CN105776309A - Europium sulfate decomposition method - Google Patents
Europium sulfate decomposition method Download PDFInfo
- Publication number
- CN105776309A CN105776309A CN201610245994.2A CN201610245994A CN105776309A CN 105776309 A CN105776309 A CN 105776309A CN 201610245994 A CN201610245994 A CN 201610245994A CN 105776309 A CN105776309 A CN 105776309A
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- CN
- China
- Prior art keywords
- europium
- hydrochloric acid
- sulfate
- acid solution
- hydrogen peroxide
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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
- C01F17/282—Sulfates
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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
- C01F17/224—Oxides or hydroxides of lanthanides
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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
- C01F17/247—Carbonates
-
- 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
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/36—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 halogen being the only anion, e.g. NaYF4
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
An europium sulfate decomposition method is characterized in that europium sulfate is added to a hydrochloric acid solution according to the 1: (2-6): (1-0.5) mass ratio of the europium sulfate to the hydrochloric acid solution to hydrogen peroxide, and stirring is performed for 10-30 minutes; then the hydrogen peroxide is added, and stirring is performed for 1-5 hours; finally, water is added for dilution according to the (0.5-4):1 mass ratio of the water to the hydrochloric acid solution, filtration is performed, filter residues are returned for re-decomposition treatment, and filtrate is used for crude europium preparation. The europium sulfate decomposition method adopts the hydrogen peroxide to decompose the europium sulfate in the hydrochloric acid solution, replaces a traditional nitric acid or alkali heating decomposition process, reduces the energy consumption and is simple in operation and low in cost.
Description
Technical field
The present invention relates to a kind of method that europous sulfate decomposes.
Background technology
Europium is good luminescent material activator, as: Eu3+It is the activator of red illuminating material, Eu2+It it is the activator of blue emitting material.Europium oxide, as luminescent material activator, is widely used among LED, trichromatic energy saving lamp, high definition screen, New X ray medical diagnostic system.Simultaneous oxidation europium applies also among laser, superconductor, magnetic bubble storage device, the control material of atomic pile, shielding material and structural material.Therefore, europium oxide demonstrates extremely important status and effect in the photoelectricity new material technology quickly grown.
Basicity reducing process produces the purifying technique of high-purity mangesium oxide europium and mainly first adopts zinc powder that trivalent europium ion is reduced into divalent europium, and divalent europium and sulfate radical form europous sulfate precipitation and other rare earths separation；Then europous sulfate is decomposed, extract, prepare high-purity europium oxide.Europous sulfate stable chemical nature, relatively difficult decomposition, currently mainly adopt following methods: 1. nitric acid heat is boiled: adopt the salpeter solution of 5mol/L to boil 6 hours oxidation dissolution europous sulfates；2. alkali heat is boiled: adopt 70g/L sodium carbonate and the mixed liquor of 15g/L sodium hydroxide or the sodium carbonate liquor of 200g/L to boil 1.5 hours, europous sulfate is converted into carbonic acid Asia europium, then (Xu Guangxian edits, " rare earth " by carbonic acid Asia europium oxidation dissolution, metallurgical industry publishing house, 1995).Both the above method is required for heating, consumes substantial amounts of heat energy, nitric acid and sodium carbonate expensive, and production cost is higher.
Summary of the invention
It is an object of the invention to provide a kind of simple to operate, it is not necessary to heating, raw material is cheap, the decomposition method of the europous sulfate that discomposing effect is good.
The method that europous sulfate of the present invention decomposes is as follows: is first added by europous sulfate in hydrochloric acid solution and stirs, is subsequently adding hydrogen peroxide and decomposes, and adds water dilution, filter after having decomposed, and filtering residue returns resolution process again, and filtrate is used for preparing thick europium.The method of the present invention is made up of following steps:
At room temperature, by europous sulfate: hydrochloric acid solution: hydrogen peroxide mass ratio is 1:2 ~ 6:0.1 ~ 0.5, is joined by europous sulfate in hydrochloric acid solution, stir 10 ~ 30 minutes；It is subsequently adding hydrogen peroxide, stirs 1 ~ 5 hour；Finally by water: hydrochloric acid solution mass ratio is 0.5 ~ 4:1 dilute, filtering, filtering residue is undecomposed europous sulfate, returns resolution process again, and filtrate is used for preparing thick europium.
