CN101942298B - Method for regenerating rare earth trichromatic fluorescent powder for lamp - Google Patents
Method for regenerating rare earth trichromatic fluorescent powder for lamp Download PDFInfo
- Publication number
- CN101942298B CN101942298B CN2010102952326A CN201010295232A CN101942298B CN 101942298 B CN101942298 B CN 101942298B CN 2010102952326 A CN2010102952326 A CN 2010102952326A CN 201010295232 A CN201010295232 A CN 201010295232A CN 101942298 B CN101942298 B CN 101942298B
- Authority
- CN
- China
- Prior art keywords
- fluorescent powder
- rare earth
- lamp
- powder
- regenerating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
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, particularly a kind of method of regenerating rare earth trichromatic fluorescent powder for lamp.
Background technology
Compare with incandescent light, electricity-saving lamp has advantages of energy-efficient, by consumers in general are accepted, becomes gradually the illuminating product of main flow.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 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, such 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 again be applied to as luminescent material the production of energy-conservation lamp, therefore present stage, the recycling of electricity-saving lamp mainly concentrates on the recycling of lamp itself and fluorescent material rare earth elements, 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 such 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 rare earth element in waste florescent lamps, it is characterized in that with highly basic melting fluorescent material, again with acid dissolving insolubles, again with extraction, the 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 again be applied to the manufacturing of LED as luminescent material through simple process.A kind of method that reclaims fluorescent powders of light emitting diode is disclosed such as CN101649197.Mainly be to utilize solvent cleaning and dry 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.
Above 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 with fluorescent RE powder of regenerating.
The technical solution used in the present invention is:
A kind of method of regenerating rare earth trichromatic fluorescent powder for lamp comprises the steps:
A) will clean up with washings through the recovery fluorescent material that sieves, removes magnetic impurity;
B) with the fluorescent powder ball-milling that cleans up, sieve, drying;
C) fluorescent material with drying reduces in reducing atmosphere;
D) fluorescent material with reduction sieves, and calcining is sieved the fluorescent material that obtains regenerating after calcining is finished.
Preferably, the temperature of reduction is 500～800 ℃, and the time of reduction is 0.5～3 hour.
Preferably, the temperature of calcining is 300～600 ℃, and the time of calcining is 0.5～3 hour.
In the cleaning process, the temperature of the washings of cleaning at least one times is not less than 90 ℃, to guarantee cleaning performance.
The present invention has realized the low cost regeneration of lamp phosphor.The fluorescent material of regeneration, under close colour temperature, the light efficiency difference only has 5～15%, and regeneration effect is better.The fluorescent material that regeneration obtains can directly apply to the manufacturing of lamp.
Embodiment
Below in conjunction with embodiment, further specify the present invention.
A kind of method of regenerating rare earth trichromatic fluorescent powder for lamp comprises the steps:
A) will clean up with washings through the recovery fluorescent material that sieves, removes magnetic impurity;
B) with the fluorescent powder ball-milling that cleans up, sieve, drying;
C) fluorescent material with drying reduces in reducing atmosphere;
D) fluorescent material with reduction sieves, and calcining is sieved the fluorescent material that obtains regenerating after calcining is finished.
Preferably, the temperature of reduction is 500～800 ℃, and the time of reduction is 0.5～3 hour.
Preferably, the temperature of calcining is 300～600 ℃, and the time of calcining is 0.5～3 hour.
In the cleaning process, the temperature of the washings of cleaning at least one times is not less than 90 ℃, to guarantee cleaning performance.
Embodiment 1
A) get the waste phosphor powder 500g that produces in the lamp factory production process 250 mesh sieves that wet, remove large granular impurity, magnetic impurity is removed in afterwards magnetic separation, is recycled 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, then after stirring 20min, 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 in the ratio ball milling 30min of powder: glass sphere=1:1, sieve, drying;
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 waste phosphor powder 500g of the removal of mercury 250 mesh sieves that wet, remove large granular impurity, magnetic impurity is removed in afterwards magnetic separation, is recycled 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, then after stirring 20min, 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 in the ratio ball milling 60min of powder: glass sphere=1:2, sieve, drying;
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 waste phosphor powder 500g of the removal of mercury 250 mesh sieves that wet, remove large granular impurity, magnetic impurity is removed in afterwards magnetic separation, is recycled 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, then after stirring 20min, 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 again 2L, 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 in the ratio ball milling 60min of powder: glass sphere=1:2, sieve, drying;
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 lamp Data Comparison with new powder
As can be known from the table data, the regeneration fluorescent material through the inventive method obtains can directly apply to the making of luminescent lamp.
