CN110629055A - Method for recovering rare earth oxide from fluorescent powder waste - Google Patents
Method for recovering rare earth oxide from fluorescent powder waste Download PDFInfo
- Publication number
- CN110629055A CN110629055A CN201910813434.6A CN201910813434A CN110629055A CN 110629055 A CN110629055 A CN 110629055A CN 201910813434 A CN201910813434 A CN 201910813434A CN 110629055 A CN110629055 A CN 110629055A
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- China
- Prior art keywords
- rare earth
- hydrochloric acid
- leaching
- material liquid
- earth oxide
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a method for recovering rare earth oxide from fluorescent powder waste, which comprises the following steps: s1, grinding the fluorescent powder waste into fine powder with the particle size of 200 meshes, adding an oxidant into the fine powder for oxidation, and adding hydrochloric acid for leaching after oxidation to obtain hydrochloric acid leaching liquid; s2, adding ammonia water into the hydrochloric acid leaching solution obtained in the step S1, neutralizing and removing impurities to obtain a first material liquid, adding sodium carbonate into leaching residues, roasting, leaching with hydrochloric acid to obtain a second material liquid, and combining the first material liquid and the second material liquid to obtain a mixed material liquid; s3: adding an oxalic acid solution into the mixture obtained in the step S2, fully precipitating, filtering, and taking filter residues; s4: and (4) burning the filter residue in the S3 at high temperature, dehydrating and oxidizing to obtain the high-purity rare earth oxide. The recovery rate of the rare earth elements in 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 recovering rare earth oxide from 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 recovering rare earth oxide from fluorescent powder waste, which can effectively recover rare earth elements in the fluorescent powder waste.
In order to achieve the above object, the present invention provides a method for recovering rare earth oxide from phosphor waste, comprising the steps of:
s1, grinding the fluorescent powder waste into fine powder with the particle size of 200 meshes, adding an oxidant into the fine powder for oxidation, and adding hydrochloric acid for leaching after oxidation to obtain hydrochloric acid leaching liquid;
s2, adding ammonia water into the hydrochloric acid leaching solution obtained in the step S1, neutralizing and removing impurities to obtain a first material liquid, adding sodium carbonate into leaching residues, roasting, leaching with hydrochloric acid to obtain a second material liquid, and combining the first material liquid and the second material liquid to obtain a mixed material liquid;
s3: adding an oxalic acid solution into the mixture obtained in the step S2, fully precipitating, filtering, and taking filter residues;
s4: and (4) burning the filter residue in the S3 at high temperature, dehydrating and oxidizing to obtain the high-purity rare earth oxide.
In a further scheme, the oxidant is sodium hypochlorite.
Preferably, in S1, the hydrochloric acid leaching conditions are: the reaction temperature is 50-70 ℃, the stirring intensity is 500-600r/min, and the hydrochloric acid concentration is 4 mol/L.
The invention has the beneficial effects that: by the method, the recovery rate of the rare earth elements in the fluorescent powder waste can reach more than 99%.
Detailed Description
The embodiment provides a method for recovering rare earth oxide from fluorescent powder waste, which comprises the following steps:
s1, grinding the fluorescent powder waste into fine powder with the particle size of 200 meshes, adding an oxidant sodium hypochlorite into the fine powder for oxidation, and adding hydrochloric acid for leaching after oxidation, wherein the hydrochloric acid leaching conditions are as follows: the reaction temperature is 50-70 ℃, the stirring intensity is 500-600r/min, the hydrochloric acid concentration is 4mol/L, and the solid-to-liquid ratio is 8:1, so as to obtain hydrochloric acid leaching solution;
s2, adding ammonia water into the hydrochloric acid leaching solution obtained in the step S1, neutralizing and removing impurities to obtain a first material liquid, adding sodium carbonate into leaching residues, roasting at the temperature of 400-;
s3: adding an oxalic acid solution into the mixture obtained in the step S2, fully precipitating, filtering, and taking filter residues;
s4: and (3) burning the filter residue in the S3 at high temperature, wherein the burning temperature is 1000-1100 ℃, and dehydrating and oxidizing to obtain the high-purity rare earth oxide.
