CN106006701B - A kind of preparation method of micrometer-submicrometer grade RE oxide powder - Google Patents
A kind of preparation method of micrometer-submicrometer grade RE oxide powder Download PDFInfo
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- CN106006701B CN106006701B CN201610334394.3A CN201610334394A CN106006701B CN 106006701 B CN106006701 B CN 106006701B CN 201610334394 A CN201610334394 A CN 201610334394A CN 106006701 B CN106006701 B CN 106006701B
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- 239000000843 powder Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 39
- -1 rare-earth oxalate Chemical class 0.000 claims abstract description 22
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 238000003801 milling Methods 0.000 claims abstract description 15
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 15
- 239000012266 salt solution Substances 0.000 claims abstract description 13
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 12
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 238000003916 acid precipitation Methods 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 14
- 238000004321 preservation Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 150000003891 oxalate salts Chemical class 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000011973 solid acid Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 210000004718 centriole Anatomy 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 229960001759 cerium oxalate Drugs 0.000 description 10
- ZMZNLKYXLARXFY-UHFFFAOYSA-H cerium(3+);oxalate Chemical compound [Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZMZNLKYXLARXFY-UHFFFAOYSA-H 0.000 description 10
- 229910000420 cerium oxide Inorganic materials 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 229910052681 coesite Inorganic materials 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 230000001376 precipitating effect Effects 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 description 5
- IBSDADOZMZEYKD-UHFFFAOYSA-H oxalate;yttrium(3+) Chemical compound [Y+3].[Y+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O IBSDADOZMZEYKD-UHFFFAOYSA-H 0.000 description 4
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 4
- 244000025254 Cannabis sativa Species 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011833 salt mixture Substances 0.000 description 1
- 238000009938 salting Methods 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
- C01F17/206—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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
Landscapes
- 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 discloses a kind of preparation method of micron-submicron grade RE oxide powder, rare earth oxide is dissolved in acid and is configured to rare-earth salt solution, precipitation reaction is carried out with oxalic acid precipitation agent, obtain rare-earth oxalate powder, after the drying of rare-earth oxalate powder, it carries out broken using airflow milling and is classified to obtain the careless rare-earth oxalate powder of center granularity in the micron-scale, RE oxide powder of the center granularity in micron-submicron grade will be obtained after the powder calcination.The production process of the method is easy to control, and preparation process is simple, and the powder granularity of preparation is thin, is evenly distributed, and good dispersion is at low cost, is easy to industrial production, and airflow milling can be also further improved, to lower the non-rare earth impurity introduced in process of production.
Description
Technical field
The present invention relates to a kind of preparation methods of micrometer-submicrometer grade RE oxide powder.
Background technology
Develop with the research of material towards limiting condition, superfine rare-earth oxide is due to special performance, more coming
More it is valued by people.The approach of currently manufactured micrometer-submicrometer grade RE oxide powder has very much, but the overwhelming majority is special
Be not liquid-phase precipitation method make because being limited by Processes and apparatus product quality it is difficult to ensure that.Jet mill grinding technology is directly used
It is crushed in rare earth oxide and also is difficult to prepare up-to-standard submicron order rare earth oxide.
Invention content
The present invention provides a kind of preparation method of micrometer-submicrometer grade RE oxide powder, at low cost, can industrialize
Production, is prepared that micrometer-submicrometer grade RE oxide powder average grain diameter is small, even particle size distribution.
In order to achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of micrometer-submicrometer grade RE oxide powder, rare earth oxide are dissolved in acid and are configured to rare earth
Salting liquid carries out precipitation reaction with oxalic acid precipitation agent, obtains rare-earth oxalate powder, after the drying of rare-earth oxalate powder, utilizes
Airflow milling carries out broken and is classified to obtain the careless rare-earth oxalate powder of center granularity in the micron-scale, will be obtained after the powder calcination
Center granularity is in the RE oxide powder of micrometer-submicrometer grade.
