CN108878235A - A kind of method of discarded fluorescent lamp recycling - Google Patents

A kind of method of discarded fluorescent lamp recycling Download PDF

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Publication number
CN108878235A
CN108878235A CN201710341661.4A CN201710341661A CN108878235A CN 108878235 A CN108878235 A CN 108878235A CN 201710341661 A CN201710341661 A CN 201710341661A CN 108878235 A CN108878235 A CN 108878235A
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CN
China
Prior art keywords
fluorescent lamp
fluorescent powder
discarded
recycling
fluorescent
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Pending
Application number
CN201710341661.4A
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Chinese (zh)
Inventor
张洪武
李鹏辉
邹晓燕
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Institute of Urban Environment of CAS
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Institute of Urban Environment of CAS
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Application filed by Institute of Urban Environment of CAS filed Critical Institute of Urban Environment of CAS
Priority to CN201710341661.4A priority Critical patent/CN108878235A/en
Publication of CN108878235A publication Critical patent/CN108878235A/en
Pending legal-status Critical Current

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/52Recovery of material from discharge tubes or lamps
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/82Recycling of waste of electrical or electronic equipment [WEEE]

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The present invention relates to a kind of methods that discarded fluorescent lamp recycling is innoxious.Mainly include:It is crushed under the liquid of discarded fluorescent lamp, the extraction of fluorescent powder and the recovering rare earth element from fluorescent powder.The present invention carries out the broken of discarded fluorescent lamp first under liquid, isolates fluorescent powder after fluorescent powder drying by simple filtration and, by mechanical lapping, realizes that the particle of fluorescent powder becomes smaller;By the fluorescent powder after grinding by acidleach, soluble matter is reacted with oxalic acid, and after high-temperature calcination, part rare earth oxide can be obtained.Insoluble matter after acidleach is refined by sodium peroxide alkali fusion, after cleaning, can obtain rare earth oxide.The present invention realizes the recycling of discarded fluorescent lamp, and method is simple, reduces acid consumption, while also protecting environment.

