CN103773357B - A kind of method removing glass dregs and sieve and silica-sesquioxide in waste and old fluorescent RE powder - Google Patents
A kind of method removing glass dregs and sieve and silica-sesquioxide in waste and old fluorescent RE powder Download PDFInfo
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- CN103773357B CN103773357B CN201410022560.7A CN201410022560A CN103773357B CN 103773357 B CN103773357 B CN 103773357B CN 201410022560 A CN201410022560 A CN 201410022560A CN 103773357 B CN103773357 B CN 103773357B
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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 belongs to resources circulation recycling field, be specifically related to a kind of method that waste and old fluorescent RE powder removes sial impurity.Waste and old fluorescent RE powder obtains acidolysis slag through preroasting, acidolysis and press filtration successively; Acidolysis slag removes coarse particles glass dregs through waterpower sorting, then particulate glass slag in wet screening removal, and last thermokalite dissolves fine particle glass dregs and sieve and silica-sesquioxide.Of the present inventionly carse, medium and small particulate glass slag in waste and old fluorescent RE powder and other sieve and silica-sesquioxide impurity efficiently can be removed, avoiding in subsequent recovery rare earth element process affects rare earth element and leaches and extracting and separating because forming sial colloid.The present invention has sial impurity in the waste and old fluorescent RE powder of efficient removal, significantly improves rare earth yield, reduces production cost, is applicable to the features such as suitability for industrialized production.
Description
Technical field
The invention belongs to resources circulation recycling field, be specifically related to a kind of method removing glass dregs and sieve and silica-sesquioxide in waste and old fluorescent RE powder.
Background technology
The waste and old fluorescent RE powder collected generally contains sieve and silica-sesquioxide (in the aluminium sesquioxide) powder about 15% of glass dregs (in silicon-dioxide) about 25% and sealing coat.Sial impurity element forms sial colloid during acidolysis after waste and old fluorescent RE powder alkali fusion, not only reduces the leaching yield of rare earth element, and causes rare earth extraction efficiency low, causes that rare earth yield is low, cost recovery is high.
Existing waste and old fluorescent RE powder reclaims document and mainly concentrates on rare earth element recovery, and the documents and materials relating to the removal of sial impurity element are few.As Chinese invention patent CN101150032 discloses a kind of method of recovering and processing discarded fluorescent lamp, comprise the cutting of luminescent lamp, the recovery of mercury, the fire concentrate of the rare earth element in the recovery of lamp holder metal and system fluorescent material.CN100577830C discloses a kind of method reclaiming rare earth element in waste florescent lamps, it is characterized in that with highly basic melting fluorescent material, then uses acid dissolve insolubles, then reclaim various valuable metal element by methods such as extraction precipitation.CN101942298A discloses the method for regenerating rare earth trichromatic fluorescent powder for lamp, the fluorescent material of the magnetic substance impurity that sieves, removes, then to wash in drying the fluorescent material that in reducing atmosphere, reduction obtains regenerating and directly apply to manufacturing again of lamp.Japanese Patent JP2005096821-A, JP2005132551-A are that the disintegrating apparatus of discarded fluorescent lamp is studied respectively; JP2004238526-A recycles the fluorescent material in discarded light source, but is mainly concerned with the recovery etc. of halogen phosphate phosphor.
Summary of the invention
The object of the invention is for solving a sial magazins' layout difficult problem in waste and old fluorescent RE powder, a kind of method removing particulate glass slag and sieve and silica-sesquioxide in waste and old fluorescent RE powder is provided, adopt the glass dregs in physics and chemistry combined method removal fluorescent material and sieve and silica-sesquioxide impurity, improve fluorescent material alkali fusion, acidolysis and effect of extracting, greatly improve rare earth yield.This energy saving technology emission reduction effect is remarkable, and production cost is low.
Principle of the present invention can illustrate with following chemical reaction.