A kind of preparation method of micrometer-submicrometer grade RE oxide powder, is as follows：
Rare earth oxide is dissolved in acid and is configured to certain density rare-earth salt solution by step 1；
Step 2 keeps the temperature rare-earth salt solution at a certain temperature；
Oxalic acid precipitation agent is added to by certain charging rate in the rare-earth salt solution of constant temperature by step 3 under stirring, charging
After continue stirring a period of time, make to be uniformly mixed, precipitation reaction is complete；
Step 4 filters, and obtains rare-earth oxalate precipitation, and repeatedly washed with the mode increased pure water and then filtered
It washs, the rare-earth oxalate powder after being drained；
Step 5, soaking time 4~6 in the baking oven that rare-earth oxalate powder after draining is 100~120 DEG C in temperature
Hour, obtain dry rare-earth oxalate powder；
Step 6, dry rare-earth oxalate powder are crushed and are classified by airflow milling, the parameter point of control pressure
Grade obtains the rare-earth oxalate that center granularity is 1~2,2~3 or 3~4 μm；
Step 7, broken oxalates carry out calcination in Muffle furnace, and calcination temperature is 750~1050 DEG C, heat preservation 2
~4 hours, you can obtain the rare earth oxide that center granularity is 0.8~1.2,1.2~2.8 or 1.8~2.4 μm.
Wherein, the rare-earth salt solution of the step 1 is that nitrate, chloride, sulfate or their salt-mixture are molten
Liquid, a concentration of 0.5-2 mol/L.
Rare-earth salt solution preheating, the heat preservation of the step 2, temperature range are 40~70 DEG C.
The oxalic acid precipitation agent of the step 3 is oxalic acid solid or oxalic acid solution, and solution concentration is 0.5-2.0 mol/L.
The rare-earth oxalate center granularity that the step 4 obtains is 10~20 μm.
After using the above scheme, then the present invention is carried out obtained oxalates using industrial common intermediate processing
Dry, airflow milling carries out calcination again after crushing, and obtains small micrometer-submicrometer grade, average grain diameter, even particle size distribution, dispersibility
Good rare earth oxide.
It is an advantage of the invention that：The production process of the method is easy to control, and preparation process is simple, the powder grain of preparation
Degree is thin, is evenly distributed, good dispersion is at low cost, is easy to industrial production, and airflow milling can be also further improved, to lower in life
Produce the non-rare earth impurity introduced in the process.
Description of the drawings
Fig. 1 is the broken SEM figures of cerium oxalate airflow milling prepared by present example 1；
Fig. 2 is the SEM figures of cerium oxide prepared by present example 1.
Specific embodiment
Example 1：It cerium oxide is dissolved in hydrochloric acid is made into the solution of 0.84 mol/L and pour into reactor, be heated to 45
℃；By the precipitating reagent oxalic acid solution of prepared a concentration of 1.0 mol/L, it is added in the liquid of bottom with the rate of 2 L/min；It treats
After the completion of charging, l0 min are stirred；Will precipitate filter, wash to get to white cerium oxalate powder.Cerium oxalate powder is put
In alumina crucible, dried 5 hours at 110 DEG C.Then it is crushed in airflow milling, the parameters such as control pressure, obtained grass
Sour cerium powder D50It is 2.04 μm（Fig. 1）.Then the powder is placed in alumina crucible, calcination 3 hours at 750 DEG C,
Obtained cerium oxide powder D50It is 1.21 μm.Powder is evenly distributed（Fig. 2）, usual impurities Fe2O3: 35ppm、SiO2:
44ppm、Al2O3: 50ppm。
Example 2：It cerium oxide is dissolved in hydrochloric acid is made into the solution of 0.84 mol/L and pour into reactor, be heated to 45
℃；By the precipitating reagent oxalic acid solution of prepared a concentration of 1.0 mol/L, it is added in the liquid of bottom with the rate of 2 L/min；It treats