Description

A kind of method of discarded fluorescent lamp recycling
Technical field
The invention belongs to the technical fields of electron wastes comprehensive utilization, and in particular to break under the liquid of different discarded fluorescent lamps Broken, fluorescent powder separation and the recycling of rare earth element.
Background technique
Currently, China is the production of fluorescent lamp and uses big country, only 2016, the yield of China's fluorescent lamp was broken through for the first time 10000000000, learies are also up to more than 40 hundred million.With the gradually intensification of people's environmental consciousness, green illumination theory has goed deep into people The heart, energy-efficient fluorescent lamp have gradually replaced incandescent lamp, become main electric light source in the world.Fluorescent lamp is mainly by aluminium Lid, glass tube, fluorescent powder, mercuryvapour, inert gas and copper conductive material composition.The wherein main component of three primary colors fluorescent powder For:Rouge and powder is europkium-activated yttrium oxide(Y2O3: Eu), green powder be aluminate that cerium and terbium activate(MgAl11O19:Ce, Tb)With And blue powder is the europkium-activated barium magnesium aluminate of low price(BaMg2Al16O27: Eu).Harmful substance mainly includes the huge sum of money such as mercury, arsenic, lead All to ambient enviroment and human health, there are serious threats for category and fluorescent powder.From the point of view of recycling, discard glimmering Light lamp also contains valuable rare earth element, and the conductive materials such as copper, nickel can be recycled by effective recovery method.Cause This, is recycled discarded fluorescent lamp, can be effectively protected environment, turn waste into wealth, and promotes recycling for resource.
Currently, it is less to the recovery processing research of discarded fluorescent lamp both at home and abroad, it is still at an early stage, it is asked there is also some Topic, industrial application are less.The difficult point of discarded fluorescent lamp is innoxious, fluorescent lamp the separation of the broken of discarded fluorescent lamp, mercury And Extraction of rare earth element, and some correlative studys have also been carried out both at home and abroad, still, only studied in one aspect, Lack systematic research.Patent(CN105097384A, CN203199489U, CN102145344A etc.)A kind of fluorescent lamp is invented Recyclable device forms closed environment, can be broken apart to discarded fluorescent lamp progress, but defines and return from fluorescent powder Receive rare earth;Patent(CN1902723A, CN101150032A, CN202957218U etc.)It has been solely focused on mercury in discarded fluorescent lamp Toxicity, other aspects are also that research is less;Patent(CN102496545B,CN102496545A,CN101461024B, CN102634667A etc.)The extracting method of rare earth in waste phosphor powder is reported, big but there are acid consumptions, there are secondary pollutions The problems such as.So there are still certain problems for the comprehensive utilization of discarded fluorescent lamp, industrialize also relatively difficult.
Summary of the invention
The object of the present invention is to provide the systems of the discarded fluorescent lamp recycling of complete set, reach discarded fluorescent lamp and follow Ring utilizes, and reduces the pollution to environment, meets the strategy of sustainable development.
A kind of systems approach of discarded fluorescent lamp recycling, mainly includes the following steps that:
Various types of discarded fluorescent lamp pipe is collected, discarded fluorescent lamp is put into the container equipped with a large amount of water, it is acute together Strong stirring is that discarded fluorescent lamp is broken, and large power supersonic concussion makes waste phosphor powder fall off thoroughly, crosses 60 mesh nylon mesh, separation Fluorescent powder, glass, metal and plastic cap etc..
Mercury-containing waste water passes through active carbon net, adsorption recovery mercury;Glass, metal and plastics etc. carry out special processing.It is glimmering Light powder obtains dry fluorescent powder by drying.
A certain amount of fluorescent powder is weighed, is put into ball mill, is fully ground, the particle of fluorescent powder is made to become smaller, it is spare.
A certain amount of ground fluorescent powder is weighed in glassware, certain density hydrochloric acid is added, in specific temperature Under, reaction a period of time is separated by filtration to obtain leachate A and leaches residue A.
Leachate A is reacted with oxalic acid, sediment obtains the oxide of Y and Eu through high-temperature calcination.
Solid residue A is uniformly mixed with suitable sodium peroxide, is placed in crucible, Muffle furnace calcining, it is cooling after by Water, dilute hydrochloric acid successively wash, and obtain the oxide of Ce and Tb.
After spent acid, the alkali waste water of each step generation are collected, by acid-base neutralization, discharged after reaching safety standard.
Of the invention is mainly characterized by:By being crushed under liquid, avoids mercury and direct influence is generated on environment;Separate fluorescence After powder, after mechanical lapping, the activation energy of reaction is reduced, reduces the dosage of acid;Recycling for waste phosphor powder is realized, With certain economic value.
Specific embodiment 1
Embodiment 1:
(1)Various types of discarded fluorescent lamp pipe is collected, discarded fluorescent lamp is put into the container equipped with a large amount of water(To stir It is easy that liquid, which is not spilt over, during mixing), it is vigorously stirred together, keeps discarded fluorescent lamp broken, shaken with plug-in type large power supersonic Device makes waste phosphor powder fall off thoroughly, crosses 60 mesh nylon mesh, separation fluorescent powder, glass, metal and plastics etc..
(2)Mercury-containing waste water is passed through into active carbon net, adsorption recovery mercury;Glass, metal and plastics etc. carry out special place Reason.Fluorescent powder obtains dry fluorescent powder by drying.
(3)Fluorescent powder is put into ball mill, 600 rmp of revolving speed, grinds 1 h, the particle of fluorescent powder is made to become smaller, it is spare.
(4)Ground fluorescent powder is placed in glassware, the hydrochloric acid of 1 M, liquid-solid ratio 60 is added:It is sour at 1,60 DEG C 15 min are soaked, are separated by filtration to obtain the phosphate rare earth phosphor of the solution containing rare earth element and indissoluble.
(5)The solution of rare earth element is reacted with the oxalic acid solution of saturation, obtains rare earth element precipitating, sediment is through 300 DEG C calcining 2 h, obtain the oxide of Y and Eu.
(6)By step(4)Solid sample be uniformly mixed with sodium peroxide, mass ratio 1:2, it is placed in crucible, 650 DEG C, 15 min are calcined, after cooling, basic anhydride washed off by water removal dissolvable oxides, 0.1 M hydrochloric acid, finally obtains The oxide of Ce and Tb.
Specific embodiment 2
(1)Various types of discarded fluorescent lamp pipe is collected, discarded fluorescent lamp is put into the container equipped with a large amount of water(To stir It is easy that liquid, which is not spilt over, during mixing), it is vigorously stirred together, keeps discarded fluorescent lamp broken, shaken with plug-in type large power supersonic Device makes waste phosphor powder fall off thoroughly, crosses 60 mesh nylon mesh, separation fluorescent powder, glass, metal and plastics etc..
(2)Mercury-containing waste water is passed through into active carbon net, adsorption recovery mercury;Glass, metal and plastics etc. carry out special place Reason.Fluorescent powder obtains dry fluorescent powder by drying.
(3)Fluorescent powder is put into ball mill, 800 rmp of revolving speed, grinds 40 min, the particle of fluorescent powder is made to become smaller, it is standby With.
(4)Ground fluorescent powder is placed in glassware, the hydrochloric acid of 1 M, liquid-solid ratio 60 is added:It is sour at 1,60 DEG C 15 min are soaked, are separated by filtration to obtain the phosphate rare earth phosphor of the solution containing rare earth element and indissoluble.
(5)The solution of rare earth element is reacted with the oxalic acid solution of saturation, obtains rare earth element precipitating, sediment is through 300 DEG C calcining 2 h, the oxide of Y and Eu still can be obtained.
(6)By step(4)Solid sample be uniformly mixed with sodium peroxide, mass ratio 1:2, it is placed in crucible, 650 DEG C, 15 min are calcined, after cooling, basic anhydride washed off by water removal dissolvable oxides, 0.1 M hydrochloric acid, finally also may be used Obtain the oxide of Ce and Tb.
Detailed description of the invention
Fig. 1 discarded fluorescent lamp recycling broad flow diagram.

