CN109852804A - A kind of circulation utilization method of rare earth silicate scintillation crystal - Google Patents
A kind of circulation utilization method of rare earth silicate scintillation crystal Download PDFInfo
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- CN109852804A CN109852804A CN201910096095.4A CN201910096095A CN109852804A CN 109852804 A CN109852804 A CN 109852804A CN 201910096095 A CN201910096095 A CN 201910096095A CN 109852804 A CN109852804 A CN 109852804A
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The present invention relates to a kind of circulation utilization method of rare earth silicate scintillation crystal, the present invention leaches scintillation crystal waste after melting, and leachate can prepare the raw materials for production of rare earth silicate scintillation crystal directly as solid phase method or wet process.The present invention can be realized rare earth element recycling in scintillation crystal production process by this quick-reading flow sheets, avoid the Complicated Flow and material consumption energy consumption for carrying out Rare Earth Separation after obtaining rare-earth enrichment liquid in traditional recovery process again.The present invention uses solid base melt process silicate scintillation crystal, and rare earth element leaching rate is high, and element ratio is identical with raw materials for production in leachate.The present invention is by selecting suitable leach to use acid and condition, the introducing of impurity during reducing；And leachate is further purified by the optimization to precipitation process precipitating reagent and deposition condition, final gained mixed rare-earth oxide product purity is high, meets scintillation crystal production requirement.
Description
Technical field
The present invention relates to the processing of rare earth silicate scintillation crystal and preparation technical fields, and in particular to a kind of rare earth silicic acid
The circulation utilization method of salt scintillation crystal.
Background technique
Rare earth silicate (RE2SiO5: Ce (RE=Y, Gd, Lu)) high-energy ray/particle can be converted to purple by scintillation crystal
Outer or visible fluorescence pulse has high density, High Light Output and the excellent properties such as die-away time is short, is widely used in high energy object
The fields such as reason, nuclear physics, nuclear medicine and safety detection.Especially mix cerium yttrium luetcium silicate scintillation crystal (Lu2SiO5: Ce) it has become
The indispensable critical component of positron emission tomography (PET-CT).In scintillation crystal preparation process, raw material oxidation
Lutetium (Lu2O3) due in mineral content it is low, hardly possible separation, yield is few, expensive, constitutes the main of scintillation crystal production cost
Part.In scintillation crystal production process, there is about 50% or more lutetium (Lu) because cutting, crystal defect and other reasons become useless
Gurry restricts its application development so that crystal production cost further increases.If the lutetium that can be discarded to this part recycles
The preparation cost that can then substantially reduce scintillation crystal is recycled, is promoted and applied, while reducing solid waste and stacking the shadow caused by environment
It rings.
Main technology to be used has in rare earth scintillating crystals recycling field at present: in Publication No. CN103436719A
State's patent discloses a kind of from mixing the luteium oxide and recovery method recycled in Cerium aluminate lutetium scintillation crystal waste, uses following work
Skill: sodium hydroxide and/or potassium hydroxide S1, are added into scintillation crystal waste, roasting obtains calcining matter；S2, by calcining matter into
Row water logging, filtering, and nitric acid and oxidant are added into obtained filter residue, stirring obtains mixed liquor；S3, mixed liquor is added
Into organic extractant, extraction obtains the extract containing cerium and the raffinate containing lutetium；And S4, into the raffinate containing lutetium plus
Enter oxalic acid, stir, filtering, the sediment calcination that will be obtained obtains luteium oxide, and Cerium aluminate lutetium is mixed in recycling.Publication No.
The Chinese patent of CN106636685A discloses a kind of method of Extraction of rare earth element from the yttrium luetcium silicate crystal for mix cerium, uses
Following technique: it step S1: is sieved the yttrium luetcium silicate crystal fracture for mixing cerium to obtain powder；Step S2: above-mentioned powder is added
In aqueous slkali, then roasted to obtain product of roasting；Step S3: above-mentioned product of roasting is washed and is filtered, obtains first
Filtrate and the first precipitating；Step S4: adding acid for adjusting pH to be settled out silicic acid the first filtrate, and silicic acid calcination is obtained silica；Step
Rapid S5: the first precipitating is subjected to acid adding, dissolution, oxidation, pH precipitating or extraction separation of quadravalence cerium ion are adjusted, remaining as extraction raffinate；
Extraction raffinate: being carried out the operation of separating yttrium, lutetium by step S6, recycles yttrium luetcium silicate.The Chinese patent of Publication No. CN106191478A
A kind of recovery method of lutetium element is disclosed, using " will contain lutetium waste material and be uniformly mixed and heat with sulfuric acid and/or nitric acid；Again
Resulting product is leached, Element Solution containing lutetium is obtained " method recycle scintillation crystal containing lutetium.