After the completion of charging, l0 min are stirred；Will precipitate filter, wash to get to white cerium oxalate powder.Cerium oxalate powder is put
In alumina crucible, dried 5 hours at 110 DEG C.Then it is crushed in airflow milling, the parameters such as control pressure obtain
Cerium oxalate powder D50It is 1.51 μm.Then the powder is placed in alumina crucible, calcination 3 hours, obtain at 750 DEG C
Cerium oxide powder D50It is 0.85 μm.Powder is evenly distributed, usual impurities Fe2O3: 38 ppm、SiO2: 53 ppm、
Al2O3: 44 ppm。
Example 3：It cerium oxide is dissolved in hydrochloric acid is made into the solution of 0.84 mol/L and pour into reactor, be heated to 45 DEG C；
By the precipitating reagent oxalic acid solution of prepared a concentration of 1.0 mol/L, it is added in the liquid of bottom with the rate of 2 L/min；It is to be added
After the completion of material, l0 min are stirred；Will precipitate filter, wash to get to white cerium oxalate powder.Cerium oxalate powder is placed in
In alumina crucible, dried 5 hours at 110 DEG C.Then it is crushed in airflow milling, the parameters such as control pressure, obtained grass
Sour cerium powder D50It is 3.25 μm.Then the powder is placed in alumina crucible, calcination 3 hours, obtain at 750 DEG C
Cerium oxide powder D50It is 2.31 μm.Powder is evenly distributed, usual impurities Fe2O3: 24 ppm、SiO2: 29 ppm、
Al2O3: 37 ppm。
Example 4：It yttrium oxide is dissolved in nitric acid is made into the solution of 1.0 mol/L and pour into reactor, be heated to 60 DEG C；
By the precipitating reagent oxalic acid solution of prepared a concentration of 1.0 mol/L, it is added in the liquid of bottom with the rate of 1.6 L/min；
After the completion of to be fed, l0 min are stirred；Will precipitate filter, wash to get to white yttrium oxalate powder.By yttrium oxalate powder
It is placed in alumina crucible, is dried 6 hours at 105 DEG C.Then it is crushed in airflow milling, the parameters such as control pressure obtain
Cerium oxalate powder D50It is 3.24 μm.Then the powder is placed in alumina crucible, calcination 3 hours at 850 DEG C,
Obtained yttrium oxide powder D50It is 2.18 μm.Powder is evenly distributed, usual impurities Fe2O3: 16 ppm、SiO2: 41
ppm、Al2O3: 25 ppm。
Example 5：It yttrium oxide is dissolved in nitric acid is made into the solution of 1.0 mol/L and pour into reactor, be heated to 60 DEG C；
By the precipitating reagent oxalic acid solution of prepared a concentration of 1.0 mol/L, it is added in the liquid of bottom with the rate of 1.6 L/min；
After the completion of to be fed, l0 min are stirred；Will precipitate filter, wash to get to white yttrium oxalate powder.By yttrium oxalate powder
It is placed in alumina crucible, is dried 6 hours at 105 DEG C.Then it is crushed in airflow milling, the parameters such as control pressure obtain
Cerium oxalate powder D50It is 1.48 μm.Then the powder is placed in alumina crucible, calcination 3 hours at 750 DEG C,
Obtained yttrium oxide powder D50It is 0.92 μm.Powder is evenly distributed, usual impurities Fe2O3: 24 ppm、SiO2: 32
ppm、Al2O3: 39 ppm。
Claims (10)
1. a kind of preparation method of micrometer-submicrometer grade RE oxide powder, it is characterised in that：Rare earth oxide is dissolved in acid and matches
Rare-earth salt solution is made, precipitation reaction is carried out with oxalic acid precipitation agent, obtains rare-earth oxalate powder, the drying of rare-earth oxalate powder
Afterwards, it is crushed and is classified using airflow milling, it is 1~2,2~3 or 3~4 μm that the parameter classification of control pressure, which obtains center granularity,
Rare-earth oxalate powder, by the powder calcination, calcination temperature is 750~1050 DEG C, and heat preservation 2~4 hours is to get to centriole
Spend the RE oxide powder for 0.8~1.2,1.2~2.8 or 1.8~2.4 μm.
