CN107487779A - A kind of extracting method of high-purity europium oxide - Google Patents
A kind of extracting method of high-purity europium oxide Download PDFInfo
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- CN107487779A CN107487779A CN201710759244.1A CN201710759244A CN107487779A CN 107487779 A CN107487779 A CN 107487779A CN 201710759244 A CN201710759244 A CN 201710759244A CN 107487779 A CN107487779 A CN 107487779A
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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
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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
- C01F17/10—Preparation or treatment, e.g. separation or purification
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- 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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Abstract
The invention discloses a kind of extracting method of high-purity europium oxide, belong to rare earth oxide preparation field, by adding dissolving with hydrochloric acid to filter, mixed extractant is added to extract in ultrasonic extraction equipment, pass through the reduction-oxidation in electric reactor, and add ammonium carbonate and europium carbonate precipitation, filtering is made, multi-step purification, high-purity europium oxide is dried to obtain finally by high temperature sintering and washing.The invention discloses a kind of extracting method of high-purity europium oxide, and it can not only be avoided using oxalic acid pollution environment, and greatly improves the purity for producing europium oxide, the europium oxide purity is reached 99.999%.
Description
Technical field
The present invention relates to rare earth oxide preparation field, and in particular to a kind of extracting method of high-purity europium oxide.
Background technology
High-purity europium oxide product refers to that the content of europium oxide is more than 99.99%, and europium oxide is a kind of swashing for red fluorescence powder
Agent living, is largely used in the equipment such as television set, display screen, with production technology improve and the raising of people's life requirement,
Pair increasing with the demand of the fluorescent material such as europium oxide, and the progress of technology, color monitor is to giant-screen, high-resolution
Degree, high-resolution direction are developed, and higher requirement is proposed to the purity of europium oxide.
At present, it is reduction-extraction to prepare the higher europium oxide main method of purity, and this method is first by rich europium rare earth
After raw material dissolving with hydrochloric acid, zinc powder is added, trivalent europium is reduced into divalent europium, the feed liquid after reduction is then put into extraction tank
In, while extractant and washing lotion are added, using divalent europium and the difference of trivalent rare earth impurity extraction behavior, extract by multistage
Separation is taken, oxalic acid is then added and produces oxalic acid europium precipitation, europium oxide is produced into oxalic acid europium ignition of precipitate, this method does not require nothing more than sternly
The oxygen barrier measure of lattice, it is also necessary to which a large amount of zinc powders, a large amount of zinc powders are easily lumpd, and certain difficulty, and oxalic acid toxicity are brought to operation
Greatly, environment is easily polluted, most important is that the europium oxide purity that this method is produced is not high, many impurity is contained in product, it is difficult to reach
To the requirement of modern production.
The content of the invention
The defects of in order to overcome prior art, the technical problems to be solved by the invention are to propose a kind of high-purity europium oxide
Extracting method, it can not only avoid, using oxalic acid pollution environment, and greatly improving the purity for producing europium oxide, making this
Europium oxide purity reaches 99.999%.