Current recycling method mostly first dissolves out scintillation crystal waste with soda acid, then passes through the methods of liquid-liquid extraction point again
The single rare earths product such as pure lutetium, cerium, yttrium is obtained from leachate.This kind of recovery process is long and complicated, gained rare earth oxide
If being re-used for crystal manufacture also to need to re-mix.If recycling product and scintillation crystal raw materials for production can be combined,
It can be to avoid this problem.The main method of rare earth silicate scintillation crystal preparation is czochralski method, which utilizes rare earth silicate
Polycrystal powder grows monocrystal material.Polycrystal powder can be synthesized by high temperature solid-state method, or with the method for liquid phase, such as homogeneous coprecipitation
Method synthesis.Rare earth partition is identical as raw materials for production in scintillation crystal waste, is hopeful by optimizing recovery process, in former ratio
Leachate is recycled from scintillation crystal waste or mixed rare-earth oxide is used for the preparation of rare earth silicate polycrystal powder.In this way
Can no longer need to realize by element sepatation rare earth entire rare earth silicate scintillation crystal production, discard, recycle this all one's life
Recycling in the life period.
Summary of the invention
The object of the present invention is to provide a kind of circulation utilization methods of rare earth silicate scintillation crystal.The present invention is that realization is dilute
Conversion process of the earth elements from waste material to raw material is difficult to be directly dissolved in the feature of acid for rare earth silicate scintillation crystal, this
The technical treatment rare earth silicate scintillation crystal of acidleach after invention is roasted using alkaline process.Gained re dip solution can be through ignition of precipitate
Mixed rare-earth oxide is obtained, then prepares rare earth silicate polycrystal powder with high temperature solid-state method, or prepare rare earth for wet process
Silicate polycrystal powder.
To achieve the goals above, technical solution of the present invention is specific as follows:
A kind of circulation utilization method of rare earth silicate scintillation crystal, comprising the following steps:
Rare earth silicate scintillation crystal fragment is crushed to 80-300 mesh powder with ball mill by step 1；
Step 2, the rare earth silicate scintillation crystal powder 1:4-4:1 in mass ratio for obtaining solid alkali and step 1 are equal
Even mixing is placed in graphite crucible with Muffle furnace high-temperature roasting, has roasted after taking-up that substance is solid-state in crucible；
Step 3, will have been roasted in step 2 after solid crush after with inorganic mineral acid that concentration is 0.1-5mol/L by solid
Liquor ratio is 1:10-1:30 reaction；
Step 4 is reacted 30 minutes at 10-90 DEG C -- after 5 hours, rare-earth enrichment feed liquid is obtained by filtration in acquired solution,
The rate of recovery is in 60-98%；Rare earth element mass fraction is 95% or more in this feed liquid；
Step 5, using step 4 gained rare-earth enrichment feed liquid as raw material, rare earth silicate is prepared using solid phase method or wet process
Scintillation crystal.
In the above-mentioned technical solutions, the rare earth silicate scintillation crystal fragment is LYSO:Ce, YSO:Ce or LSO:Ce.
In the above-mentioned technical solutions, the solid alkali is NaOH, Na2O, CaO or KOH.
In the above-mentioned technical solutions, the inorganic mineral acid is hydrochloric acid, nitric acid or sulfuric acid.
In the above-mentioned technical solutions, the temperature of step 2 high temperature calcining is 400-900 DEG C, and the time is 2-5 hours.
In the above-mentioned technical solutions, step 5 prepares rare earth silicate scintillation crystal specific step is as follows using solid phase method:
It is 0.001-1mol/L by gained rare-earth enrichment feed liquid adjusts Acidity Range in step 4, with oxalic acid or its salt, carbonic acid
Salt or alkali amine anion are precipitated in the ratio that rare earth ion molar ratio is 1:1-4:1, and gained is deposited in Muffle furnace and is used
800-1100 DEG C of temperature calcination obtains mixed rare-earth oxide product；
By above-mentioned gained mixed rare-earth oxide product and SiO2It is uniformly mixed in mortar for 13:1-3:1 in mass ratio,
Then by hybrid solid in tube furnace nitrogen with obtained within calcining 1-7 hours under hydrogen mixed gas atmosphere in 1200-2000 DEG C it is dilute
Native silicate scintillation crystal.
In the above-mentioned technical solutions, the oxalates is potassium oxalate or sodium oxalate.
Step 5 can be found in Publication No. using the specific steps that wet process prepares rare earth silicate scintillation crystal
It is prepared by a kind of preparation method of cerium dopping rare earth silicate polycrystal powder disclosed in CN107880884A.