When alkali lye is NaOH solution:
Al
2O
3(s)+2NaOH(aq)+3H
2O=2Al(OH)
4 -(aq)+2Na
+(aq), (1)
SiO
2(s)+NaOH(aq)+2H
2O=Na
+(aq)+ Si(OH)
5 -(aq), (2)
Al
2O
3?2SiO
2?2H
2O(s)+2NaOH(aq)+5H
2O=2Al(OH)
4 - (aq)+2Si(OH)
4(aq)+2Na
+(aq), (3)
When alkali lye is KOH solution:
Al
2O
3(s)+2KOH(aq)+3H
2O=2Al(OH)
4 -(aq)+2K
+(aq), (4)
SiO
2(s)+KOH(aq)+2H
2O=K
+(aq)+ Si(OH)
5 -(aq), (5)
Al
2O
3?2SiO
2?2H
2O(s)+2NaOH(aq)+5H
2O=2Al(OH)
4 - (aq)+2Si(OH)
4(aq)+2Na
+(aq), (6)
Also there is following chemical reaction in complicated silicate and aluminates system:
xNaAlO
2(aq)+yNa
2SiO
3(aq)+(y+z)H
2O=Na
x[(AlO
2)
x(SiO
2)
y]?zH
2O+2yNaOH(aq). (7)
xKAlO
2(aq)+yK
2SiO
3(aq)+(y+z)H
2O=K
x[(AlO
2)
x(SiO
2)
y]?zH
2O+2yKOH(aq). (8)
A kind of method removing particulate glass slag and sieve and silica-sesquioxide in waste and old fluorescent RE powder of the present invention is as follows:
(1) the waste and old fluorescent RE powder collected is carried out preroasting process, temperature is 300 ~ 800 DEG C, and the treatment time is 0.5 ~ 4h, removes the organic impurities be mixed into wherein, impels glass dregs to be effectively separated with fluorescent material, obtain fired slags;
(2) fired slags obtains acidolysis slag and earth solution through acidolysis and press filtration, wherein need wash acidolysis slag with water during press filtration, make acidolysis slag not containing rare earth acidic solution, acidolysis slag adopts waterpower sorting, wet screening and sedimentation combination process, coarse particles glass dregs (>0.5mm) is wherein removed in waterpower sorting, wherein waterpower is divided and is elected swirler sorting as, the one of separation by shaking table or screw classifying sorting, sand setting is again by wet screening sorting removal middle particulate glass slag (0.05 ~ 0.5mm) wherein, the screen underflow obtained after overflow and wet screening obtains the acidolysis slag containing fine particle glass dregs and sial impurity through sedimentation filtration, wet screening size of mesh is 300 ~ 600 orders, sedimentation water returns waterpower sorting operation,
(3) containing the acidolysis slag of fine particle glass dregs (<0.05mm) and sial impurity, thermokalite is adopted to leach fine particle glass dregs and sieve and silica-sesquioxide impurity, extraction temperature is 60 ~ 100 DEG C, extraction time is 0.5 ~ 4h, solid-to-liquid ratio is 1:10 ~ 1:3, alkaline solution is one in NaOH and KOH solution or mixing solutions, alkali concn 30 ~ 60
wt%, obtains sial alkali lye and alkali cleaning slag after press filtration;
(4) thermokalite leach and the sial alkali fusion of alkali fusion after washing and rare earth reclaim after spent acid carry out neutralizing treatment and reclaim sial element.
The invention discloses preroasting, waterpower sorting, wet screening and thermokalite combination process and remove sial impurity.Organic inclusion in waste and old fluorescent RE powder is removed in preroasting, is conducive to improving waterpower separating effect.Acidolysis slag after acidolysis carries out waterpower sorting and mainly removes coarse particles glass dregs in waste and old fluorescent RE powder, wet screening mainly remove in particulate glass slag, thermokalite dissolves fine grain glass dregs and sieve and silica-sesquioxide impurity.Of the present inventionly carse, medium and small particulate glass slag in waste and old fluorescent RE powder and sieve and silica-sesquioxide impurity efficiently can be removed, to avoid in subsequent recovery rare earth element process and cause because forming sial colloid the problem that rare earth leaches and extraction efficiency is low.The present invention has glass dregs and sieve and silica-sesquioxide impurity in the waste and old fluorescent RE powder of efficient removal, significantly improves rare earth yield, reduces material usage quantity, reduce production cost, there is significant energy-saving and emission-reduction, non-secondary pollution, improve the feature such as Working environment and applicable suitability for industrialized production.
Accompanying drawing explanation
Accompanying drawing 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but the present invention is not only confined to following examples.
Embodiment 1
The waste and old fluorescent RE powder collected is carried out preroasting process, roasting 3h at 300 DEG C, fired slags obtains earth solution and acidolysis slag through peracid acidolysis, acidolysis slag adopts hydrocyclone sorting, wet screening and sedimentation combination process, coarse particles glass dregs is removed in hydrocyclone sorting, sand setting carries out particulate glass slag in the removal of sorting again by wet screening, wet screening sieve aperture is 400 orders, screen underflow after overflow and wet screening obtains the acidolysis slag containing fine particle glass dregs and sial impurity through sedimentation filtration, and sedimentation water returns hydrocyclone sorting operation.Containing the acidolysis slag of fine particle glass dregs and sial impurity, adopt 30
wtthe NaOH solution of %, leach residual fine particles glass dregs and Si oxide, solid-to-liquid ratio is 1:4, extraction temperature 90 DEG C, extraction time 1h.Alkali cleaning slag, through alkali fusion and washing process, can remove glass dregs and sieve and silica-sesquioxide impurity in waste and old fluorescent RE powder.
