CN101942298A - Method for regenerating rare earth trichromatic fluorescent powder for lamp - Google Patents
Method for regenerating rare earth trichromatic fluorescent powder for lamp Download PDFInfo
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- CN101942298A CN101942298A CN2010102952326A CN201010295232A CN101942298A CN 101942298 A CN101942298 A CN 101942298A CN 2010102952326 A CN2010102952326 A CN 2010102952326A CN 201010295232 A CN201010295232 A CN 201010295232A CN 101942298 A CN101942298 A CN 101942298A
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- fluorescent powder
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- fluorescent material
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
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Abstract
The invention discloses a method for regenerating rare earth trichromatic fluorescent powder for a lamp. The method comprises the following steps of: cleaning sieved and magnetic impurity-removed reclaimed fluorescent powder with cleaning solution; performing ball-milling on the cleaned fluorescent powder, sieving and drying; reducing dry fluorescent powder under a reducing atmosphere; sieving and calcining the reduced fluorescent powder; and sieving the calcined fluorescent powder to obtain regenerated fluorescent powder. The method realizes the low cost regeneration of fluorescent powder for the lamp. The regenerated fluorescent powder has only 5 to 15 percent of light efficiency difference at a similar color temperature and good regeneration effect and can be directly applied to the manufacturing of the lamp. The reclamation method has low cost, realizes the low cost reutilization of rare earth fluorescent powder and effectively recycles precious rare earth resources.
Description
Technical field
The present invention relates to a kind of recycling method of fluorescent material, the particularly a kind of method of lamp of regenerating with rare-earth trichromatic fluorescent powder.
Background technology
Compare with incandescent light, electricity-saving lamp has energy-efficient advantage, by consumers in general are accepted, becomes the illuminating product of main flow gradually.Common electricity-saving lamp has low pressure mercury lamp.The luminescent material that uses in the electricity-saving lamp is rare earth luminescent material.
According to statistic data, 2009, only the output of China's electricity-saving lamp just reaches about 3,800,000,000, accounts for 1/3rd of world wide production, uses fluorescent RE powder to reach about 6000 tons, and wherein rare earths material is about 3000 tons.Rare earth element is important non-renewable strategic resource, and along with the exploitation utilization of rare earth resources, the price of rare earth element also goes up thereupon, and China limits the exploitation and the outlet of rare earth, more reasonably to utilize limited rare earth resources.
Lamp phosphor generally forms by multiple fluorescent material is composite, as common energy-conservation lamp phosphor, generally by Y
2O
3: Eu(rouge and powder), CeMgAl
11O
19: the green powder of Tb() and BaMgA
L1O
17: Eu, Mn(blue powder) composition such as, complicated component, as without suitable processing, can't be applied to the production of energy-conservation lamp as luminescent material again, so present stage, the recycling of electricity-saving lamp mainly concentrates on the recycling of lamp itself and fluorescent material middle-weight rare earths element, also easily causes secondary pollution in the removal process of this rare earth element.
Disclose a kind of method of recovering and processing discarded fluorescent lamp as CN101150032, comprised the cutting of luminescent lamp, the recovery of mercury, the recovery of lamp holder metal and the pyrogenic process Separation and Recovery of the rare earth element in the fluorescent RE powder.Do not relate to the direct reclaiming of fluorescent material.
CN100577830C discloses a kind of method that reclaims discarded fluorescent lamp middle-weight rare earths element, it is characterized in that with highly basic fusion fluorescent material, again with acid dissolving insolubles, again with extraction, methods such as co-precipitation reclaim various valuable metal elements, also are the direct reclaimings that does not relate to fluorescent RE powder.
The composition of LED lamp phosphor is comparatively simple, generally can be applied to the manufacturing of LED again as luminescent material through simple process.A kind of method that reclaims fluorescent powders of light emitting diode is disclosed as CN101649197.Mainly be to utilize solvent cleaning and exsiccant method regeneration fluorescent powders of light emitting diode.Do not relate to the recycling of fluorescent-lamp-use fluorescent RE powder.
