CN110627104A - Method for preparing high-purity rare earth oxide by recovering fluorescent powder waste - Google Patents
Method for preparing high-purity rare earth oxide by recovering fluorescent powder waste Download PDFInfo
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- CN110627104A CN110627104A CN201910813439.9A CN201910813439A CN110627104A CN 110627104 A CN110627104 A CN 110627104A CN 201910813439 A CN201910813439 A CN 201910813439A CN 110627104 A CN110627104 A CN 110627104A
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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 provides a method for preparing high-purity rare earth oxide by recovering fluorescent powder waste, which comprises the following steps: s1, adding sodium hydroxide into the fluorescent powder waste, uniformly stirring, and roasting; s2, adding water into the roasted solid for pulping; s3, adding hydrochloric acid into the serous fluid obtained in the step S2, fully stirring, adjusting the pH value to 4-5 by using an ammonium bicarbonate solution, and performing filter pressing to obtain filtrate and filter residue; s4, extracting the filtrate obtained in the step S3 to respectively obtain a Ce feed liquid, a Tb feed liquid, a Eu feed liquid and a Y feed liquid; s5, adding sodium carbonate into the Ce feed liquid for precipitation, filtering and washing, and then burning the precipitate containing Ce to obtain cerium oxide; adding oxalic acid into the Tb solution, the Eu solution and the Y solution respectively for precipitation, filtering and washing, and then burning the precipitate containing Tb, Eu and Y respectively to obtain terbium oxide, europium oxide and yttrium oxide. The purity of the cerium oxide, the terbium oxide, the europium oxide and the yttrium oxide prepared by the method can reach more than 99 percent.
Description
Technical Field
The invention relates to the field of rare earth, in particular to a method for preparing high-purity rare earth oxide by recovering fluorescent powder waste.
Background
In the 80 s of the 20 th century, the rare earth industry in China rose rapidly by virtue of possessing the advantages of the world's largest rare earth resources, and the rare earth elements are widely applied because of the unique properties of the rare earth elements in the aspects of magnetophotoelectricity and the like. Since the rare earth elements are added into the fluorescent powder, the luminous efficiency, the color rendering property and the service life of the fluorescent lamp can be obviously improved, so the rare earth fluorescent powder is widely applied to the fields of fluorescent lamps, semiconductor lighting light-emitting diodes, color picture tubes and other luminescent materials. With the popularization of green lighting engineering in China, the generation of waste rare earth fluorescent lamps is increased year by year, and if the waste rare earth fluorescent powder is not treated, the environment is polluted, and the waste of rare earth resources is caused.
Disclosure of Invention
The invention aims to provide a method for preparing a high-purity rare earth oxide by recovering fluorescent powder waste, which can effectively recover rare earth elements in the fluorescent powder waste and can prepare the rare earth oxide with high purity.
In order to achieve the purpose, the method for preparing the high-purity rare earth oxide by recovering the fluorescent powder waste comprises the following steps:
s1, adding sodium hydroxide into the fluorescent powder waste, uniformly stirring, and roasting;
s2, adding water into the roasted solid for pulping;
s3, adding hydrochloric acid into the serous fluid obtained in the step S2, fully stirring, adjusting the pH value to 4-5 by using an ammonium bicarbonate solution, and performing filter pressing to obtain filtrate and filter residue;
s4, extracting the filtrate obtained in the step S3 to respectively obtain a Ce feed liquid, a Tb feed liquid, a Eu feed liquid and a Y feed liquid;
s5, adding sodium carbonate into the Ce feed liquid for precipitation, filtering and washing, and then burning the precipitate containing Ce to obtain cerium oxide; adding oxalic acid into the Tb solution, the Eu solution and the Y solution respectively for precipitation, filtering and washing, and then burning the precipitate containing Tb, Eu and Y respectively to obtain terbium oxide, europium oxide and yttrium oxide.
In the step S1, the mass ratio of the sodium hydroxide to the fluorescent powder waste is 2:1, and the roasting temperature is 400-500 ℃.
Further, the hydrochloric acid concentration in the step S3 is 4 mol/L.
Further proposal is that the filter residue obtained in the step S3 is washed by water and is filtered by pressure, and then the filtrate is added into the serous fluid again.
The invention has the beneficial effects that: the purity of the cerium oxide, the terbium oxide, the europium oxide and the yttrium oxide prepared by the method can reach more than 99 percent.
Detailed Description
The embodiment provides a method for preparing high-purity rare earth oxide by recovering fluorescent powder waste, which comprises the following steps:
s1, adding sodium hydroxide into the fluorescent powder waste, uniformly stirring, and roasting;
s2, adding water into the roasted solid for pulping;
s3, adding hydrochloric acid into the serous fluid obtained in the step S2, fully stirring, adjusting the pH value to 4-5 by using an ammonium bicarbonate solution, and performing filter pressing to obtain filtrate and filter residue;
s4, extracting the filtrate obtained in the step S3 to respectively obtain a Ce feed liquid, a Tb feed liquid, a Eu feed liquid and a Y feed liquid;
s5, adding sodium carbonate into the Ce feed liquid for precipitation, filtering and washing, and then burning the precipitate containing Ce to obtain cerium oxide; adding oxalic acid into the Tb solution, the Eu solution and the Y solution respectively for precipitation, filtering and washing, and then burning the precipitate containing Tb, Eu and Y respectively to obtain terbium oxide, europium oxide and yttrium oxide.