To use following technical scheme up to this purpose, the present invention：
The invention provides a kind of extracting method of high-purity europium oxide, comprise the following steps：
S1：Dissolving with hydrochloric acid, the weight ratio of the hydrochloric acid of addition and rich europium rare earth oxide are added into rich europium rare earth oxide
1-2：1；Filtrate is taken after filtering, trivalent europium ion is reduced into divalent europium by obtained filtrate on the negative electrode of electrochemical reactor
Ion, obtain EuCl2Solution；
S2：By EuCl2Solution is added in ultrasonic extraction equipment, adds mixed extractant, EuCl2Solution and mixed extractant
Volume ratio be 1：1-5, it operates supersonic frequency 15-25kHz, ultrasonication intensity 5-10W/cm2, 45-55 degrees Celsius of temperature,
EuCl is obtained after extraction2Refined liquid；
The mixed extractant be percent by volume be respectively 60-80%P507 extractants, 10-15%P204 extractants,
5-15% sulfonated kerosenes and 5-10% washing lotions composition；
S3：By EuCl2Refined liquid adds the anode of electrochemical reactor, and divalent europium is oxidized into trivalent europium ion,
Generate EuCl3Refined liquid, toward EuCl3Refined liquid adds adsorbent, separation of solid and liquid after adsorption-edulcoration, obtains high-purity EuCl3Solution；
S4：To S3 high-purity EuCl3Ammonium carbonate, the ammonium carbonate anion and rare-earth chloride solution of addition are added in solution
In the ratio between the mole of cation be 2-3：1,70-80 degrees Celsius of temperature, it is sufficiently stirred, time 1-2h, filters to obtain europium carbonate
Sediment；
S5：The europium carbonate sediment distillation water washing that S4 is obtained 1-3 times, dries 20- under 50-70 degrees Celsius
40min, obtain pure europium carbonate sediment；
S6：Pure europium carbonate sediment in S5 is aoxidized into obtain europium oxide in 900-1000 degrees Celsius of lower calcination, dehydration.
S7：By the europium oxide that S6 is obtained with water washing is distilled 1-3 times, 20-40min is dried under 60-80 degrees Celsius, is obtained
High-purity europium oxide.
In the present invention preferably technical scheme, the weight of hydrochloric acid and rich europium rare earth oxide is than 1.5 in the S1：1.
In the present invention preferably technical scheme, the volume ratio of EuCl2 solution and mixed extractant is 1 in the S2：3,
It operates supersonic frequency 20kHz, ultrasonication intensity 8W/cm2, 50 degrees Celsius of temperature.
In the present invention preferably technical scheme, the S2 mixed extractants are that percent by volume is respectively 70%P507 extractions
Take agent, 13%P204 extractants, 10% sulfonated kerosene and 7% washing lotion composition.
In the present invention preferably in technical scheme, in the S4 ammonium carbonate anion and the sun in rare-earth chloride solution from
The ratio between mole of son is 2.5：1,75 degrees Celsius of temperature, time 1.5h.
In the present invention preferably technical scheme, europium carbonate sediment uses distillation water washing 2 times in the S5, Celsius 60
Degree is lower to dry 30min.
In the present invention preferably technical scheme, the pure europium carbonate sediment in the S6 burns under 1000 degrees Celsius
Burn.
In the present invention preferably technical scheme, europium oxide is done with water washing is distilled 2 times under 70 degrees Celsius in the S7
Dry 30min.
In the present invention preferably technical scheme, described electrochemical reactor is three-diemsnional electrode barrier film electrochemical reaction
Device.
Beneficial effects of the present invention are：
The extracting method of high-purity europium oxide provided by the invention, change agent by introducing a kind of uvioresistant and inhaling, by adding salt
Sour dissolution filter, add mixed extractant and extracted in ultrasonic extraction equipment, pass through the reduction-oxidation in electric reactor, Yi Jijia
Enter ammonium carbonate and europium carbonate precipitation, filtering is made, multi-step purification, high pure oxygen is dried to obtain finally by high temperature sintering and washing
Change europium, obtained europium oxide purity is more than 99.999%.
Embodiment
Technical scheme is further illustrated below by embodiment.
