CN102634667A - Method for recycling rear-earth elements form abandoned fluorescent lamps - Google Patents
Method for recycling rear-earth elements form abandoned fluorescent lamps Download PDFInfo
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- CN102634667A CN102634667A CN2012101252316A CN201210125231A CN102634667A CN 102634667 A CN102634667 A CN 102634667A CN 2012101252316 A CN2012101252316 A CN 2012101252316A CN 201210125231 A CN201210125231 A CN 201210125231A CN 102634667 A CN102634667 A CN 102634667A
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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
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Abstract
The invention relates to a method for recycling rear-earth elements form abandoned fluorescent lamps, wherein the method comprises the following steps of: breaking abandoned energy-saving lamps; separating fluorescent powder; and recycling rear-earth elements from the fluorescent powder. According to the invention, the method specifically comprises the following steps of: firstly breaking the abandoned energy-saving lamps mechanically in an enclosed container; separating the fluorescent powder out of the abandoned fluorescent lamps through a simple mechanical separation method; separating and recycling the rear-earth elements and other useful elements through carrying out a two-step acid dissolution method and adding oxalate for precipitation; fusing and refining solid powder insoluble in acid by using alkali metal carbonate; and then processing simply. Through the method provided by the invention, the reasonable recycling of all rear-earth element compositions in the abandoned energy-saving lamps can be realized, the rear-earth resources are expected to be comprehensively recycled maximally, and the method is simple and has wide application prospect.
Description
Technical field
The present invention relates to a kind of method that all kinds of discarded fluorescent lamps comprise middle-weight rare earths elements such as electricity-saving lamp, efficient straight tube fluorescent lamp, three-color fluorescent lamp of recycling, belong to the method that a kind of environment protection and electron wastes resource utilization are recycled.
Background technology
At present, China's electric consumption on lighting amount has accounted for the 7-8% of total electricity consumption.According to " Chinese Green Lighting Project " that China proposes, illuminating energy-saving has become energy-conservation importance.Economize on electricity is under the prerequisite that guarantees illumination, promotes the efficient energy-saving lighting utensil, improves utilization rate of electrical, reduces power consumption.Therefore the incandescent light of tradition use because power consumption is high, is substituted by efficient straight tube fluorescent lamp, electricity-saving lamp, rare-earth trichromatic luminescent lamp gradually, becomes the light source of illumination consumption maximum.Meanwhile, the mercury in the discarded fluorescent lamp, lead and three kinds of materials of arsenic might cause serious pollution to environment, and owing to the scarcity of REE, the contained REE of three-color fluorescent lamp is expected to obtain recycle through otherwise effective technique on the other hand.Therefore, from the angle of environmental protection and recycling economy, must recycle and resource circulation utilization all kinds of luminescent lamps of depleted.
Present few to the recovery research report of discarded fluorescent lamp middle-weight rare earths element both at home and abroad, and domestic more research concern is to reclaim the toxic pollutant mercury (like CN1902723) in the luminescent lamp, decomposes fluorescent material though there is domestic patent (CN101150032) to report through chlorination; Form rare earth chloride and recycle REE, but have secondary environmental pollution problem and processing cost height, do not possess industrialized possibility; Also have patent (CN101307391A) report to adopt alkali to dissolve, the acid neutralization is used in the back, and extracts with extraction agent; After precipitate and separate; Obtain the rare-earth fluorescent powder mixture, complex steps, the prospect that also is difficult to carry out industrialization.External report reclaims the method for fluorescent material; The general selective dissolution fluorescent RE powder that adopts separates through sedimentary method again, and the problem of existence mainly is the co-precipitation of calcium and terbium; The fluorescent RE powder mass-limited (DE-A 34 10 989, and DD-A246 551) that makes extraction; Also have method to adopt selective dissolution impurity, separate the purification fluorescent RE powder, the problem of existence mainly is the problem of thin glass slag and fluorescent RE powder coexistence, makes fluorescent RE powder utilize limited (DE-A 196 17 942) again.
Summary of the invention
The purpose of this invention is to provide a kind of easy, effective method of from discarded fluorescent lamp, extracting REE, REE is extracted the back utilize again as fluorescent material, turn waste into wealth, the realization resource circulation is utilized again.
A kind of method of from discarded fluorescent lamp, recycling REE mainly may further comprise the steps:
The discarded electricity-saving lamp of Mechanical Crushing in airtight container, behind the adding zero(ppm) water, the large power supersonic concussion fully comes off fluorescent material, and wet method is crossed 80 purpose sieves, the fluorescent material in the separated and collected old and useless fluorescent lamp.Should contain halogen calcium phosphate fluoressent powder, rare-earth trichromatic fluorescent powder in the fluorescent material.
