CN108285166A - A kind of preparation method of ultrafine yttria - Google Patents
A kind of preparation method of ultrafine yttria Download PDFInfo
- Publication number
- CN108285166A CN108285166A CN201710012362.6A CN201710012362A CN108285166A CN 108285166 A CN108285166 A CN 108285166A CN 201710012362 A CN201710012362 A CN 201710012362A CN 108285166 A CN108285166 A CN 108285166A
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- preparation
- ultrafine yttria
- ultrafine
- yttria
- sediment
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- 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
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to a kind of preparation methods of ultrafine yttria, belong to the preparing technical field of rare earth compound, it is characterised in that：The medium particle diameter of the yttrium oxide is in 1.0 1.5um, and grain diameter is evenly distributed.The present invention has process conditions fairly simple, and industrialized production easy to implement, whole preparation process meets environmental requirement.
Description
Technical field
The present invention uses the precipitation method, makees precipitating reagent with oxalic acid, and anion surfactant is additive, precipitating rare earth from
Son, prepares ultra-fine, and the yttrium oxide of even particle size distribution belongs to a kind of material preparation process.
Background technology
Being widely used for rare earth oxide is general, especially plays an important role in fields such as glass, ceramics, electronics.With
The continuous development of science and technology, it is desirable that the rare earth oxide of production has specific physical chemistry form.Currently, market is to controllable grain size
The requirement of product obviously increase.
In many application scenarios, granular size and size distribution situation to RE oxide powder have more stringent
It is required that.Such as when yttrium oxide is applied in LED powder, to improve the brightness of product, dispersion is reduced, extends its service life, generally
It is required that the purity of yttrium oxide is 99.999%, medium particle diameter will reach 1.0-1.5um, and size distribution have to it is narrow, it is uniform.
The patent of Patent No. CN1195647A is provided one kind and is dissolved in formic acid with yttrium nitrate, hydrazine, gained mixture is then added
Yttrium oxide granularity after calcination is less than 1um, but such method is of high cost, and formic acid and hydrazine all have a certain impact to environmental protection, formic acid
Corrosivity is stronger, and sucking is excessive harmful.Contain ammonia nitrogen inside hydrazine, is unfavorable for producing.
Invention content
A kind of particle of present invention offer is uniform, the preparation method of the nano oxidized holmium of good dispersion and environmental protection.
The object of the present invention is to provide a kind of oxalate precipitation process to produce little particle yttrium oxide, D50 1.0-1.5, and grain
Spend narrow distribution and uniformly.
A kind of preparation method of ultrafine yttria of the present invention is realized by following scheme：
Single yttrium salt solution is obtained as yttrium nitrate, yttrium chloride or sulfuric acid by rare earth extraction workshop section or by rare earth carbonate through acid is molten
Yttrium, configuration concentration 0.1-0.4mol/l, pH value 1-2, this solution are A.
Oxalic acid solution is prepared, the dosage of oxalic acid is 2.3-2.5 times, a concentration of 0.1-0.4mol/l of total amount of rare earth, is added
A certain amount of anion surfactant makees additive, and anion surfactant is neopelex or dodecyl
Sodium sulphate, addition be total amount of rare earth 2%-6%, mass concentration 15%-25%, be sufficiently stirred dissolve solution be B, continuous
Under stirring, A is added in B, it is general, uniform to drip speed.Filtered, detached between 8-10 hours after mixed liquor is precipitated completely,
Washing.The oxalates drained is placed on 90-120 DEG C of drying, then at 750-900 DEG C after calcination through sieving, obtain ultrafine yttria
Powder.Medium particle diameter D50 is measured between 1.0-1.5 through Malvern 2000, and is evenly distributed.
The present invention has the effect of positive：
The effect of the present invention is that preparation process is simple, the rare-earth oxidation of small grain size directly just can be obtained by oxalate precipitation process
Yttrium, and even particle distribution can cause Particle Breakage, impurity to increase, can be directly used for avoid what is worked it out with Physical
The application of luminescent material.
Specific implementation mode
Embodiment 1：
Yttrium chloride solution, allotment to a concentration of 0.4mol/l, PH are obtained after extraction tank detaches by Rare Earth Mine：1.Take this solution
1107ml takes oxalic acid 115g, and solution 2.28L is obtained after dilution.2g neopelexes are added to be dissolved in water, it is continuous in oxalic acid solution
Yttrium chloride solution, charging rate are added in the case of stirring：1L/min, stirring, ageing 8 hours, then filter, wash to PH：7,
Sediment is placed on 120 DEG C of drying, then ultrafine yttria is obtained after 800 DEG C of calcinations.Detecting D50 through Malvern 2000 is
1.443um。
Embodiment 2：
Yttrium oxide is obtained yttrium nitrate solution, allotment to a concentration of 0.3mol/l, PH after nitric acid dissolves：1.Take this solution
2362ml takes oxalic acid 184g, solution 4.87L is obtained after dilution, adds 4g neopelexes, stirring, oxalic acid solution not
Yttrium nitrate solution, stirring, ageing 6 hours, through filtering, washing to PH are added in the case of disconnected stirring：7, sediment is placed on 100
DEG C drying, then obtains ultrafine yttria after 850 DEG C of calcinations.It is 1.38um to detect D50 through Malvern 2000.
Embodiment 3：
Yttrium oxide is obtained yttrium nitrate solution, allotment to 0.2mol/l, PH after nitric acid dissolves：1.This solution 4430ml is taken, grass is taken
Sour 250g obtains solution 9.92L after dilution.Add 6g lauryl sodium sulfate to stir, adds in the case where oxalic acid solution is stirred continuously
Enter yttrium nitrate solution, stirring, ageing 10 hours, through filtering, washing to PH：7, sediment is placed on 100 DEG C of drying, then 850 DEG C
Ultrafine yttria is obtained after calcination.D50 is detected through Malvern 2000：1.31um.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical solution and advantageous effect
It describes in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the guarantor of the present invention
Within the scope of shield.