Claims (8)
1. the method for a regenerating rare earth trichromatic fluorescent powder for lamp comprises the steps:
A) will clean up with washings through the recovery fluorescent material that sieves, removes magnetic impurity;
B) with the fluorescent powder ball-milling that cleans up, sieve, drying;
C) fluorescent material with drying reduces in reducing atmosphere;
D) fluorescent material with reduction sieves, and calcining is sieved the fluorescent material that obtains regenerating after calcining is finished.
2. the method for a kind of regenerating rare earth trichromatic fluorescent powder for lamp according to claim 1, it is characterized in that: the temperature of reduction is 500～800 ℃.
3. the method for a kind of regenerating rare earth trichromatic fluorescent powder for lamp according to claim 1, it is characterized in that: the time of reduction is 0.5～3 hour.
4. the method for a kind of regenerating rare earth trichromatic fluorescent powder for lamp according to claim 1, it is characterized in that: the temperature of calcining is 300～600 ℃.
5. the method for a kind of regenerating rare earth trichromatic fluorescent powder for lamp according to claim 1, it is characterized in that: the time of calcining is 0.5～3 hour.
6. the method for a kind of regenerating rare earth trichromatic fluorescent powder for lamp according to claim 1 is characterized in that: washings is at least a in water, hydrogen peroxide and the organic solvent.
7. the method for a kind of regenerating rare earth trichromatic fluorescent powder for lamp according to claim 6, it is characterized in that: organic solvent is selected from ethanol, acetone, cyclohexanone, benzene, chloroform, acetic acid.
8. the method for a kind of regenerating rare earth trichromatic fluorescent powder for lamp according to claim 1, it is characterized in that: in the cleaning process, the temperature of the washings of cleaning at least one times is not less than 90 ℃.
Priority Applications (1)
| 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 |
Applications Claiming Priority (1)
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101942298A CN101942298A (en) | 2011-01-12 |
| CN101942298B true CN101942298B (en) | 2013-02-13 |
Family
ID=43434508
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102952326A Active CN101942298B (en) | 2010-09-29 | 2010-09-29 | Method for regenerating rare earth trichromatic fluorescent powder for lamp |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101942298B (en) |
Families Citing this family (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 (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Family Cites Families (1)
| 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 |
-
2010
- 2010-09-29 CN CN2010102952326A patent/CN101942298B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2004-238526A 2004.08.26 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101942298A (en) | 2011-01-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102496545B (en) | Method for recovery of rare earths from fluorescent lamps | |
| CN102643992B (en) | Method for recovering rare-earth waste material | |
| CN101942298B (en) | Method for regenerating rare earth trichromatic fluorescent powder for lamp | |
| CN1319853C (en) | Process for preparing quartz sand using quartz gravel | |
| CN104576848B (en) | The method that gallium is reclaimed from waste and old gallium nitride based light emitting diode | |
| CN103627906B (en) | The synthetical recovery treatment process of useless rare-earth fluorescent light | |
| CN103288116B (en) | Method for preparing high-purity calcium hydroxide from carbide slag | |
| WO2011106167A1 (en) | Rare earth recovery from fluorescent material and associated method | |
| CN107630143A (en) | Method for extracting rare earth from rare earth fluorescent powder waste and fluorine-containing rare earth electrolysis waste residue | |
| CN102634667A (en) | Method for recycling rear-earth elements form abandoned fluorescent lamps | |
| KR101381728B1 (en) | Method for recycling abrasive used for sapphire wafer lapping drive | |
| CN101200638B (en) | Regeneration method of phosphor for rear earth three primary colors lamp | |
| CN104593608A (en) | Method for intensified leaching of rare earth metals from waste fluorescent powder by mechanical activation method | |
| CN104532012B (en) | Produce from gallium nitride chip and waste material reclaims gallium, the method for gold | |
| CN110629055A (en) | Method for recovering rare earth oxide from fluorescent powder waste | |
| CN109439891B (en) | Method for recycling rare earth from LED fluorescent powder silica gel waste | |
| CN112317101B (en) | Physical separation system for metal impurities in broken waste glass | |
| CN103773357A (en) | Method for removing glass residue and silicon aluminum oxide in waste rare earth phosphor | |
| CN103985620B (en) | A kind of recoverying and utilizing method of waste fluorescent lamp | |
| CN105568005A (en) | Method for recycling rare earth from waste fluorescent powder | |
| CN101565617A (en) | Method for regenerating UV excitation rare-earth phosphor | |
| CN110627104A (en) | Method for preparing high-purity rare earth oxide by recovering fluorescent powder waste | |
| Pan et al. | Recovery of Y and Eu from waste phosphors of CRT TVs and the preparation of yttrium europium oxide | |
| CN114427041A (en) | Method for recovering cerium and terbium from waste rare earth-based aluminate fluorescent powder through selective vulcanization-flotation separation | |
| CN103374661B (en) | Method for extracting rare and noble metals from waste LED (light-emitting diode) lamps |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |