wherein
Nitrate concentration in feed liquid is 2.0mol/L, n (Lu3+): n(NO3 -)=1:3, wherein n (Lu3+)=0.8mol/L*500L=
400mol, n(NO3 -)=14.5mol/L * 82.75L=1200mol, thus n (Lu3+): n(NO3 -)=1:3.
(2) precipitating reagent is prepared: using concentration for the purification oxalic acid solution of 150g/L, the volume for refining oxalic acid solution is
0.655m3, wherein Fe, Ca, SO4 2-The quality of equal impurity and mass ratio < 20ug/g of purification oxalic acid solution, temperature are heated to 50
DEG C or so make refine oxalic acid solution in solid oxalic acid be completely dissolved, so that required precipitating reagent be made.
(3) precipitating dechlorination root: can be toward 5m32m is added in enamel clarifying kettle3High purity water, temperature are controlled at 50 DEG C or so, system
At bottom water, above-mentioned feed liquid and precipitating reagent are added simultaneously in enamel clarifying kettle using parallel-flow precipitation mode, using electromagnetic flowmeter
Control and regulation feed liquid flow is 16.7L/min, and precipitating agent flux is 21.83L/min, and above-mentioned configuration honest material liquid, precipitating reagent is complete
Portion is transferred in enamel clarifying kettle, the stoichiometric ratio of the lutecium chloride and oxalic acid that put into reaction are as follows: n (lutecium chloride): n (oxalic acid)=
1:1.95, in this present embodiment, the oxalic acid molar concentration of 150g/L is 150/126.06=1.19mol/L, n (lutecium chloride)=
0.8mol/L*500L=400mol, n (oxalic acid)=1.19mol/L*655L=780mol, n (lutecium chloride): n (oxalic acid)=400/780
=1:1.95。
(4) washing dechlorination root: after the reaction was completed, it is aged 5min, sediment oxalic acid lutetium in enamel clarifying kettle is put to filtering
Trough washery.Stop washing behind filtrate pH > 6 of lautertuns washing oxalic acid lutetium using 60 DEG C of high-purity water washings to detection.
(5) it calcination: by the sediment oxalic acid lutetium after washing after 950 DEG C of calcination 3h of electrical kiln, obtains low chlorine root luteium oxide and produces
Product.
Cl content < 20ppm in low chlorine root luteium oxide product is detected, to illustrate to sink using chloride system of the invention
It forms sediment the method for low chlorine root luteium oxide, can prevent chloride ion package problem and powder reuniting leads to the higher problem of impurity.
Technology contents and technical characterstic of the invention have revealed that as above, composition of the invention is not limited with above-mentioned, ability
The technical staff in domain is still potentially based on announcement of the invention and makees various replacements and modification without departing substantially from creation spirit of the present invention.Cause
This, protection scope of the present invention should be not limited to disclosed in embodiment, and should include it is various without departing substantially from replacement and modification of the invention,
And covered by claims.
Claims (6)
1. a kind of method that chloride system precipitates low chlorine root luteium oxide, which comprises the following steps:
(1) feed liquid is prepared: the LuCl for being 0.1 ~ 0.8 mol/L by concentration3Solution and concentrated nitric acid solution mix to form concentration
Stable feed liquid, wherein the nitrate concentration in feed liquid is 0.3 ~ 2.0mol/L；
(2) precipitating reagent is prepared: using concentration for the oxalic acid solution of 120 ~ 150g/L, it is complete to be heated to solid oxalic acid in oxalic acid solution
Dissolution, so that required precipitating reagent be made；
(3) precipitating dechlorination root: parallel-flow precipitation mode is used, by bottom water, above-mentioned feed liquid and above-mentioned precipitating reagent in temperature at 35 ~ 60 DEG C
Hybrid reaction precipitating, make reaction put into lutecium chloride and oxalic acid stoichiometric ratio n (lutecium chloride): n (oxalic acid)=1:(1.65 ~
1.95)；
(4) washing dechlorination root: sediment oxalic acid lutetium is washed；
(5) the sediment oxalic acid lutetium calcination after washing calcination: is obtained into low chlorine root luteium oxide product.
2. a kind of method that chloride system precipitates low chlorine root luteium oxide according to claim 1, it is characterised in that: oxalic acid is molten
Mass ratio < 20ug/g of the quality of impurity and oxalic acid solution in liquid.
3. a kind of method that chloride system precipitates low chlorine root luteium oxide according to claim 1, it is characterised in that: the bottom
The volume of water is 2 ~ 3 times of material liquid volume.
4. a kind of method that chloride system precipitates low chlorine root luteium oxide, feature exist according to any one of the claim 1 to 3
Sediment oxalic acid lutetium in: step (5) after the washing calcination 3h under 950 ~ 1100 DEG C of environment.
5. a kind of method that chloride system precipitates low chlorine root luteium oxide according to claim 1, it is characterised in that: step
(4) 5min is aged before the washing of sediment oxalic acid lutetium in.
6. according to claim 1 or a kind of 5 methods that chloride system precipitates low chlorine root luteium oxide, it is characterised in that: step
Suddenly sediment oxalic acid lutetium uses 50 ~ 65 DEG C of high-purity water washing in (4), until detecting filtrate pH > 6 through lautertuns washing oxalic acid lutetium
Stop washing afterwards.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111874937A (en) * | 2019-12-27 | 2020-11-03 | 广西国盛稀土新材料有限公司 | Preparation method of low-chlorine lutetium oxide |
| CN115536053A (en) * | 2022-10-29 | 2022-12-30 | 中稀(广西)金源稀土新材料有限公司 | Preparation method of low-chloride high-purity lutetium oxide |
| CN115961157A (en) * | 2022-12-28 | 2023-04-14 | 江西离子型稀土工程技术研究有限公司 | Method for removing thorium from lutetium-containing feed liquid |
| CN117446851A (en) * | 2023-12-26 | 2024-01-26 | 全南县新资源稀土有限责任公司 | High-purity low-aluminum gadolinium oxide and preparation method thereof |
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| CN101780970A (en) * | 2010-02-04 | 2010-07-21 | 包头稀土研究院 | Method for preparing rare earth oxide with large particles |
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| CN101780970A (en) * | 2010-02-04 | 2010-07-21 | 包头稀土研究院 | Method for preparing rare earth oxide with large particles |
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| CN117446851B (en) * | 2023-12-26 | 2024-03-19 | 全南县新资源稀土有限责任公司 | High-purity low-aluminum gadolinium oxide and preparation method thereof |
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