CN102851506A - Method for extracting and recovering silver from waste solar cell - Google Patents
Method for extracting and recovering silver from waste solar cell Download PDFInfo
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- CN102851506A CN102851506A CN2012102841483A CN201210284148A CN102851506A CN 102851506 A CN102851506 A CN 102851506A CN 2012102841483 A CN2012102841483 A CN 2012102841483A CN 201210284148 A CN201210284148 A CN 201210284148A CN 102851506 A CN102851506 A CN 102851506A
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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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
- Y02W30/82—Recycling of waste of electrical or electronic equipment [WEEE]
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Abstract
The invention provides a method for extracting and recovering silver from a waste solar cell, and relates to a technology of solar material washing. The method comprises the following steps: a, washing the surface of a waste solar cell; b, soaking in hydrochloric acid to remove an aluminum back surface field; c, rinsing a silicon wafer subjected to aluminum back surface field removal with pure water, and then soaking in nitrohydrochloric acid to remove a silver electrode on the silicon wafer; d, adding HF into the nitrohydrochloric acid to remove a silicon nitride blue membrane on the surface, thus obtaining a clean silver extraction wafer; e, rinsing the silver extraction wafer with pure water, soaking in mixed acid, and cleaning to obtain clean fragments; and f, adding high-purity iron powder into the nitrohydrochloric acid solution, stirring, filtering silver powder after the reaction is finished, drying, proportioning, and smelting to obtain a high-quality silver ingot. The invention has the following beneficial effects: through the properties of different kinds of acid, the aluminum, silver and silicon nitride on the cell can be subjected to independent treatment, so that the cell can be fully utilized; meanwhile, the silver can be recovered, and about 0.6kg of silver can be recovered from 50kg of cell; and the silicon ingot production cost can be effectively reduced, thereby achieving the synergy purpose.
Description
Technical field
The present invention relates to solar energy single crystal, polysilicon chip technology manufacturing field, especially relate to sun power and wash the material technology.
Background technology
Solar energy industry is sunrise industry, environment protection is paid attention to the increasing of dynamics along with people, and solar energy industry develops rapidly especially.The silica-based cell piece of photovoltaic solar is one of green energy resource of popularizing at present, and the waste battery sheet produces in production process, has apparatus and process, human error etc. to cause, and the waste battery sheet can not reach throwing stove ingot casting standard must be to its cleanup acid treatment.In the market pickling is generally hydrofluoric acid and adds the Neutral ammonium fluoride immersion, and processing cost is high, and poor processing effect is thrown stove has certain influence to the silicon ingot quality.Adding hydrofluoric acid by salt acid soak, chloroazotic acid soaks and to wash pure water rinsing with nitration mixture again and totally can throw stove.
Each cell piece of waste battery sheet contains 0.2 to 0.3g silver, and in the market pickling is generally hydrofluoric acid and adds Neutral ammonium fluoride and soak wash clean and throw stove and use, but silver can't reclaim and causes very large waste.
Summary of the invention
The purpose of this invention is to provide a kind of useless solar battery sheet and move back the silver recovery method, it has overcome the defective of prior art, and processing cost is low and meet next procedure and throw the stove standard.The low silver recovery utilization ratio that improves of processing cost.
The present invention adopts salt acid soak, chloroazotic acid immersion, hydrofluoric acid dips to remove first the surfaces of aluminum back surface field, then remove the blue film of the last surface nitrogen SiClx of surperficial silver electrode, the waste battery sheet is rinsed well and can be thrown stove on the one hand, and Silver Nitrate cements out with high-purity iron powder on the other hand.
For achieving the above object, the present invention adopts following technical scheme:
Useless solar battery sheet moves back the silver recovery method, it is characterized in that comprising the steps: that a is with sun power waste battery sheet surface wash clean; Wherein, hydrochloric acid referred to that analytical pure content was 36%～38% to b usefulness salt acid soak with the removal of aluminium back surface field in 2～5 hours; Silicon chip after c aluminium back surface field is removed (containing the blue film of silver electrode and silicon nitride) is clean with pure water rinsing, puts into chloroazotic acid and soaks 2～5 hours, removes silver electrode above the silicon chip; D is in chloroazotic acid and HF(hydrofluoric acid) ratio of volume ratio 17～19:1, in chloroazotic acid, add HF(hydrofluoric acid), the silicon chip of removing silver electrode inserted soaked 2～5 hours, remove the blue film of surface nitrogen SiClx, obtain the clean silver strip that moves back; Described HF(hydrofluoric acid) refer to analytical pure content: 42%～50%; E move back silver strip clean with pure water rinsing after, soaked 4.5～5.5 hours with nitration mixture, clean and obtain clean fragment; Wherein, nitration mixture refers to: the mixing liquid of nitric acid and hydrofluoric acid, ratio are nitric acid: hydrofluoric acid=1.25～1.35:1; F throws in the ratio of 0.9～1.1kg high-purity iron powder in the cell piece of every 50kg, high-purity iron powder is put into the described chloroazotic acid hydrofluoric acid of d step mixing solutions stir, and described high-purity iron powder refers to purity 〉=99%, and granularity is 150～500 μ m; After finishing, reaction (represents that to react not bubbling reaction finishes) silver powder filtered that oven dry can obtain the silver ingot of quality higher (purity reaches 90%) after the melting of preparing burden.