Claims (8)
1. a kind of preparation method of ultrafine yttria, it is characterised in that include the following steps：
（A）Anion surfactant is added in oxalic acid solution, stirs evenly；
（B）Rare-earth salt solution is added in the oxalic acid solution, sediment is obtained；
（C）Sediment is agitated, ageing, filter, washing, dries acquisition filter cake；
（D）Calcination is carried out to above-mentioned filter cake, ultrafine yttria is obtained after product sieving.
2. the preparation method of ultrafine yttria according to claim 1, it is characterised in that：Rare-earth salt solution be nitrate,
Chlorate or sulfate, and a concentration of 0.1-0.4mol/l, pH value 1.0-2.0.
3. the preparation method of ultrafine yttria according to claim 1, it is characterised in that：Step（A）Middle addition it is cloudy from
Sub- additive is neopelex or lauryl sodium sulfate.
4. the preparation method of ultrafine yttria according to claim 1, it is characterised in that：Step（A）Middle anion addition
The addition of agent is the 2-6% of rare earth quality.
5. the preparation method of ultrafine yttria according to claim 1, it is characterised in that：Step（B）Mesoxalic acid and rare earth
Mass ratio be 2.3-2.5/1.
6. the preparation method of ultrafine yttria according to claim 1, it is characterised in that：Step（C）In precipitating completely
Suction filtration separation, washing are carried out after 8-10 hours.
7. the preparation method of ultrafine yttria according to claim 1, it is characterised in that：Step（C）Middle sediment is in 90-
120 DEG C of drying.
8. the preparation method of ultrafine yttria according to claim 1, it is characterised in that：Step（D）Middle filter cake is in 750-
Calcination at 900 DEG C, product grain grain size D50 are evenly distributed between 1.0-1.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710012362.6A CN108285166A (en) | 2017-01-09 | 2017-01-09 | A kind of preparation method of ultrafine yttria |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710012362.6A CN108285166A (en) | 2017-01-09 | 2017-01-09 | A kind of preparation method of ultrafine yttria |
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| Publication Number | Publication Date |
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| CN108285166A true CN108285166A (en) | 2018-07-17 |
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| CN201710012362.6A Pending CN108285166A (en) | 2017-01-09 | 2017-01-09 | A kind of preparation method of ultrafine yttria |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970090A (en) * | 2019-05-14 | 2019-07-05 | 常州市卓群纳米新材料有限公司 | The ultra-fine ytterbium oxide chemical preparation process that a kind of D50 is 1.5-2um |
| CN110655099A (en) * | 2019-11-01 | 2020-01-07 | 常州市卓群纳米新材料有限公司 | Submicron yttrium oxide with high specific surface area and preparation method thereof |
| WO2025138457A1 (en) * | 2023-12-27 | 2025-07-03 | 赣州湛海新材料科技有限公司 | Method and device for preparing superfine rare earth oxide powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1426963A (en) * | 2001-12-17 | 2003-07-02 | 暨南大学 | Manufacturing method of nano cerium oxide powder |
| CN105084407A (en) * | 2014-05-22 | 2015-11-25 | 常州市卓群纳米新材料有限公司 | Ultrafine lanthanum oxide and preparation method thereof |
| CN106277020A (en) * | 2015-06-12 | 2017-01-04 | 常州卓煜新材料科技有限公司 | A kind of bigger serface micron cerium oxide preparation method |
| CN106277021A (en) * | 2015-06-12 | 2017-01-04 | 常州卓煜新材料科技有限公司 | A kind of large-specific surface area nano Dineodymium trioxide preparation method |
-
2017
- 2017-01-09 CN CN201710012362.6A patent/CN108285166A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1426963A (en) * | 2001-12-17 | 2003-07-02 | 暨南大学 | Manufacturing method of nano cerium oxide powder |
| CN105084407A (en) * | 2014-05-22 | 2015-11-25 | 常州市卓群纳米新材料有限公司 | Ultrafine lanthanum oxide and preparation method thereof |
| CN106277020A (en) * | 2015-06-12 | 2017-01-04 | 常州卓煜新材料科技有限公司 | A kind of bigger serface micron cerium oxide preparation method |
| CN106277021A (en) * | 2015-06-12 | 2017-01-04 | 常州卓煜新材料科技有限公司 | A kind of large-specific surface area nano Dineodymium trioxide preparation method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970090A (en) * | 2019-05-14 | 2019-07-05 | 常州市卓群纳米新材料有限公司 | The ultra-fine ytterbium oxide chemical preparation process that a kind of D50 is 1.5-2um |
| CN109970090B (en) * | 2019-05-14 | 2021-06-25 | 常州市卓群纳米新材料有限公司 | Chemical preparation method of superfine ytterbium oxide with D50 of 1.5-2um |
| CN110655099A (en) * | 2019-11-01 | 2020-01-07 | 常州市卓群纳米新材料有限公司 | Submicron yttrium oxide with high specific surface area and preparation method thereof |
| CN110655099B (en) * | 2019-11-01 | 2022-05-03 | 常州市卓群纳米新材料有限公司 | Submicron yttrium oxide with high specific surface area and preparation method thereof |
| WO2025138457A1 (en) * | 2023-12-27 | 2025-07-03 | 赣州湛海新材料科技有限公司 | Method and device for preparing superfine rare earth oxide powder |
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