CN107935017A - A kind of process that oxide nano rare earth is prepared using ultrasonic wave - Google Patents
A kind of process that oxide nano rare earth is prepared using ultrasonic wave Download PDFInfo
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- CN107935017A CN107935017A CN201711227343.1A CN201711227343A CN107935017A CN 107935017 A CN107935017 A CN 107935017A CN 201711227343 A CN201711227343 A CN 201711227343A CN 107935017 A CN107935017 A CN 107935017A
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- Prior art keywords
- rare earth
- ultrasonic wave
- prepared
- oxide nano
- nano rare
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Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Abstract
The invention belongs to rare earth processing technique field, specifically discloses a kind of process that oxide nano rare earth is prepared using ultrasonic wave.By rare-earth original ore acid treatment, then precipitated, be then ultrasonically treated, last calcination crush and etc. be made.The rare earth oxide of preparation adds speed control by precipitating reagent, dispersant adds, is ultrasonically treated etc., avoids the generation of agglomeration.The present invention is easy to operate, and the rare earth oxide of preparation reaches Nano grade and utilizes space with larger.
Description
【Technical field】
The invention belongs to rare earth processing technique field, and in particular to a kind of to prepare oxide nano rare earth using ultrasonic wave
Process.
【Background technology】
Rare earth element is the lanthanide series in the periodic table of elements --- lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium
(Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), with
And with the closely related yttrium of group of the lanthanides (Y) and scandium (Sc) totally 17 kinds of elements.The special electron configuration of rare earth element make its have special light,
Electricity, magnetic property, are known as the treasure-house of new material.Rare earth oxide is one kind important in rare earth compound, widely used.And receive
Rice rare earth oxide can show more superior performance.But easily reunite in oxide nano rare earth preparation process,
Cause rare-earth oxidation amount of substance bad, influence to use.
【The content of the invention】
The present invention provides a kind of process that oxide nano rare earth is prepared using ultrasonic wave, to solve existing rare earth oxygen
The problem of easily reuniting in compound preparation process.
In order to solve the above technical problems, the present invention uses following technical scheme：
The process of oxide nano rare earth is prepared using ultrasonic wave, this method comprises the following steps：
S1：Rare-earth original ore is added in acid solution, and stirring, then adds precipitating reagent, continue to stir, obtain precipitate A；
S2：Precipitate A adds water, adds dispersant, and 20-45min is handled in the ultrasonic wave of 30-60kHz, and filtering to precipitate
B；
S3：Precipitate B is burnt 30-180min at 800-1500 DEG C, and cooling, pulverizes and sieves obtained rare earth oxide.
Contain hydrochloric acid and sulfuric acid in the acid solution.
Sulfuric acid concentration is 4-8% in the acid solution.
Concentration of hydrochloric acid is 2-5% in the acid solution.
The precipitating reagent is hydroxide, one kind of oxalates.
PH7-9 in solution when the precipitating reagent stops adding.
The stir speed (S.S.) is 200-500r/min.
The addition speed of the precipitating reagent is 10-25mL/min.
The dispersant is neopelex.
The crushing is ultramicro grinding.
The sieve diameter of the sieving is 500-800 mesh.
The beneficial effects of the present invention are：The present invention controls the addition speed of precipitating reagent during rare earth oxide is prepared
Rate, it is too fast to prevent that precipitating reagent from adding, and in combination with the use of dispersant, it is existing to avoid the too fast caused reunion of precipitation formation speed
As.The present invention is easy to operate, and the rare earth oxide of preparation reaches Nano grade and utilizes space with larger.
【Embodiment】
For ease of more fully understanding the present invention, it is illustrated by following instance, these examples belong to the protection of the present invention
Scope, but do not limit the scope of the invention.
Embodiment 1
The process that oxide nano rare earth is prepared using ultrasonic wave is comprised the following steps：
S1：Rare-earth original ore is added in acid solution, and stirring, then adds calcium hydroxide, continue to stir, obtain precipitate A；
S2：Precipitate A adds water, adds dispersant, and 20min is handled in the ultrasonic wave of 30kHz, filters to obtain precipitate B；
S3：Precipitate B is burnt 30min at 800 DEG C, and cooling, pulverizes and sieves obtained rare earth oxide.
Contain hydrochloric acid and sulfuric acid in acid solution.
Sulfuric acid concentration is 4% in acid solution.
Concentration of hydrochloric acid is 2% in acid solution.
PH7 in solution when precipitating reagent stops adding.
Stir speed (S.S.) is 200r/min.
The addition speed of precipitating reagent is 10mL/min.
Dispersant is neopelex.
Crush as ultramicro grinding.
The sieve diameter of sieving is 500 mesh.
Embodiment 2
The process that oxide nano rare earth is prepared using ultrasonic wave is comprised the following steps：
S1：Rare-earth original ore is added in acid solution, and stirring, then adds sodium oxalate, continue to stir, obtain precipitate A；
S2：Precipitate A adds water, adds dispersant, and 32min is handled in the ultrasonic wave of 50kHz, filters to obtain precipitate B；
S3：Precipitate B is burnt 140min at 1200 DEG C, and cooling, pulverizes and sieves obtained rare earth oxide.
Contain hydrochloric acid and sulfuric acid in acid solution.