Also have the patent WO2005064637-A1 of Samsung Electronics that the mercury in the LCD fluorescent material has been carried out the pyrogenic process recovery, Japanese Patent JP2005096821-A, JP2005132551-A are respectively that the disintegrating apparatus of discarded fluorescent lamp is studied; JP2004238526-A recycles the fluorescent material in the discarded light source, but the main recovery that relates to halogen-phosphate fluorescent material etc., most patent mainly concentrates on the recovery of light source, and shorter mention is to the direct reclaiming of fluorescent material.
More than these recovery methods no doubt can reclaim a part of resource, but its comprehensive cost recovery is higher.
Summary of the invention
The object of the present invention is to provide a kind of method of lamp of regenerating with fluorescent RE powder.
The technical solution used in the present invention is:
A kind of lamp of regenerating method of rare-earth trichromatic fluorescent powder comprises the steps:
A) will clean up with washings through the recovery fluorescent material that sieves, removes magnetic impurity;
B), sieve, drying with the fluorescent material ball milling that cleans up;
C) exsiccant fluorescent material is reduced in reducing atmosphere;
D) reductive fluorescent material is sieved, calcining is sieved after calcining is finished, and obtains regenerated fluorescent material.
Preferably, the reductive temperature is 500～800 ℃, and the reductive time is 0.5～3 hour.
Preferably, the incinerating temperature is 300～600 ℃, and the incinerating time is 0.5～3 hour.
In the cleaning process, the temperature of the washings of cleaning at least once is not less than 90 ℃, to guarantee cleaning performance.
The present invention has realized the low cost regeneration of lamp phosphor.Regenerated fluorescent material, under close colour temperature, the light efficiency difference has only 5～15%, and regeneration effect is better.The fluorescent material that obtains of regeneration can directly apply to the manufacturing of lamp.
Embodiment
Below in conjunction with embodiment, further specify the present invention.
A kind of lamp of regenerating method of rare-earth trichromatic fluorescent powder comprises the steps:
A) will clean up with washings through the recovery fluorescent material that sieves, removes magnetic impurity;
B), sieve, drying with the fluorescent material ball milling that cleans up;
C) exsiccant fluorescent material is reduced in reducing atmosphere;
D) reductive fluorescent material is sieved, calcining is sieved after calcining is finished, and obtains regenerated fluorescent material.
Preferably, the reductive temperature is 500～800 ℃, and the reductive time is 0.5～3 hour.
Preferably, the incinerating temperature is 300～600 ℃, and the incinerating time is 0.5～3 hour.
In the cleaning process, the temperature of the washings of cleaning at least once is not less than 90 ℃, to guarantee cleaning performance.
Embodiment 1
A) get the discarded fluorescent material 500g that produces in the lamp factory production process 250 mesh sieves that wet, remove large granular impurity, magnetic impurity is removed in magnetic separation afterwards, obtains reclaiming powder;
B) adding 100ml concentration in reclaiming powder is the acetum of 1mol/L, add water the powder volume of slurry is increased to 2L, after stirring 20min then, leave standstill, wait the layering of powder slurry after, the turbid liquid in upper strata is outwelled, and then to add 100ml concentration be 95% ethanol, adds water to 2L again, stir 20min after, leave standstill, after the layering of powder slurry, the turbid liquid in upper strata is outwelled, and then added water to 2L, be heated to water temp greater than more than 90 ℃, after stirring 20min, leave standstill, wait the layering of powder slurry after, the turbid liquid in upper strata is outwelled, obtained the recovery powder slurry that lower floor cleans up;
C) will reclaim powder slurry ratio ball milling 30min, sieve, drying in powder: glass sphere=1:1;
D) with dry powder in 600 ℃, H
2(5%)/N
2(95%) reduction is 1 hour in the reducing atmosphere;
E) powder after will reducing is calcined 30min in 500 ℃, air atmosphere, sieves, and obtains the fluorescent material of regenerating.