Described concentration of hydrochloric acid solution 4 ~ 10mol/L.
Described hydrogen peroxide concentration 20 ~ 50%.
Chemical equation in the present invention is as follows:
2HCl-+H2O2→Cl2+2H2O；
3Cl2+6EuSO4→2Eu2(SO4)3+2EuCl3。
Europous sulfate stable chemical nature, insoluble in soda acid, not easily reacts with other material, but europium sulfate and Europium chloride have a good water solublity, easy-to-use produces other europium product.The present invention adds hydrogen peroxide in hydrochloric acid, produces chlorine and heat, utilizes the heat energy of reaction releasing and the strong oxidizing property of chlorine that the divalent europium in europous sulfate is oxidized to trivalent europium, is decomposed by europous sulfate, generate water-soluble europium sulfate and Europium chloride.Owing to europium sulfate dissolubility is big not, only about 40g/L, in order to after preventing solution cooling trivalent europium with europium sulfate Precipitation, dilute after decomposition.The present invention adopts hydrogen peroxide to decompose europous sulfate in hydrochloric acid solution, substitutes tradition nitric acid or alkali heat resolve technique, and energy efficient is simple to operate, with low cost.
Detailed description of the invention
Embodiment 1
At room temperature, europous sulfate 50Kg is joined in the hydrochloric acid solution that 100L concentration is 4mol/L and stir 10 minutes；It is subsequently adding the hydrogen peroxide that 5Kg concentration is 50%, stirs 5 hours；Being eventually adding the dilution of 150L water, filter, filtering residue is undecomposed europous sulfate, weight 3Kg, returns resolution process again, and filtrate is the mixed solution of europium sulfate and Europium chloride, adds ammonia precipitation process and prepares europium hydroxide.By analysis, europous sulfate resolution ratio is 93%.
Embodiment 2
At room temperature, europous sulfate 50Kg is joined in the hydrochloric acid solution that 185L concentration is 10mol/L and stir 20 minutes；It is subsequently adding the hydrogen peroxide that 15Kg concentration is 30%, stirs 3 hours；Being eventually adding the dilution of 200L water, filter, filtering residue is undecomposed europous sulfate, weight 0.25Kg, returns resolution process again, and filtrate is the mixed solution of europium sulfate and Europium chloride, adds ammonium bicarbonate precipitation and prepares europium carbonate.By analysis, europous sulfate resolution ratio is 99.5%.
Embodiment 3
At room temperature, europous sulfate 50Kg is joined in the hydrochloric acid solution that 250L concentration is 5mol/L and stir 30 minutes；It is subsequently adding the hydrogen peroxide quality that 25Kg concentration is 20%, stirs 1 hour；Being eventually adding the dilution of 120L water, filter, filtering residue is undecomposed europous sulfate, weight 1Kg, returns resolution process again, and filtrate is the mixed solution of europium sulfate and Europium chloride, adds ammonium bicarbonate precipitation and prepares europium carbonate.By analysis, europous sulfate resolution ratio is 98%.
Embodiment 4
At room temperature, europous sulfate 50Kg is joined in the hydrochloric acid solution that 180L concentration is 5mol/L and stir 20 minutes；It is subsequently adding the hydrogen peroxide that 10Kg concentration is 40%, stirs 3 hours；Being eventually adding the dilution of 700L water, filter, filtering residue is undecomposed europous sulfate, weight 0.5Kg, returns resolution process again, and filtrate is the mixed solution of europium sulfate and Europium chloride, adds ammonia and ammonium hydrogen carbonate mixed liquor precipitation europium carbonate.By analysis, europous sulfate resolution ratio is 99%.