The beneficial effects of the present invention are:
The partition of rare earth oxide used in rare earth partition and production scintillation crystal in rare earth silicate scintillation crystal waste
Ratio is identical, and for this feature, the present invention leaches scintillation crystal waste after melting, and leachate can be directly as solid phase method
Or wet process prepares the raw materials for production of rare earth silicate scintillation crystal.By taking solid phase method as an example, rare-earth precipitation in leachate can be obtained
Mixed rare-earth oxide product is subsequently used for manufacture scintillation crystal.It can be realized rare earth element by this quick-reading flow sheets flashing
Recycling during crystal production avoids and carries out Rare Earth Separation after obtaining rare-earth enrichment liquid in traditional recovery process again
Complicated Flow and material consumption energy consumption.
The present invention uses solid base melt process silicate scintillation crystal, and rare earth element leaching rate is high, element in leachate
Ratio is identical with raw materials for production.
The present invention is by selecting suitable leach to use acid and condition, the introducing of impurity during reducing；And by heavy
Leachate is further purified in the optimization of shallow lake process precipitating reagent and deposition condition, final gained mixed rare-earth oxide product purity
Height meets scintillation crystal production requirement.
Detailed description of the invention
Invention is further described in detail with reference to the accompanying drawings and detailed description.
Fig. 1 is the XRD spectrum of rare earth silicate polycrystal powder；Wherein a is sample prepared by embodiment 6；B is embodiment 7
The sample of preparation.
Fig. 2 is excitation and the transmitting map of rare earth silicate polycrystal powder prepared by embodiment 7.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawing.
The present invention provides a kind of circulation utilization method of rare earth silicate scintillation crystal, comprising the following steps:
Rare earth silicate scintillation crystal fragment is crushed to 80-300 mesh powder with ball mill by step 1；
Step 2, the rare earth silicate scintillation crystal powder 1:4-4:1 in mass ratio for obtaining solid alkali and step 1 are equal
Even mixing, which is placed in graphite crucible, uses Muffle furnace high-temperature roasting, and temperature is 400-900 DEG C, and the time is 2-5 hours, has roasted and has taken
Substance is solid-state in crucible after out；
Step 3, will have been roasted in step 2 after solid crush after with inorganic mineral acid that concentration is 0.1-5mol/L by solid
Liquor ratio is 1:10-1:30 reaction；
Step 4 is reacted 30 minutes at 10-90 DEG C -- after 5 hours, rare-earth enrichment feed liquid is obtained by filtration in acquired solution,
The rate of recovery is in 60-98%；Rare earth element mass fraction is 95% or more in this feed liquid；
Step 5, using step 4 gained rare-earth enrichment feed liquid as raw material, rare earth silicate is prepared using solid phase method or wet process
Scintillation crystal；
Preparing rare earth silicate scintillation crystal using solid phase method, specific step is as follows:
It is 0.001-1mol/L by gained rare-earth enrichment feed liquid adjusts Acidity Range in step 4, with oxalic acid or its salt, carbonic acid
Salt or alkali amine anion are precipitated in the ratio that rare earth ion molar ratio is 1:1-4:1, and gained is deposited in Muffle furnace and is used
800-1100 DEG C of temperature calcination obtains mixed rare-earth oxide product；
By above-mentioned gained mixed rare-earth oxide product and SiO2It is uniformly mixed in mortar for 10:1-3:1 in mass ratio,
Then by hybrid solid in tube furnace nitrogen with obtained within calcining 1-7 hours under hydrogen mixed gas atmosphere in 1200-2000 DEG C it is dilute
Native silicate scintillation crystal.
It is public to can be found in Publication No. CN107880884A using the specific steps that wet process prepares rare earth silicate scintillation crystal
It is prepared by a kind of preparation method for the cerium dopping rare earth silicate polycrystal powder opened.
It is preferred that the rare earth silicate scintillation crystal fragment is LYSO:Ce, YSO:Ce or LSO:Ce.
It is preferred that the solid alkali is NaOH, Na2O, CaO or KOH.
It is preferred that the inorganic mineral acid is hydrochloric acid, nitric acid or sulfuric acid.
It is preferred that the oxalates is potassium oxalate or sodium oxalate.
Embodiment 1
LYSO:Ce crystal is struck and is placed in ball mill for fine grained chippings, pellet mass ratio is 1:1, and revolving speed 600rpm is obtained
The LYSO:Ce powder of 100 mesh.