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 (3)
1. A method for recovering rare earth oxide from fluorescent powder waste is characterized by comprising the following steps:
s1, grinding the fluorescent powder waste into fine powder with the particle size of 200 meshes, adding an oxidant into the fine powder for oxidation, and adding hydrochloric acid for leaching after oxidation to obtain hydrochloric acid leaching liquid;
s2, adding ammonia water into the hydrochloric acid leaching solution obtained in the step S1, neutralizing and removing impurities to obtain a first material liquid, adding sodium carbonate into leaching residues, roasting, leaching with hydrochloric acid to obtain a second material liquid, and combining the first material liquid and the second material liquid to obtain a mixed material liquid;
s3: adding an oxalic acid solution into the mixture obtained in the step S2, fully precipitating, filtering, and taking filter residues;
s4: and (4) burning the filter residue in the S3 at high temperature, dehydrating and oxidizing to obtain the high-purity rare earth oxide.
2. The process of claim 1, wherein the rare earth oxide is extracted from the phosphor waste by:
the oxidant is sodium hypochlorite.
3. The process of claim 1, wherein the rare earth oxide is extracted from the phosphor waste by:
in the S1, the hydrochloric acid leaching conditions are as follows: the reaction temperature is 50-70 ℃, the stirring intensity is 500-600r/min, and the hydrochloric acid concentration is 4 mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910813434.6A CN110629055A (en) | 2019-08-30 | 2019-08-30 | Method for recovering rare earth oxide from fluorescent powder waste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910813434.6A CN110629055A (en) | 2019-08-30 | 2019-08-30 | Method for recovering rare earth oxide from fluorescent powder waste |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110629055A true CN110629055A (en) | 2019-12-31 |
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| CN201910813434.6A Pending CN110629055A (en) | 2019-08-30 | 2019-08-30 | Method for recovering rare earth oxide from fluorescent powder waste |
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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 |
| CN112853098A (en) * | 2020-12-30 | 2021-05-28 | 赣州市恒源科技股份有限公司 | Phosphor powder waste oxide dissolving, co-precipitating and screening device and operation method thereof |
| CN115092953A (en) * | 2022-05-05 | 2022-09-23 | 龙南京利有色金属有限责任公司 | Method for extracting rare earth oxide from rare earth fluorescent powder waste |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4650652A (en) * | 1984-01-31 | 1987-03-17 | Kasei Optonix, Ltd. | Process for recovering highly pure rare earth oxides from a waste rare earth phosphor |
| JPH08333642A (en) * | 1995-06-02 | 1996-12-17 | Mitsubishi Materials Corp | Recovering method of rare earth element from scrap cathode ray tube |
| CA2878486A1 (en) * | 2012-11-08 | 2014-05-15 | Electrochem Technologies & Materials Inc. | Process for recovering rare earth oxides from phosphors, fluorescent lamps and light bulbs, cathode ray tubes and other industrial wastes |
| CN104046806A (en) * | 2014-06-30 | 2014-09-17 | 江西理工大学 | Method for recovering rare earth from waste aluminate green rare-earth 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 |
-
2019
- 2019-08-30 CN CN201910813434.6A patent/CN110629055A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4650652A (en) * | 1984-01-31 | 1987-03-17 | Kasei Optonix, Ltd. | Process for recovering highly pure rare earth oxides from a waste rare earth phosphor |
| JPH08333642A (en) * | 1995-06-02 | 1996-12-17 | Mitsubishi Materials Corp | Recovering method of rare earth element from scrap cathode ray tube |
| CA2878486A1 (en) * | 2012-11-08 | 2014-05-15 | Electrochem Technologies & Materials Inc. | Process for recovering rare earth oxides from phosphors, fluorescent lamps and light bulbs, cathode ray tubes and other industrial wastes |
| CN104046806A (en) * | 2014-06-30 | 2014-09-17 | 江西理工大学 | Method for recovering rare earth from waste aluminate green rare-earth 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 |
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| 杨幼明等: "《从荧光粉废料中提取稀土工艺研究》", 《有色金属(冶炼部分)》 * |
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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 |
| CN112853098A (en) * | 2020-12-30 | 2021-05-28 | 赣州市恒源科技股份有限公司 | Phosphor powder waste oxide dissolving, co-precipitating and screening device and operation method thereof |
| CN115092953A (en) * | 2022-05-05 | 2022-09-23 | 龙南京利有色金属有限责任公司 | Method for extracting rare earth oxide from rare earth fluorescent powder waste |
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Application publication date: 20191231 |