Embodiment 2
The waste and old fluorescent RE powder collected is carried out preroasting process, roasting 3.5h at 400 DEG C, fired slags obtains earth solution and acidolysis slag through peracid acidolysis, acidolysis slag adopts separation by shaking table, wet screening and sedimentation combination process, coarse particles glass dregs is removed in hydrocyclone sorting, sand setting carries out particulate glass slag in the removal of sorting again by wet screening, wet screening sieve aperture is 300 orders, screen underflow after overflow and wet screening obtains the acidolysis slag containing fine particle glass dregs and sial impurity through sedimentation filtration, and sedimentation water returns hydrocyclone sorting operation.Containing the acidolysis slag of fine particle glass dregs and sial impurity, adopt 30
wtthe KOH solution of %, leach residual fine particles glass dregs and Si oxide, solid-to-liquid ratio is 1:5, extraction temperature 100 DEG C, extraction time 1.5h.Alkali cleaning slag, through alkali fusion and washing process, can remove glass dregs and sieve and silica-sesquioxide impurity in waste and old fluorescent RE powder.
Embodiment 3
The waste and old fluorescent RE powder collected is carried out preroasting process, roasting 4h at 500 DEG C, fired slags obtains earth solution and acidolysis slag through peracid acidolysis, acidolysis slag adopts waterpower screw thread classification and sorting, wet screening and sedimentation combination process, coarse particles glass dregs is removed in hydrocyclone sorting, sand setting carries out particulate glass slag in the removal of sorting again by wet screening, wet screening sieve aperture is 300 orders, screen underflow after overflow and wet screening obtains the acidolysis slag containing fine particle glass dregs and sial impurity through sedimentation filtration, and sedimentation water returns hydrocyclone sorting operation.Containing the acidolysis slag of fine particle glass dregs and sial impurity, adopt 50
wtthe NaOH solution of % and the mixed solution of KOH solution, leach residual fine particles glass dregs and Si oxide, solid-to-liquid ratio is 1:6, extraction temperature 60 DEG C, extraction time 2h.Alkali cleaning slag, through alkali fusion and washing process, can remove glass dregs and sieve and silica-sesquioxide impurity in waste and old fluorescent RE powder.
Embodiment 4
The waste and old fluorescent RE powder collected is carried out preroasting process, roasting 0.5h at 600 DEG C, fired slags obtains earth solution and acidolysis slag through peracid acidolysis, acidolysis slag adopts separation by shaking table, wet screening and sedimentation combination process, coarse particles glass dregs is removed in hydrocyclone sorting, sand setting carries out particulate glass slag in the removal of sorting again by wet screening, wet screening sieve aperture is 300 orders, screen underflow after overflow and wet screening obtains the acidolysis slag containing fine particle glass dregs and sial impurity through sedimentation filtration, and sedimentation water returns hydrocyclone sorting operation.Containing the acidolysis slag of fine particle glass dregs and sial impurity, adopt 30
wtthe KOH solution of %, leach residual fine particles glass dregs and Si oxide, solid-to-liquid ratio is 1:7, extraction temperature 70 DEG C, extraction time 2.5h.Alkali cleaning slag, through alkali fusion and washing process, can remove glass dregs and sieve and silica-sesquioxide impurity in waste and old fluorescent RE powder.
Embodiment 5
The waste and old fluorescent RE powder collected is carried out preroasting process, roasting 1h at 700 DEG C, fired slags obtains earth solution and acidolysis slag through peracid acidolysis, acidolysis slag adopts waterpower screw thread classification and sorting, wet screening and sedimentation combination process, coarse particles glass dregs is removed in hydrocyclone sorting, sand setting carries out particulate glass slag in the removal of sorting again by wet screening, wet screening sieve aperture is 400 orders, screen underflow after overflow and wet screening obtains the acidolysis slag containing fine particle glass dregs and sial impurity through sedimentation filtration, and sedimentation water returns hydrocyclone sorting operation.Containing the acidolysis slag of fine particle glass dregs and sial impurity, adopt 30
wtthe NaOH solution of %, leach residual fine particles glass dregs and Si oxide, solid-to-liquid ratio is 1:8, extraction temperature 80 DEG C, extraction time 3h.Alkali cleaning slag, through alkali fusion and washing process, can remove glass dregs and sieve and silica-sesquioxide impurity in waste and old fluorescent RE powder.