Embodiment one：
S1：Dissolving with hydrochloric acid, the weight ratio of the hydrochloric acid of addition and rich europium rare earth oxide are added into rich europium rare earth oxide
1.5：1；Filtrate is taken after filtering, trivalent europium ion is reduced into divalent europium by obtained filtrate on the negative electrode of electrochemical reactor
Ion, obtain EuCl2Solution；
S2：By EuCl2Solution is added in ultrasonic extraction equipment, adds mixed extractant, EuCl2Solution and mixed extractant
Volume ratio be 1：3, it operates supersonic frequency 20kHz, ultrasonication intensity 8W/cm2, 50 degrees Celsius of temperature, after extraction
EuCl2Refined liquid；
The mixed extractant is that percent by volume is respectively 70%P507 extractants, 13%P204 extractants, 10% sulphur
Change kerosene and 7% washing lotion composition；
S3：By EuCl2Refined liquid adds the anode of electrochemical reactor, and divalent europium is oxidized into trivalent europium ion,
Generate EuCl3Refined liquid, toward EuCl3Refined liquid adds adsorbent, separation of solid and liquid after adsorption-edulcoration, obtains high-purity EuCl3Solution；
S4：To S3 high-purity EuCl3Ammonium carbonate, the ammonium carbonate anion and rare-earth chloride solution of addition are added in solution
In the ratio between the mole of cation be 2.5：1,75 degrees Celsius of temperature, it is sufficiently stirred, time 1.5h, filters to obtain europium carbonate precipitation
Thing；
S5：The europium carbonate sediment distillation water washing that S4 is obtained 2 times, dries 30min, obtains pure at 60 c
Net europium carbonate sediment；
S6：Pure europium carbonate sediment in S5 is aoxidized into obtain europium oxide in 1000 degrees Celsius of lower calcinations, dehydration.
S7：By the europium oxide that S6 is obtained with water washing is distilled 2 times, 30min is dried under 70 degrees Celsius, obtains high pure zirconia
Europium.
Embodiment two：
S1：Dissolving with hydrochloric acid, the weight ratio of the hydrochloric acid of addition and rich europium rare earth oxide are added into rich europium rare earth oxide
1：1；Filtrate is taken after filtering, by obtained filtrate on the negative electrode of electrochemical reactor trivalent europium ion be reduced into divalent europium from
Son, obtain EuCl2Solution；
S2：EuCl2 solution is added in ultrasonic extraction equipment, adds mixed extractant, EuCl2Solution and mixed extractant
Volume ratio be 1：1, it operates supersonic frequency 15kHz, ultrasonication intensity 5W/cm2, 45 degrees Celsius of temperature, after extraction
EuCl2Refined liquid；
The mixed extractant is that percent by volume is respectively 80%P507 extractants, 10%P204 extractants, 5% sulfonation
Kerosene and 5% washing lotion composition；
S3：By EuCl2Refined liquid adds the anode of electrochemical reactor, and divalent europium is oxidized into trivalent europium ion,
Generate EuCl3Refined liquid, toward EuCl3Refined liquid adds adsorbent, separation of solid and liquid after adsorption-edulcoration, obtains high-purity EuCl3Solution；
S4：To S3 high-purity EuCl3Ammonium carbonate, the ammonium carbonate anion and rare-earth chloride solution of addition are added in solution
In the ratio between the mole of cation be 2：1,70 degrees Celsius of temperature, it is sufficiently stirred, time 1h, filters to obtain europium carbonate sediment；
S5：The europium carbonate sediment distillation water washing that S4 is obtained 1 time, dries 20min, obtains pure at 50 c
Net europium carbonate sediment；
S6：Pure europium carbonate sediment in S5 is aoxidized into obtain europium oxide in 900 degrees Celsius of lower calcinations, dehydration.
S7：By the europium oxide that S6 is obtained with water washing is distilled 1 time, 20min is dried at 60 c, obtains high pure zirconia
Europium.
Embodiment three：
S1：Dissolving with hydrochloric acid, the weight ratio of the hydrochloric acid of addition and rich europium rare earth oxide are added into rich europium rare earth oxide
2：1；Filtrate is taken after filtering, by obtained filtrate on the negative electrode of electrochemical reactor trivalent europium ion be reduced into divalent europium from
Son, obtain EuCl2Solution；
S2：By EuCl2Solution is added in ultrasonic extraction equipment, adds mixed extractant, EuCl2Solution and mixed extractant
Volume ratio be 1：5, it operates supersonic frequency 25kHz, ultrasonication intensity 10W/cm2, 55 degrees Celsius of temperature, after extraction
EuCl2Refined liquid；
The mixed extractant is that percent by volume is respectively 60%P507 extractants, 15%P204 extractants, 15% sulphur
Change kerosene and 10% washing lotion composition；
S3：By EuCl2Refined liquid adds the anode of electrochemical reactor, and divalent europium is oxidized into trivalent europium ion,
Generate EuCl3Refined liquid, toward EuCl3Refined liquid adds adsorbent, separation of solid and liquid after adsorption-edulcoration, obtains high-purity EuCl3Solution；
S4：To S3 high-purity EuCl3Ammonium carbonate, the ammonium carbonate anion and rare-earth chloride solution of addition are added in solution
In the ratio between the mole of cation be 3：1,80 degrees Celsius of temperature, it is sufficiently stirred, time 2h, filters to obtain europium carbonate sediment；
S5：The europium carbonate sediment distillation water washing that S4 is obtained 3 times, 40min is dried under 70 degrees Celsius, is obtained pure
Net europium carbonate sediment；
S6：Pure europium carbonate sediment in S5 is aoxidized into obtain europium oxide in 1000 degrees Celsius of lower calcinations, dehydration.
S7：By the europium oxide that S6 is obtained with water washing is distilled 3 times, 40min is dried at 80 degrees celsius, obtains high pure zirconia
Europium.
Comparative example one：
S1：Rich europium rare earth oxide is taken, adds dissolving with hydrochloric acid, the hydrochloric acid weight of addition and the weight of rich europium rare earth oxide
Than 1.5：1, zinc powder is added toward filtrate after filtering, is sufficiently stirred, reduction feed liquid, the zinc powder of addition and rich europium rare earth oxide is made
Between weight than 3：1；
S1：Reduction feed liquid is added in extraction tank, extractant and washing lotion is added, carries out multitple extraction separation, be made higher
The divalent europium solution of purity, while add dilute sulfuric acid, in the sulfate ion and rare earth of the dilute sulfuric acid of addition contained europium from
The ratio of son is 3：2, europous sulfate precipitation is made；
S2：Contain barium sulfate, magnesium sulfate and non-europium rare earth element in europous sulfate sediment, using 5mol/L concentration
Nitric acid discharges the europous sulfate sediment at 80 degrees celsius, and divalent europium is oxidized to trivalent europium ion, adds ammoniacal liquor regulation
PH is more than 11, generation Eu (OH)3Precipitation, toward Eu (OH) after filtering3Dissolving with hydrochloric acid is added in precipitation, adds excessive oxalic acid, is made
Oxalic acid europium precipitates；
S3：By oxalic acid europium sediment in 1000 degrees Celsius of lower high temperature sinterings, obtained europium oxide.
GB/T 3504-2015 are respectively adopted in the obtained europium oxide of embodiment one to embodiment three and comparative example one
The detection test method of europium oxide detects to its purity, obtained result such as following table：
| Embodiment one | Embodiment two | Embodiment three | Comparative example one | |
| Europium oxide purity (%) | 99.9996 | 99.9992 | 99.9994 | 93.6942 |
The present invention is described with reference to the preferred embodiments, and those skilled in the art know, is not departing from the present invention's
In the case of spirit and scope, various changes or equivalence replacement can be carried out to these features and embodiment.The present invention is not by this
The limitation of specific embodiment disclosed in place, other embodiments fallen into claims hereof belong to protection of the present invention
Scope.
Claims (9)
1. a kind of extracting method of high-purity europium oxide, it is characterised in that comprise the following steps：
S1：Dissolving with hydrochloric acid is added toward rich europium rare earth oxide, the weight of the hydrochloric acid of addition and rich europium rare earth oxide compares 1-2：1；
Filtrate is taken after filtering, trivalent europium ion is reduced into divalent europium by obtained filtrate on the negative electrode of electrochemical reactor,
Obtain EuCl2Solution；
S2：By EuCl2Solution is added in ultrasonic extraction equipment, adds mixed extractant, EuCl2The body of solution and mixed extractant
Product is than being 1：1-5, it operates supersonic frequency 15-25kHz, ultrasonication intensity 5-10W/cm2, 45-55 degrees Celsius of temperature, extraction
EuCl is obtained afterwards2Refined liquid；
The mixed extractant is that percent by volume is respectively 60-80%P507 extractants, 10-15%P204 extractants, 5-
15% sulfonated kerosene and 5-10% washing lotions composition；
S3：By EuCl2Refined liquid adds the anode of electrochemical reactor, and divalent europium is oxidized into trivalent europium ion, generates
EuCl3Refined liquid, toward EuCl3Refined liquid adds adsorbent, separation of solid and liquid after adsorption-edulcoration, obtains high-purity EuCl3Solution；
S4：To S3 high-purity EuCl3Add ammonium carbonate in solution, the ammonium carbonate anion of addition with rare-earth chloride solution
The ratio between mole of cation is 2-3：1,70-80 degrees Celsius of temperature, it is sufficiently stirred, time 1-2h, filters to obtain europium carbonate precipitation
Thing；
S5：The europium carbonate sediment distillation water washing that S4 is obtained 1-3 times, 20-40min is dried under 50-70 degrees Celsius, is obtained
To pure europium carbonate sediment；
S6：Pure europium carbonate sediment in S5 is decomposed in 900-1000 degrees Celsius of lower calcination, obtains europium oxide.
S7：By the europium oxide that S6 is obtained with water washing is distilled 1-3 times, 20-40min is dried under 60-80 degrees Celsius, is obtained high-purity
Europium oxide.
2. the extracting method of high-purity europium oxide according to claim 1, it is characterised in that：
The weight of hydrochloric acid and rich europium rare earth oxide is than 1.5 in the S1：1.
3. the extracting method of high-purity europium oxide according to claim 1, it is characterised in that：
EuCl in the S22The volume ratio of solution and mixed extractant is 1：3, it operates supersonic frequency 20kHz, and ultrasonication is strong
Spend 8W/cm2, 50 degrees Celsius of temperature.
4. the extracting method of high-purity europium oxide according to claim 1, it is characterised in that：
The S2 mixed extractants are respectively 70%P507 extractants, 13%P204 extractants, 10% sulfonation by percent by volume
Kerosene and 7% washing lotion composition.
5. the extracting method of high-purity europium oxide according to claim 1, it is characterised in that：
The ratio between mole of cation in the S4 in ammonium carbonate anion and rare-earth chloride solution is 2.5：1, temperature 75
Degree Celsius, time 1.5h.
6. the extracting method of high-purity europium oxide according to claim 1, it is characterised in that：
Europium carbonate sediment dries 30min at 60 c with water washing is distilled 2 times in the S5.
7. the extracting method of high-purity europium oxide according to claim 1, it is characterised in that：
Pure europium carbonate sediment in the S6 is in 1000 degrees Celsius of lower calcinations.
8. the extracting method of high-purity europium oxide according to claim 1, it is characterised in that：
Europium oxide dries 30min with water washing is distilled 2 times under 70 degrees Celsius in the S7.
9. the extracting method of high-purity europium oxide according to claim 1, it is characterised in that：
Described electrochemical reactor is three-diemsnional electrode barrier film electrochemical reactor.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108408758A (en) * | 2018-04-11 | 2018-08-17 | 内蒙古科技大学 | The method for preparing europium oxide with plant precipitating reagent |
| CN115072759A (en) * | 2022-05-05 | 2022-09-20 | 龙南京利有色金属有限责任公司 | Method for recovering high-purity europium oxide from rare earth fluorescent powder waste |
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