Take by weighing a certain amount of fluorescent material, add cold Hydrogen chloride, after fully soaking, filter, separate and contain AlCl
3, SiCl
4, SbCl
3, HgCl
2, PbCl
2, BaCl
2Solution, obtain solid sample A.
A puts into Glass Containers with solid sample, adds certain density hydrochloric acid, at a certain temperature, refluxes and soaks, and separation solution B obtains solid sample B.
With solid sample B, mix with an amount of yellow soda ash, after stirring, in porcelain crucible.
With the porcelain crucible that mixture is housed, place and carry out high-temperature calcination in the retort furnace, product is used earlier water washing, and the back is with the Hydrogen chloride washing, and remaining solid sample is the oxide compound that contains La, Eu, Ce and Tb.
Solution B is used oxalic acid precipitation earlier, and high-temperature calcination can contain the rare earth oxide of Y and Ce again.
A kind of method of from discarded fluorescent lamp, recycling REE of the present invention; Be primarily characterized in that: isolate the fluorescent material in the discarded fluorescent lamp through simple mechanical phonograph recorder separation; Then through two step acid pasting; And add the Separation and Recovery that oxalic acid precipitation can be realized REE and other useful element subsequently; And solid sample can pass through the alkalimetal oxide high-temperature fusion, further extracts the REE of high value such as the oxide compound of Tb, realizes that the maximum of rare-earth fluorescent element resource is recycled.
The present invention compared with prior art has the following advantages:
1) after the fragmentation, auxiliary use is powerful ultrasonic, realizes that waste fluorescent lamp middle-weight rare earths fluorescent material farthest comes off, separates.
2) recycling of various REEs in the realization fluorescent RE powder makes the rare earth resources circulation maximize.
3) reaction is simple and convenient, is easy to apply.
Description of drawings
Fig. 1 is a synoptic diagram of from discarded fluorescent lamp, recycling REE.
Embodiment
Embodiment 1:
(1) with crusher discarded fluorescent lamp is broken into the fragment about 2 mm, adds certain zero(ppm) water then, liquid level did not have glass fragment; Use plug-type ultrasonator; Realize peeling off of fluorescent material, wet method is crossed 80 purpose sieves, the fluorescent material in the separated and collected old and useless fluorescent lamp.
(2) fluorescent material is put into flask, add the hydrochloric acid of 0.1M, soaked 2 hours under the room temperature; The filtering separation deposition; The hydrochloric acid that adds 1M, 80 ° of C refluxed reactions 2 hours, fluorescent RE powders such as the solution that filtering separation obtains containing REE and some undissolvable phosphoric acid salt.
(3) in the solution that contains REE, add saturated oxalic acid solution, obtain the REE deposition, filtering separation, calcining is one hour under 400 ° of C, obtains high-quality rare-earth oxide phosphor.
(4) with the solid sample in the step (2), in ratio and the Na of 1:1
2CO
3Mixing is inserted in the porcelain crucible, is placed on calcining in the retort furnace; Temperature is controlled at 900 ° of C, calcines after 3 hours, and pressed powder is with the oxide compound of zero(ppm) water flush away solubility; Wash with 0.1M Hydrogen chloride again, the flush away basic oxide, remaining at last pressed powder is a rare-earth oxide phosphor.
Embodiment 2:
Other content and operation are with embodiment 1, and different is that in the step (2), temperature is 90 ° of C back flow reaction 1 hour, also can realize containing the solution of REE and separating of some undissolvable fluorescent RE powders; In the step (3), calcining temperature is 300 ° of C two hours, also can obtain high-quality rare-earth oxide phosphor; In the step (4), calcining temperature is 1000 ° of C, calcines 2 hours, also can obtain high-quality rare-earth oxide phosphor.
Claims (2)
1. method of from discarded fluorescent lamp, recycling REE; Be primarily characterized in that: isolate the fluorescent material in the discarded fluorescent lamp through simple mechanical phonograph recorder separation; Then go on foot acid pasting, and add the Separation and Recovery that oxalic acid precipitation can be realized REE and other useful element subsequently through two.