Embodiment 6
The waste and old fluorescent RE powder collected is carried out preroasting process, roasting 1.5h at 800 DEG C, fired slags obtains earth solution and acidolysis slag through peracid acidolysis, acidolysis slag adopts hydrocyclone sorting, wet screening and sedimentation combination process, coarse particles glass dregs is removed in hydrocyclone sorting, sand setting carries out particulate glass slag in the removal of sorting again by wet screening, wet screening sieve aperture is 500 orders, screen underflow after overflow and wet screening obtains the acidolysis slag containing fine particle glass dregs and sial impurity through sedimentation filtration, and sedimentation water returns hydrocyclone sorting operation.Containing the acidolysis slag of fine particle glass dregs and sial impurity, adopt 40
wtthe NaOH solution of % and the mixed solution of KOH solution, leach residual fine particles glass dregs and Si oxide, solid-to-liquid ratio is 1:10, extraction temperature 50 DEG C, extraction time 4h.Alkali cleaning slag, through alkali fusion and washing process, can remove glass dregs and sieve and silica-sesquioxide impurity in waste and old fluorescent RE powder.
Embodiment 7
The waste and old fluorescent RE powder collected is carried out preroasting process, roasting 2h at 300 DEG C, fired slags obtains earth solution and acidolysis slag through peracid acidolysis, acidolysis slag adopts waterpower screw thread classification and sorting, wet screening and sedimentation combination process, coarse particles glass dregs is removed in hydrocyclone sorting, sand setting carries out particulate glass slag in the removal of sorting again by wet screening, wet screening sieve aperture is 400 orders, screen underflow after overflow and wet screening obtains the acidolysis slag containing fine particle glass dregs and sial impurity through sedimentation filtration, and sedimentation water returns hydrocyclone sorting operation.Containing the acidolysis slag of fine particle glass dregs and sial impurity, adopt 50
wtthe NaOH solution of %, leach residual fine particles glass dregs and Si oxide, solid-to-liquid ratio is 1:9, extraction temperature 100 DEG C, extraction time 0.5h.Alkali cleaning slag, through alkali fusion and washing process, can remove glass dregs and sieve and silica-sesquioxide impurity in waste and old fluorescent RE powder.
Embodiment 8
The waste and old fluorescent RE powder collected is carried out preroasting process, roasting 2.5h at 400 DEG C, fired slags obtains earth solution and acidolysis slag through peracid acidolysis, acidolysis slag adopts separation by shaking table, wet screening and sedimentation combination process, coarse particles glass dregs is removed in hydrocyclone sorting, sand setting carries out particulate glass slag in the removal of sorting again by wet screening, wet screening sieve aperture is 300 orders, screen underflow after overflow and wet screening obtains the acidolysis slag containing fine particle glass dregs and sial impurity through sedimentation filtration, and sedimentation water returns hydrocyclone sorting operation.Containing the acidolysis slag of fine particle glass dregs and sial impurity, adopt 60
wtthe K5OH solution of %, leach residual fine particles glass dregs and Si oxide, solid-to-liquid ratio is 1:9, extraction temperature 80 DEG C, extraction time 0.5h.Alkali cleaning slag, through alkali fusion and washing process, can remove glass dregs and sieve and silica-sesquioxide impurity in waste and old fluorescent RE powder.
Embodiment 9
The waste and old fluorescent RE powder collected is carried out preroasting process, roasting 3h at 400 DEG C, fired slags obtains earth solution and acidolysis slag through peracid acidolysis, acidolysis slag adopts hydrocyclone sorting, wet screening and sedimentation combination process, coarse particles glass dregs is removed in hydrocyclone sorting, sand setting carries out particulate glass slag in the removal of sorting again by wet screening, wet screening sieve aperture is 200 orders, screen underflow after overflow and wet screening obtains the acidolysis slag containing fine particle glass dregs and sial impurity through sedimentation filtration, and sedimentation water returns hydrocyclone sorting operation.Containing the acidolysis slag of fine particle glass dregs and sial impurity, adopt 30
wtthe NaOH solution of % and KOH solution mixing solutions, leach residual fine particles glass dregs and Si oxide, solid-to-liquid ratio is 1:8, extraction temperature 90 DEG C, extraction time 1.5h.Alkali cleaning slag, through alkali fusion and washing process, can remove glass dregs and sieve and silica-sesquioxide impurity in waste and old fluorescent RE powder.