Claims (2)

1. a kind of method of discarded fluorescent lamp recycling can be effectively reduced by fluorescent powder out broken apart under simple liquid The direct emission of mercury, obtained fluorescent powder passes through mechanical lapping, can effectively reduce acid consumption, energy saving.
2. a kind of method of discarded fluorescent lamp recycling as described in claim 1, the fluorescent powder after grinding, can after acidleach Molten object adds oxalic acid precipitation, and after high-temperature calcination, the oxide of Y and Eu can be obtained;Indissoluble object can be by sodium peroxide high temperature alkali fuse, clearly After washing, the oxide of Ce and Tb can be obtained, realize the recycling of discarded fluorescent lamp.
CN201710341661.4A 2017-05-16 2017-05-16 A kind of method of discarded fluorescent lamp recycling Pending CN108878235A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710341661.4A CN108878235A (en) 2017-05-16 2017-05-16 A kind of method of discarded fluorescent lamp recycling

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710341661.4A CN108878235A (en) 2017-05-16 2017-05-16 A kind of method of discarded fluorescent lamp recycling

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CN108878235A true CN108878235A (en) 2018-11-23

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111826177A (en) * 2020-07-10 2020-10-27 北京工业大学 Method for pyrolysis treatment of waste light-emitting diode packaging material and recovery of rare earth phosphor powder

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102110560A (en) * 2011-02-24 2011-06-29 宜兴市苏南固废处理有限公司 Innocent treatment method for mercury-containing waste tube
CN105568007A (en) * 2016-01-25 2016-05-11 江西理工大学 Method for recovering rare earth from waste rare earth phosphor

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102110560A (en) * 2011-02-24 2011-06-29 宜兴市苏南固废处理有限公司 Innocent treatment method for mercury-containing waste tube
CN105568007A (en) * 2016-01-25 2016-05-11 江西理工大学 Method for recovering rare earth from waste rare earth phosphor

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘虎: "《废旧稀土荧光粉的回收及其碱熔机理研究》", 30 September 2015 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111826177A (en) * 2020-07-10 2020-10-27 北京工业大学 Method for pyrolysis treatment of waste light-emitting diode packaging material and recovery of rare earth phosphor powder
CN111826177B (en) * 2020-07-10 2021-08-13 北京工业大学 Method for pyrolysis treatment of waste light-emitting diode packaging material and recovery of rare earth phosphor powder
WO2022007980A1 (en) * 2020-07-10 2022-01-13 北京工业大学 Combination waste light emitting diode packaging material pyrolysis treatment and method of recovery of rare earth elements from phosphor powder

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Application publication date: 20181123