2. a kind of method of from discarded fluorescent lamp, recycling REE as claimed in claim 1; Its principal character also is: through s.t.; The solid sample that is insoluble to acid can pass through the alkalimetal oxide high-temperature fusion; Further extract the REE of high value such as the oxide compound of Tb, realize that the maximum of rare-earth fluorescent element resource is recycled.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101252316A CN102634667A (en) | 2012-04-26 | 2012-04-26 | Method for recycling rear-earth elements form abandoned fluorescent lamps |
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|---|---|---|---|
| CN2012101252316A CN102634667A (en) | 2012-04-26 | 2012-04-26 | Method for recycling rear-earth elements form abandoned fluorescent lamps |
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| CN102634667A true CN102634667A (en) | 2012-08-15 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131862A (en) * | 2013-03-13 | 2013-06-05 | 龙南县中利再生资源开发有限公司 | Pretreatment decomposition method for extracting high-purity rare earth oxide from phosphor powder waste material |
| CN103436719A (en) * | 2013-08-29 | 2013-12-11 | 湖南稀土金属材料研究院 | Lutetium oxide recovered from cerium-doped lutetium aluminate scintillation crystal waste and recovery method |
| CN104593608A (en) * | 2015-02-02 | 2015-05-06 | 上海第二工业大学 | Method for intensified leaching of rare earth metals from waste fluorescent powder by mechanical activation method |
| CN105039698A (en) * | 2015-04-21 | 2015-11-11 | 南京林业大学 | Method of high-effectively recycling rare earth from waste CRT fluorescent powder |
| CN105568005A (en) * | 2015-12-31 | 2016-05-11 | 瑞科稀土冶金及功能材料国家工程研究中心有限公司 | Method for recycling rare earth from waste fluorescent powder |
| 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 |
| CN112264037A (en) * | 2020-10-21 | 2021-01-26 | 优赛环保工程(天津)有限公司 | Method for preparing ozonolysis catalyst by using waste LED lamp beads, ozonolysis catalyst prepared by method and application of ozonolysis catalyst |
| TWI812218B (en) * | 2022-05-12 | 2023-08-11 | 國立臺北科技大學 | Phosphor powder separation and purification method |
-
2012
- 2012-04-26 CN CN2012101252316A patent/CN102634667A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 石富主编: "《稀土冶金技术》", 30 April 2009, 冶金工业出版社 * |
| 解科峰: "废弃荧光灯无害化、资源化回收处理研究", 《中国优秀硕士学位论文全文数据库》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131862A (en) * | 2013-03-13 | 2013-06-05 | 龙南县中利再生资源开发有限公司 | Pretreatment decomposition method for extracting high-purity rare earth oxide from phosphor powder waste material |
| CN103131862B (en) * | 2013-03-13 | 2016-09-14 | 龙南县中利再生资源开发有限公司 | Pretreatment decomposition method extracts high purity rare earth oxides from fluorescent powder scrap |
| CN103436719A (en) * | 2013-08-29 | 2013-12-11 | 湖南稀土金属材料研究院 | Lutetium oxide recovered from cerium-doped lutetium aluminate scintillation crystal waste and recovery method |
| CN104593608A (en) * | 2015-02-02 | 2015-05-06 | 上海第二工业大学 | Method for intensified leaching of rare earth metals from waste fluorescent powder by mechanical activation method |
| CN104593608B (en) * | 2015-02-02 | 2017-03-22 | 上海第二工业大学 | Method for intensified leaching of rare earth metals from waste fluorescent powder by mechanical activation method |
| CN105039698A (en) * | 2015-04-21 | 2015-11-11 | 南京林业大学 | Method of high-effectively recycling rare earth from waste CRT fluorescent powder |
| CN105568005A (en) * | 2015-12-31 | 2016-05-11 | 瑞科稀土冶金及功能材料国家工程研究中心有限公司 | Method for recycling rare earth from waste fluorescent powder |
| 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 |
| CN112264037A (en) * | 2020-10-21 | 2021-01-26 | 优赛环保工程(天津)有限公司 | Method for preparing ozonolysis catalyst by using waste LED lamp beads, ozonolysis catalyst prepared by method and application of ozonolysis catalyst |
| CN112264037B (en) * | 2020-10-21 | 2023-04-07 | 优赛环保工程(天津)有限公司 | Method for preparing ozonolysis catalyst by using waste LED lamp beads, ozonolysis catalyst prepared by method and application of ozonolysis catalyst |
| TWI812218B (en) * | 2022-05-12 | 2023-08-11 | 國立臺北科技大學 | Phosphor powder separation and purification method |
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Application publication date: 20120815 |