Embodiment 2
A) get from discarded light fixture and reclaim and the discarded fluorescent material 500g of the removal of mercury 250 mesh sieves that wet, remove large granular impurity, magnetic impurity is removed in magnetic separation afterwards, obtains reclaiming powder;
B) adding 100ml concentration in reclaiming powder is the hydrogen peroxide solution of 1mol/L, add water the powder volume of slurry is increased to 2L, after stirring 20min then, leave standstill, wait the layering of powder slurry after, the turbid liquid in upper strata is outwelled, and then to add 100ml concentration be the benzole soln of 1mg/ml, adds water to 2L again, stir 20min after, leave standstill, after the layering of powder slurry, the turbid liquid in upper strata is outwelled, and then added water to 2L, be heated to water temp greater than more than 90 degrees centigrade, after stirring 20min, leave standstill, wait the layering of powder slurry after, the turbid liquid in upper strata is outwelled the recovery powder slurry that obtains cleaning up;
C) will reclaim powder slurry ratio ball milling 60min, sieve, drying in powder: glass sphere=1:2;
D) with dry powder in 500 ℃, H
2(5%)/N
2(95%) reduction is 3 hours in the reducing atmosphere;
E) powder after will reducing is calcined 60min in 600 ℃, air atmosphere, sieves, and obtains the fluorescent material of regenerating.
Embodiment 3
A) get from discarded light fixture and reclaim and the discarded fluorescent material 500g of the removal of mercury 250 mesh sieves that wet, remove large granular impurity, magnetic impurity is removed in magnetic separation afterwards, obtains reclaiming powder;
B) adding 100ml concentration in reclaiming powder is the hydrogen peroxide solution of 1mol/L, add water the powder volume of slurry is increased to 2L, after stirring 20min then, leave standstill, wait the layering of powder slurry after, the turbid liquid in upper strata is outwelled, and then the benzole soln of adding 100ml, add water to 2L again, behind the stirring 20min, leave standstill, after the layering of powder slurry, the turbid liquid in upper strata is outwelled, and then added water to 2L, be heated to water temp greater than more than 90 degrees centigrade, after stirring 20min, leave standstill, wait the layering of powder slurry after, the turbid liquid in upper strata is outwelled the recovery powder slurry that obtains cleaning up;
C) will reclaim powder slurry ratio ball milling 60min, sieve, drying in powder: glass sphere=1:2;
D) with dry powder in 800 ℃, NH
3Reduce 30min in the reducing atmosphere;
E) calcining 3 hours in 300 ℃, air atmosphere of the powder after will reducing is sieved, and obtains the fluorescent material of regenerating.
With the regeneration fluorescent material that above embodiment obtains, the brand-new fluorescent material close with colour temperature is made luminescent lamp with processing condition in the same way, and its luminescent properties contrast is as shown in the table.
Table 1 reclaims powder and becomes the contrast of lamp data with new powder
As can be known from the table data, through the regeneration fluorescent material that the inventive method obtains, can directly apply to the making of luminescent lamp.
Claims (8)
1. the method for lamp usefulness rare-earth trichromatic fluorescent powder of regenerating comprises the steps:
A) will clean up with washings through the recovery fluorescent material that sieves, removes magnetic impurity;
B), sieve, drying with the fluorescent material ball milling that cleans up;
C) exsiccant fluorescent material is reduced in reducing atmosphere;
D) reductive fluorescent material is sieved, calcining is sieved after calcining is finished, and obtains regenerated fluorescent material.
2. a kind of lamp of regenerating according to claim 1 method of rare-earth trichromatic fluorescent powder, it is characterized in that: the reductive temperature is 500～800 ℃.