A kind of 2. preparation method of micrometer-submicrometer grade RE oxide powder as described in claim 1, it is characterised in that step
It is rapid as follows：
Rare earth oxide is dissolved in acid and is configured to rare-earth salt solution by step 1；
Step 2 keeps the temperature rare-earth salt solution；
Oxalic acid precipitation agent, is added in the rare-earth salt solution of constant temperature by step 3 under stirring, continues to stir after charging, makes to mix
It closes uniformly, precipitation reaction is complete；
Step 4 filters, and obtains rare-earth oxalate precipitation, and washed with the mode increased pure water and then filtered, is taken out
Rare-earth oxalate powder after dry；
Step 5, the rare-earth oxalate powder drying after draining, obtains dry rare-earth oxalate powder；
Step 6, dry rare-earth oxalate powder are crushed and are classified by airflow milling, and the parameter classification of control pressure obtains
To rare-earth oxalate；
Step 7, broken oxalates carry out calcination to get to the rare earth oxide of micrometer-submicrometer grade in Muffle furnace.
3. a kind of preparation method of micrometer-submicrometer grade RE oxide powder as claimed in claim 2, it is characterised in that：
The rare-earth salt solution of the step 1 is nitrate, chloride, sulfate or their mixing salt solution, a concentration of 0.5-
2mol/L。
4. a kind of preparation method of micrometer-submicrometer grade RE oxide powder as claimed in claim 2, it is characterised in that：
Rare-earth salt solution preheating, the heat preservation of the step 2, temperature range are 40~70 DEG C.
5. a kind of preparation method of micrometer-submicrometer grade RE oxide powder as claimed in claim 2, it is characterised in that：
The oxalic acid precipitation agent of the step 3 be oxalic acid solid or oxalic acid solution, solution concentration 0.5-2.0mol/L.
6. a kind of preparation method of micrometer-submicrometer grade RE oxide powder as claimed in claim 2, it is characterised in that：
The rare-earth oxalate center granularity that the step 4 obtains is 10~20 μm.
7. a kind of preparation method of micrometer-submicrometer grade RE oxide powder as claimed in claim 2, it is characterised in that：
The drying of the step 5 carries out in an oven, and temperature is 100~120 DEG C, and soaking time is 4~6 hours.
8. a kind of preparation method of micrometer-submicrometer grade RE oxide powder as claimed in claim 2, it is characterised in that：
The airflow milling of the step 6, which crushes, to be classified rear to the rare-earth oxalate that center granularity is 1~2,2~3 or 3~4 μm.
9. a kind of preparation method of micrometer-submicrometer grade RE oxide powder as claimed in claim 2, it is characterised in that：
The step 7 calcination carries out in Muffle furnace, and calcination temperature is 750~1050 DEG C, keeps the temperature 2~4 hours.
10. a kind of preparation method of micrometer-submicrometer grade RE oxide powder as claimed in claim 2, it is characterised in that：
The rare earth oxide that center granularity is 0.8~1.2,1.2~2.8 or 1.8~2.4 μm is obtained after the step 7 calcination.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110468275A (en) * | 2019-09-27 | 2019-11-19 | 中国恩菲工程技术有限公司 | Remove the method for sulfate radical and the product obtained by this method in rare-earth precipitation object |
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| CN108557864A (en) * | 2018-06-05 | 2018-09-21 | 常州市卓群纳米新材料有限公司 | A kind of D50:The preparation method and application of the samarium oxide of 7-10um |
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