Preferably, in step S1, the mass ratio of the sodium hydroxide to the phosphor waste is 2:1, and the baking temperature is 400-.
Preferably, the hydrochloric acid concentration in step S3 is 4 mol/L.
Preferably, the filter residue obtained in step S3 is washed with water and subjected to pressure filtration, and the filtrate is added to the slurry again.
Finally, it should be emphasized that the above-described preferred embodiments of the present invention are merely examples of implementations, rather than limitations, and that many variations and modifications of the invention are possible to those skilled in the art, without departing from the spirit and scope of the invention.
Claims (4)
1. The method for preparing the high-purity rare earth oxide by recovering the fluorescent powder waste is characterized by comprising the following steps of:
s1, adding sodium hydroxide into the fluorescent powder waste, uniformly stirring, and roasting;
s2, adding water into the roasted solid for pulping;
s3, adding hydrochloric acid into the serous fluid obtained in the step S2, fully stirring, adjusting the pH value to 4-5 by using an ammonium bicarbonate solution, and performing filter pressing to obtain filtrate and filter residue;
s4, extracting the filtrate obtained in the step S3 to respectively obtain a Ce feed liquid, a Tb feed liquid, a Eu feed liquid and a Y feed liquid;
s5, adding sodium carbonate into the Ce feed liquid for precipitation, filtering and washing, and then burning the precipitate containing Ce to obtain cerium oxide; adding oxalic acid into the Tb solution, the Eu solution and the Y solution respectively for precipitation, filtering and washing, and then burning the precipitate containing Tb, Eu and Y respectively to obtain terbium oxide, europium oxide and yttrium oxide.
2. The method for preparing high-purity rare earth oxide by recovering the phosphor waste according to claim 1, wherein the method comprises the following steps:
in step S1, the mass ratio of the sodium hydroxide to the phosphor waste is 2:1, and the baking temperature is 400-500 ℃.
3. The method for preparing high-purity rare earth oxide by recovering the phosphor waste according to claim 1, wherein the method comprises the following steps:
the hydrochloric acid concentration in step S3 was 4 mol/L.
4. The method for preparing high-purity rare earth oxide by recovering the phosphor waste according to claim 1, wherein the method comprises the following steps:
and (5) washing the filter residue obtained in the step (S3) with water, performing pressure filtration, and adding the filtrate into the slurry again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910813439.9A CN110627104A (en) | 2019-08-30 | 2019-08-30 | Method for preparing high-purity rare earth oxide by recovering fluorescent powder waste |
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| CN201910813439.9A CN110627104A (en) | 2019-08-30 | 2019-08-30 | Method for preparing high-purity rare earth oxide by recovering fluorescent powder waste |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111392756A (en) * | 2020-05-06 | 2020-07-10 | 龙南县中利再生资源开发有限公司 | Process for extracting high-purity rare earth oxide from fluorescent powder waste |
| CN114427041A (en) * | 2022-01-24 | 2022-05-03 | 中南大学 | Method for recovering cerium and terbium from waste rare earth-based aluminate fluorescent powder through selective vulcanization-flotation separation |
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| CN101307391A (en) * | 2008-07-11 | 2008-11-19 | 广州有色金属研究院 | Process for recovering rare earth element in waste florescent lamps |
| CN101994004A (en) * | 2009-08-11 | 2011-03-30 | 北京有色金属研究总院 | Process for extracting and separating rare-earth elements |
| CN102660688A (en) * | 2012-05-10 | 2012-09-12 | 北京科技大学 | Method for recovering rare earth from waste rare earth luminescent material |
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| US20130309150A1 (en) * | 2011-12-15 | 2013-11-21 | Reenewal Corporation | Rare earth recovery from phosphor |
| CN107513620A (en) * | 2017-08-30 | 2017-12-26 | 赣州齐畅新材料有限公司 | A kind of process of the Extraction of rare earth oxide from fluorescent powder scrap |
| CN109055783A (en) * | 2018-08-15 | 2018-12-21 | 湖南稀土金属材料研究院 | The recovery method of the middle rare earth of waste material containing rare earth oxide |
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2019
- 2019-08-30 CN CN201910813439.9A patent/CN110627104A/en active Pending
Patent Citations (7)
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| CN101307391A (en) * | 2008-07-11 | 2008-11-19 | 广州有色金属研究院 | Process for recovering rare earth element in waste florescent lamps |
| CN101994004A (en) * | 2009-08-11 | 2011-03-30 | 北京有色金属研究总院 | Process for extracting and separating rare-earth elements |
| US20130309150A1 (en) * | 2011-12-15 | 2013-11-21 | Reenewal Corporation | Rare earth recovery from phosphor |
| CN102660688A (en) * | 2012-05-10 | 2012-09-12 | 北京科技大学 | Method for recovering rare earth from waste rare earth luminescent material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111392756A (en) * | 2020-05-06 | 2020-07-10 | 龙南县中利再生资源开发有限公司 | Process for extracting high-purity rare earth oxide from fluorescent powder waste |
| CN114427041A (en) * | 2022-01-24 | 2022-05-03 | 中南大学 | Method for recovering cerium and terbium from waste rare earth-based aluminate fluorescent powder through selective vulcanization-flotation separation |
| CN114427041B (en) * | 2022-01-24 | 2022-09-27 | 中南大学 | Method for recovering cerium and terbium from waste rare earth-based aluminate fluorescent powder through selective vulcanization-flotation separation |
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Application publication date: 20191231 |
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