3. a kind of lamp of regenerating according to claim 1 method of rare-earth trichromatic fluorescent powder, it is characterized in that: the reductive time is 0.5～3 hour.
4. a kind of lamp of regenerating according to claim 1 method of rare-earth trichromatic fluorescent powder, it is characterized in that: the incinerating temperature is 300～600 ℃.
5. a kind of lamp of regenerating according to claim 1 method of rare-earth trichromatic fluorescent powder, it is characterized in that: the incinerating time is 0.5～3 hour.
6. a kind of lamp of regenerating according to claim 1 is characterized in that with the method for rare-earth trichromatic fluorescent powder: scavenging solution is at least a in water, hydrogen peroxide, acetic acid and the organic solvent.
7. a kind of lamp of regenerating according to claim 6 method of rare-earth trichromatic fluorescent powder, it is characterized in that: organic solvent comprises ethanol, acetone, cyclohexanone, benzene, chloroform.
8. a kind of lamp of regenerating according to claim 1 method of rare-earth trichromatic fluorescent powder, it is characterized in that: in the cleaning process, the temperature of the washings of cleaning at least once is not less than 90 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102952326A CN101942298B (en) | 2010-09-29 | 2010-09-29 | Method for regenerating rare earth trichromatic fluorescent powder for lamp |
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|---|---|---|---|
| CN2010102952326A CN101942298B (en) | 2010-09-29 | 2010-09-29 | Method for regenerating rare earth trichromatic fluorescent powder for lamp |
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| Publication Number | Publication Date |
|---|---|
| CN101942298A true CN101942298A (en) | 2011-01-12 |
| CN101942298B CN101942298B (en) | 2013-02-13 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329616A (en) * | 2011-07-18 | 2012-01-25 | 江苏石诺节能科技股份有限公司 | Fluorescent powder special for energy-saving lamp in broiler farm |
| CN102983047A (en) * | 2012-11-28 | 2013-03-20 | 大连东泰产业废弃物处理有限公司 | Waste fluorescent lamp handling method |
| CN105694843A (en) * | 2014-11-25 | 2016-06-22 | 广东雪莱特光电科技股份有限公司 | Phosphor recovering treatment technology |
| US10533239B2 (en) | 2016-11-01 | 2020-01-14 | Battelle Energy Alliance, Llc | Methods of recovering rare earth elements from a material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004238526A (en) * | 2003-02-06 | 2004-08-26 | Kobelco Eco-Solutions Co Ltd | Method for recycling fluorescent substance, fluorescent substance recycled by the recycling treatment method |
| CN101200638A (en) * | 2007-11-30 | 2008-06-18 | 彩虹集团电子股份有限公司 | Regeneration method of phosphor for rear earth three primary colors lamp |
-
2010
- 2010-09-29 CN CN2010102952326A patent/CN101942298B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004238526A (en) * | 2003-02-06 | 2004-08-26 | Kobelco Eco-Solutions Co Ltd | Method for recycling fluorescent substance, fluorescent substance recycled by the recycling treatment method |
| CN101200638A (en) * | 2007-11-30 | 2008-06-18 | 彩虹集团电子股份有限公司 | Regeneration method of phosphor for rear earth three primary colors lamp |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329616A (en) * | 2011-07-18 | 2012-01-25 | 江苏石诺节能科技股份有限公司 | Fluorescent powder special for energy-saving lamp in broiler farm |
| CN102983047A (en) * | 2012-11-28 | 2013-03-20 | 大连东泰产业废弃物处理有限公司 | Waste fluorescent lamp handling method |
| CN105694843A (en) * | 2014-11-25 | 2016-06-22 | 广东雪莱特光电科技股份有限公司 | Phosphor recovering treatment technology |
| US10533239B2 (en) | 2016-11-01 | 2020-01-14 | Battelle Energy Alliance, Llc | Methods of recovering rare earth elements from a material |
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| Publication number | Publication date |
|---|---|
| CN101942298B (en) | 2013-02-13 |
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