Embodiment 2
Take 300 mesh LSO:Ce crystal powder of 5g in crucible with 5g potassium hydroxide after mixing in Muffle kiln roasting
500 DEG C roast 2 hours, take out after having reacted and are placed in 100mL 0.8mol/L HNO3In be stirred to react at 90 DEG C 40 minutes.Institute
Oxalic acid precipitation is used after obtaining solution filtering, then 950 DEG C calcination 1 hour in Muffle furnace.Content of rare earth is higher than in gained oxide
99%, the rate of recovery 85%.
Embodiment 3
Take 200 mesh LYSO:Ce crystal powder of 20g in crucible with 40g sodium hydroxide after mixing in Muffle furnace
450 DEG C roast 4 hours, take out after having reacted and are placed in 100mL 0.8mol/L HNO3In be stirred to react at 70 DEG C 40 minutes, institute
Oxalic acid precipitation is used after obtaining solution filtering, then 900 DEG C calcination 1 hour in Muffle furnace.Content of rare earth is higher than in gained oxide
99.9%, the rate of recovery 97.0%.
Embodiment 4
Take 200 mesh YSO:Ce crystal powder of 10g in crucible with 5g sodium oxide molybdena after mixing 900 DEG C in Muffle furnace
Roasting 3 hours, taking-up is placed in 80mL 3mol/L HCl after having reacted is stirred to react 1 hour at 80 DEG C.Acquired solution filtering
Oxalic acid precipitation is used afterwards, then 850 DEG C calcination 1 hour in Muffle furnace.Content of rare earth is higher than 99% in gained oxide, the rate of recovery
It is 95%.
Embodiment 5
Take 100 mesh YSO:Ce crystal powder of 10g in crucible with 15g sodium hydroxide after mixing 400 in Muffle furnace
DEG C roasting 5 hours, react after taking-up be placed in 80mL 3mol/L H2SO4In 30 minutes are stirred to react at 50 DEG C, acquired solution
Oxalic acid precipitation is used after filtering, then 900 DEG C calcination 1 hour in Muffle furnace.Content of rare earth is higher than 99.9% in gained oxide,
The rate of recovery is 85%.
Embodiment 6
Gained mixed rare-earth oxide 13g and 1g high-purity Si O in Example 22It is uniformly mixed in mortar, then in nitrogen
It is calcined 4 hours in gas and hydrogen mixed gas atmosphere in 1400 DEG C, obtains LSO:Ce.Referring to Fig. 1 it is found that the LSO:Ce polycrystal powder of preparation
Body is consistent with rare earth silicate scintillation crystal standard diagram.The photoluminescent property of gained polycrystal powder are as follows: excitation peak: 359nm, transmitting
Peak: 394nm, 419nm, 433nm, fluorescence lifetime: 35ns.
Embodiment 7
Gained mixed rare-earth oxide 6g and 1g high-purity Si O in Example 32It is uniformly mixed in mortar, then in nitrogen
It is calcined 5 hours in gas and hydrogen mixed gas atmosphere in 1500 DEG C, obtains LYSO:Ce.Referring to Fig. 1 it is found that the LYSO:Ce polycrystalline of preparation
Powder is consistent with rare earth silicate scintillation crystal standard diagram.The photoluminescent property of gained polycrystal powder are as follows: excitation peak: 359nm, hair
Penetrate peak: 392nm, 417nm, 442nm, fluorescence lifetime: 31ns, referring to fig. 2.
Embodiment 8
Gained mixed rare-earth oxide 3.5g and 1g high-purity Si O in Example 42It uniformly mixes in mortar, then exists
It is calcined 4 hours in nitrogen and hydrogen mixed gas atmosphere in 1600 DEG C, obtains YSO:Ce.The photoluminescent property of gained polycrystal powder are as follows: swash
Send out peak: 359nm, emission peak: 392nm, 418nm, 435nm, fluorescence lifetime: 51ns.
Embodiment 9
Gained mixed rare-earth oxide 5.5g and 1.5g high-purity Si O in Example 52It is uniformly mixed in mortar, then
It is calcined 5 hours in nitrogen and hydrogen mixed gas atmosphere in 1300 DEG C, obtains YSO:Ce.The photoluminescent property of gained polycrystal powder are as follows:
Excitation peak: 358nm, emission peak: 393nm, 416nm, 439nm, fluorescence lifetime: 55ns.