Embodiment 10
The waste and old fluorescent RE powder collected is carried out preroasting process, roasting 3.5h at 600 DEG C, fired slags obtains earth solution and acidolysis slag through peracid acidolysis, acidolysis slag adopts separation by shaking table, wet screening and sedimentation combination process, coarse particles glass dregs is removed in hydrocyclone sorting, sand setting carries out particulate glass slag in the removal of sorting again by wet screening, wet screening sieve aperture is 300 orders, screen underflow after overflow and wet screening obtains the acidolysis slag containing fine particle glass dregs and sial impurity through sedimentation filtration, and sedimentation water returns hydrocyclone sorting operation.Containing the acidolysis slag of fine particle glass dregs and sial impurity, adopt 40
wtthe NaOH solution of %, leach residual fine particles glass dregs and Si oxide, solid-to-liquid ratio is 1:7, extraction temperature 70 DEG C, extraction time 2.5h.Alkali cleaning slag, through alkali fusion and washing process, can remove glass dregs and sieve and silica-sesquioxide impurity in waste and old fluorescent RE powder.
Claims (4)
1. remove a method for glass dregs and sieve and silica-sesquioxide in waste and old fluorescent RE powder, it is characterized in that comprising the following steps:
(1) waste and old fluorescent RE powder carries out preroasting, obtains fired slags;
(2) fired slags obtains acidolysis slag and earth solution through acidolysis and press filtration, acidolysis slag adopts waterpower sorting, wet screening and sedimentation combination process to carry out sorting, sorting obtains raw glass slag, overflow and sand setting, the screen underflow of overflow and wet screening obtains through sedimentation the acidolysis slag containing fine particle glass dregs and sial impurity, and sedimentation water returns waterpower sorting operation;
(3) the acidolysis slag containing fine particle glass dregs and sial impurity adopts thermokalite to leach, and obtains sial alkali lye and alkali cleaning slag through press filtration;
(4) alkali cleaning slag obtains washed-residue and sial alkali lye through alkali fusion, washing and press filtration, and washed-residue obtains rare earth and raffinate through acidolysis, extraction;
(5) sial alkali lye and raffinate reclaim sial art breading reclaim sial element through neutralizing.
2. a kind of method removing glass dregs and sieve and silica-sesquioxide in waste and old fluorescent RE powder according to claim 1, it is characterized in that: described step (1) pre-calcination temperature is 300 ~ 800 DEG C, pre-firing times is 0.5 ~ 4h.
3. a kind of method removing glass dregs and sieve and silica-sesquioxide in waste and old fluorescent RE powder according to claim 1, it is characterized in that: the waterpower in described step (2) is divided and elected swirler sorting, separation by shaking table and screw classifying as and divide the one chosen, and wet screening size of mesh is 300 ~ 600 orders.
4. a kind of method removing glass dregs and sieve and silica-sesquioxide in waste and old fluorescent RE powder according to claim 1, it is characterized in that: the extraction temperature that described step (3) thermokalite leaches fine particle glass dregs and sieve and silica-sesquioxide impurity is 60 ~ 100 DEG C, extraction time is 0.5 ~ 4h, solid-to-liquid ratio is 1:10 ~ 1:3, wherein thermokalite is one in NaOH and KOH solution or mixing solutions, and alkali concn is 30 ~ 60
wt%.
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CN104357665B (en) * | 2014-11-24 | 2016-06-15 | 北京科技大学 | The method and apparatus that the enrichment of a kind of waste and old fluorescent RE powder and residual heat integrative utilize |
CN107099254A (en) * | 2017-05-02 | 2017-08-29 | 王丹 | A kind of method of ornaments crystal glass polishing powder from rare earth regeneration |
CN109439891B (en) * | 2018-12-28 | 2020-08-11 | 虔东稀土集团股份有限公司 | Method for recycling rare earth from LED fluorescent powder silica gel waste |
CN109913638A (en) * | 2019-04-01 | 2019-06-21 | 中钢集团南京新材料研究院有限公司 | A kind of method of silicon in reduction extraction of superpure concentrate of magnetite, aluminium content |
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CN101461024A (en) * | 2006-06-02 | 2009-06-17 | 奥斯兰姆有限公司 | Method for recovery of rare earths from fluorescent lamps |
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US6531814B1 (en) * | 2000-02-17 | 2003-03-11 | General Electric Company | Fluorescent lamp coating and coating recycling method |
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2014
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CN1037429A (en) * | 1988-04-29 | 1989-11-22 | 彩色电视公司 | Recovery is used for the no-mill method of the phosphor of three-colour television picture tube |
CN101461024A (en) * | 2006-06-02 | 2009-06-17 | 奥斯兰姆有限公司 | Method for recovery of rare earths from fluorescent lamps |
Non-Patent Citations (1)
Title |
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