Claims (3)
1. the method that europous sulfate decomposes, is characterized in that at room temperature, by europous sulfate: hydrochloric acid solution: hydrogen peroxide mass ratio is 1:2 ~ 6:0.1 ~ 0.5, is joined by europous sulfate in hydrochloric acid solution, stirs 10 ~ 30 minutes；It is subsequently adding hydrogen peroxide, stirs 1 ~ 5 hour；Finally by water: hydrochloric acid solution mass ratio is 0.5 ~ 4:1 dilute；Filtering, filtering residue returns resolution process again, and filtrate is used for preparing thick europium.
2. the method that europous sulfate according to claim 1 decomposes, is characterized in that described concentration of hydrochloric acid solution 4 ~ 10mol/L.
3. the method that europous sulfate according to claim 1 decomposes, is characterized in that described hydrogen peroxide concentration 20 ~ 50%.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610245994.2A CN105776309A (en) | 2016-04-20 | 2016-04-20 | Europium sulfate decomposition method |
| PCT/CN2016/090144 WO2017181541A2 (en) | 2016-04-20 | 2016-07-15 | Method for decomposing europium(ii) sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610245994.2A CN105776309A (en) | 2016-04-20 | 2016-04-20 | Europium sulfate decomposition method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105776309A true CN105776309A (en) | 2016-07-20 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610245994.2A Pending CN105776309A (en) | 2016-04-20 | 2016-04-20 | Europium sulfate decomposition method |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN105776309A (en) |
| WO (1) | WO2017181541A2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109680167A (en) * | 2019-01-17 | 2019-04-26 | 广东省稀有金属研究所 | A method of the continuously Separation Europium from rare-earth liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4386056A (en) * | 1982-07-30 | 1983-05-31 | Westinghouse Electric Corp. | Recovery of yttrium and europium from contaminated solutions |
| US4432948A (en) * | 1982-07-30 | 1984-02-21 | U.S. Philips Corporation | Recovery of yttrium and europium from contaminated solutions |
| CN1033783A (en) * | 1987-12-30 | 1989-07-12 | 兰州大学 | A kind of method with photoreduction met hod separating and extracting fluorescence-level europiumsesquioxide from rareearth enriching material |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD298762A5 (en) * | 1990-04-02 | 1992-03-12 | Stickstoffwerke Ag Wittenberg-Piesteritz,De | METHOD FOR PRODUCING PURE EUROPA OXIDE |
| CN100485056C (en) * | 2004-06-12 | 2009-05-06 | 包头市京瑞新材料有限公司 | Zinc powder reduction process of preparing europium-enriched solution |
| CN101985694A (en) * | 2010-10-26 | 2011-03-16 | 赣县金鹰稀土实业有限公司 | Preparation method for recovering high-purity yttrium europium from fluorescent powder scrap |
| CN104532006B (en) * | 2015-01-26 | 2016-08-17 | 山东科技大学 | Europium oxide and the method for yittrium oxide is extracted from Waste fluorescent powder |
-
2016
- 2016-04-20 CN CN201610245994.2A patent/CN105776309A/en active Pending
- 2016-07-15 WO PCT/CN2016/090144 patent/WO2017181541A2/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4386056A (en) * | 1982-07-30 | 1983-05-31 | Westinghouse Electric Corp. | Recovery of yttrium and europium from contaminated solutions |
| US4432948A (en) * | 1982-07-30 | 1984-02-21 | U.S. Philips Corporation | Recovery of yttrium and europium from contaminated solutions |
| CN1033783A (en) * | 1987-12-30 | 1989-07-12 | 兰州大学 | A kind of method with photoreduction met hod separating and extracting fluorescence-level europiumsesquioxide from rareearth enriching material |
Non-Patent Citations (2)
| Title |
|---|
| 李杏英等: "还原分离法制取粗铕回收率的影响因素", 《材料研究与应用》 * |
| 韩旗英等: "高纯氧化铕分离提纯工艺综述", 《湖南有色金属》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109680167A (en) * | 2019-01-17 | 2019-04-26 | 广东省稀有金属研究所 | A method of the continuously Separation Europium from rare-earth liquid |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2017181541A3 (en) | 2017-11-30 |
| WO2017181541A2 (en) | 2017-10-26 |
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