Technological parameter in above-described embodiment may be replaced by the arbitrary value in the range of above-mentioned restriction, not another here
One enumerates.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (7)
1. a kind of circulation utilization method of rare earth silicate scintillation crystal, which comprises the following steps:
Rare earth silicate scintillation crystal fragment is crushed to 80-300 mesh powder with ball mill by step 1；
Step 2 uniformly mixes the rare earth silicate scintillation crystal powder 1:4-4:1 in mass ratio that solid alkali is obtained with step 1
Conjunction is placed in graphite crucible with Muffle furnace high-temperature roasting, has roasted after taking-up that substance is solid-state in crucible；
Step 3, will have been roasted in step 2 after solid crush after with concentration be 0.1-5mol/L inorganic mineral acid by solid-to-liquid ratio
For 1:10-1:30 reaction；
After reacting -5 hours 30 minutes at 10-90 DEG C, rare-earth enrichment feed liquid, the rate of recovery is obtained by filtration in acquired solution by step 4
In 60-98%；Rare earth element mass fraction is 95% or more in this feed liquid；
Step 5, using step 4 gained rare-earth enrichment feed liquid as raw material, using solid phase method or wet process prepare rare earth silicate flashing
Crystal.
2. the circulation utilization method of rare earth silicate scintillation crystal according to claim 1, which is characterized in that the rare earth
Silicate scintillation crystal fragment is LYSO:Ce, YSO:Ce or LSO:Ce.
3. the circulation utilization method of rare earth silicate scintillation crystal according to claim 1, which is characterized in that the solid-state
Alkali be NaOH, Na2O, CaO or KOH.
4. the circulation utilization method of rare earth silicate scintillation crystal according to claim 1, which is characterized in that described inorganic
Mineral acid is hydrochloric acid, nitric acid or sulfuric acid.
5. the circulation utilization method of rare earth silicate scintillation crystal according to claim 1, which is characterized in that in step 2
The temperature of high-temperature calcination is 400-900 DEG C, and the time is 2-5 hours.
6. the circulation utilization method of rare earth silicate scintillation crystal described in -5 any one, feature exist according to claim 1
In step 5 use solid phase method prepares rare earth silicate scintillation crystal, and specific step is as follows:
It is 0.001-1mol/L that gained rare-earth enrichment feed liquid in step 4, which is adjusted Acidity Range, with oxalic acid or its salt, carbonate or
Alkali amine anion and rare earth ion are the ratio precipitating of 1:1-4:1 in molar ratio, and gained is deposited in Muffle furnace and uses 800-
1100 DEG C of temperature calcination obtains mixed rare-earth oxide product；
By above-mentioned gained mixed rare-earth oxide product and SiO2It is uniformly mixed in mortar for 13:1-3:1 in mass ratio, then
By hybrid solid in obtaining rare earth silicon within calcining 1-7 hours in 1200-2000 DEG C under nitrogen and hydrogen mixed gas atmosphere in tube furnace
Hydrochlorate scintillation crystal.
7. the circulation utilization method of rare earth silicate scintillation crystal according to claim 6, which is characterized in that the oxalic acid
Salt is potassium oxalate or sodium oxalate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110306059A (en) * | 2019-07-30 | 2019-10-08 | 江西省科学院应用化学研究所 | A method of rare earth in recycling cerium dopping yttrium luetcium silicate waste material |
| CN111977680A (en) * | 2020-09-10 | 2020-11-24 | 中国科学院长春应用化学研究所 | Preparation method of yttrium oxide lutetium cerium for scintillator crystal |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101377020A (en) * | 2008-02-25 | 2009-03-04 | 中国科学院上海硅酸盐研究所 | Rare earth silicates polycrystal material doped with Ce<3+> and preparing method thereof |
| CN108004410A (en) * | 2017-12-15 | 2018-05-08 | 清远先导材料有限公司 | A kind of extracting method of rare earth silicate crystals element |
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2019
- 2019-01-31 CN CN201910096095.4A patent/CN109852804A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101377020A (en) * | 2008-02-25 | 2009-03-04 | 中国科学院上海硅酸盐研究所 | Rare earth silicates polycrystal material doped with Ce<3+> and preparing method thereof |
| CN108004410A (en) * | 2017-12-15 | 2018-05-08 | 清远先导材料有限公司 | A kind of extracting method of rare earth silicate crystals element |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110306059A (en) * | 2019-07-30 | 2019-10-08 | 江西省科学院应用化学研究所 | A method of rare earth in recycling cerium dopping yttrium luetcium silicate waste material |
| CN110306059B (en) * | 2019-07-30 | 2020-12-25 | 江西省科学院应用化学研究所 | Method for recycling rare earth in cerium-doped lutetium yttrium silicate waste |
| CN111977680A (en) * | 2020-09-10 | 2020-11-24 | 中国科学院长春应用化学研究所 | Preparation method of yttrium oxide lutetium cerium for scintillator crystal |
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Application publication date: 20190607 |