Sulfuric acid concentration is 6% in acid solution.
Concentration of hydrochloric acid is 3% in acid solution.
PH8.2 in solution when precipitating reagent stops adding.
Stir speed (S.S.) is 450r/min.
The addition speed of precipitating reagent is 118mL/min.
Dispersant is neopelex.
Crush as ultramicro grinding.
The sieve diameter of sieving is 600 mesh.
Embodiment 3
The process that oxide nano rare earth is prepared using ultrasonic wave is comprised the following steps：
S1：Rare-earth original ore is added in acid solution, and stirring, then adds sodium hydroxide, continue to stir, obtain precipitate A；
S2：Precipitate A adds water, adds dispersant, and 45min is handled in the ultrasonic wave of 60kHz, filters to obtain precipitate B；
S3：Precipitate B is burnt 180min at 1500 DEG C, and cooling, pulverizes and sieves obtained rare earth oxide.
Contain hydrochloric acid and sulfuric acid in acid solution.
Sulfuric acid concentration is 8% in acid solution.
Concentration of hydrochloric acid is 5% in acid solution.
PH9 in solution when precipitating reagent stops adding.
Stir speed (S.S.) is 500r/min.
The addition speed of precipitating reagent is 25mL/min.
Dispersant is neopelex.
Crush as ultramicro grinding.
The sieve diameter of sieving is 800 mesh.
Above content is to combine specific/preferred embodiment further description made for the present invention, it is impossible to
Assert that the specific implementation of the present invention is confined to these explanations.Come for general technical staff of the technical field of the invention
Say, without departing from the inventive concept of the premise, it can also make some replacements or modification to the embodiment that these have been described,
And these are substituted or variant should all be considered as belonging to protection scope of the present invention.
Claims (10)
1. a kind of process that oxide nano rare earth is prepared using ultrasonic wave, it is characterised in that this method includes following step
Suddenly：
S1：Rare-earth original ore is added in acid solution, and stirring, then adds precipitating reagent, continue to stir, obtain precipitate A；
S2：Precipitate A adds water, adds dispersant, and 20-45min is handled in the ultrasonic wave of 30-60kHz, filters to obtain precipitate B；
S3：Precipitate B is burnt 30-180min at 800-1500 DEG C, and cooling, pulverizes and sieves obtained rare earth oxide.
2. the process of oxide nano rare earth is prepared using ultrasonic wave according to claim 1, it is characterised in that described
Contain hydrochloric acid and sulfuric acid in acid solution.
3. the process of oxide nano rare earth is prepared using ultrasonic wave according to claim 2, it is characterised in that described
Sulfuric acid concentration is 4-8% in acid solution.
4. the process of oxide nano rare earth is prepared using ultrasonic wave according to claim 2, it is characterised in that described
Concentration of hydrochloric acid is 2-5% in acid solution.
5. the process of oxide nano rare earth is prepared using ultrasonic wave according to claim 1, it is characterised in that described
PH7-9 in solution when precipitating reagent stops adding.
6. the process of oxide nano rare earth is prepared using ultrasonic wave according to claim 1, it is characterised in that described
Stir speed (S.S.) is 200-500r/min.
7. the process of oxide nano rare earth is prepared using ultrasonic wave according to claim 1, it is characterised in that described
The addition speed of precipitating reagent is 10-25mL/min.
8. the process of oxide nano rare earth is prepared using ultrasonic wave according to claim 1, it is characterised in that described
Dispersant is neopelex.
9. the process of oxide nano rare earth is prepared using ultrasonic wave according to claim 1, it is characterised in that described
Crush as ultramicro grinding.
10. the process of oxide nano rare earth is prepared using ultrasonic wave according to claim 1, it is characterised in that institute
The sieve diameter for stating sieving is 500-800 mesh.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711227343.1A CN107935017A (en) | 2017-11-29 | 2017-11-29 | A kind of process that oxide nano rare earth is prepared using ultrasonic wave |
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| CN201711227343.1A CN107935017A (en) | 2017-11-29 | 2017-11-29 | A kind of process that oxide nano rare earth is prepared using ultrasonic wave |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1607180A (en) * | 2003-10-14 | 2005-04-20 | 包头华美稀土高科有限公司 | Technology for preparing nanometer rare-earth oxide |
| CN102161498A (en) * | 2011-06-03 | 2011-08-24 | 北京化工大学 | Preparation method of uniformly dispersed nano lanthanum oxide |
| CN102249283A (en) * | 2011-06-03 | 2011-11-23 | 北京化工大学 | Method for preparing highly-dispersed nano-sized lanthanum oxide by carbon black system |
-
2017
- 2017-11-29 CN CN201711227343.1A patent/CN107935017A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1607180A (en) * | 2003-10-14 | 2005-04-20 | 包头华美稀土高科有限公司 | Technology for preparing nanometer rare-earth oxide |
| CN102161498A (en) * | 2011-06-03 | 2011-08-24 | 北京化工大学 | Preparation method of uniformly dispersed nano lanthanum oxide |
| CN102249283A (en) * | 2011-06-03 | 2011-11-23 | 北京化工大学 | Method for preparing highly-dispersed nano-sized lanthanum oxide by carbon black system |
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Application publication date: 20180420 |
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