The objective of the invention is and can further realize by following scheme:
Useless solar battery sheet moves back the silver recovery method, it is characterized in that comprising the steps: that a is with sun power waste battery sheet surface wash clean; Wherein, hydrochloric acid referred to that analytical pure content was 36%～38% to b usefulness salt acid soak with the removal of aluminium back surface field in 3～4 hours; Silicon chip after c aluminium back surface field is removed is clean with pure water rinsing, puts into chloroazotic acid and soaks 3～4 hours, removes silver electrode above the silicon chip; D adds HF in the ratio of chloroazotic acid and HF volume ratio 18:1 in chloroazotic acid, the silicon chip of removing silver electrode is inserted soaked 3～4 hours, removes the blue film of surface nitrogen SiClx, obtains the clean silver strip that moves back; Described HF refers to analytical pure HF content: 42%～50%; E move back silver strip clean with pure water rinsing after, soaked 4～6 hours with nitration mixture, clean and obtain clean fragment; Wherein, nitration mixture refers to: the mixing liquid of nitric acid and hydrofluoric acid, nitration mixture ratio are nitric acid: hydrofluoric acid=1.3:1; F throws in the ratio of 1kg high-purity iron powder in the cell piece of every 50kg, high-purity iron powder is put into the described chloroazotic acid hydrofluoric acid of d step mixing solutions stir, and described high-purity iron powder refers to purity 〉=99%, and granularity is 150～500 μ m; After reaction finishes, silver powder to be filtered, oven dry can obtain purity and be the silver ingot more than 90% after the batching melting.
Further:
Described chloroazotic acid refers to that its ratio of mixed solution of hydrochloric acid and nitric acid is hydrochloric acid: nitric acid=3:1, wherein, content of hydrochloric acid: analytical pure 36%～38%, nitric acid content: analytical pure 68%～70%.
Described pure water can be standard compliant any pure water, specifically refers to: pure water is the deionization pure water, and resistivity is that 10 megaohm mommes are to 18 megaohm mommes.
Described silicon nitride is high-purity monocrystalline silicon nitride.
The invention has the beneficial effects as follows: be by the character of different acid the aluminium above the cell piece, silver, silicon nitride to be carried out individual curing, can be fully reacted during processing, the processing cost poor efficiency is high, and cell piece is fully used.Add hydrofluoric acid immersion generation Silver Nitrate by salt acid soak, chloroazotic acid out silver-colored with iron replacement, show through repetition test: the 50kg cell piece can reclaim silver about 0.6kg.Adopt the technology of the present invention, can effectively reduce the silicon ingot production cost, reach the purpose of synergy.
Embodiment
In order to make those skilled in the art person understand better the present invention program, and above-mentioned purpose of the present invention, feature and advantage can be become apparent more, the present invention is further detailed explanation below in conjunction with embodiment.
Embodiment:
Useless solar battery sheet moves back the silver recovery method, successively progressive following steps:
The first step: with the sun power waste battery sheet surface wash clean (mainly being to remove dust, metal, greasy dirt) of 50kg;
Second step: the gaily decorated basket that cell piece will be housed is put into soaking compartment and is poured pure water and hydrochloric acid into, hydrochloric acid: water=1:15,2 liters of hydrochloric acid, 30 liters in water.
Hydrochloric acid is analytical pure content: 36%～38% soaked 2～5 hours.Remove the surfaces of aluminum back surface field.
Reaction formula is: 2Al+6HCl=2AlCl
3+ 3H
2↑
Its advantage is: hydrochloric acid and reactive aluminum form rapidly hydrogen, effectively remove the aluminium back surface field and carry out place mat for moving back silver.
The 3rd step: preparation chloroazotic acid (hydrochloric acid and nitric acid mixed solution) hydrochloric acid: nitric acid=3:1,27 liters of hydrochloric acid, 9 liters in nitric acid, putting into chloroazotic acid after the cell piece that has moved back aluminium rinsed well with pure water (resistivity 10 megaohm mommes are to 18 megaohm mommes) soaks, soaked 2～5 hours, each hour stirs once.Remove the silver electrode above the cell piece.Chloroazotic acid refers to that its ratio of mixed solution of hydrochloric acid and nitric acid is hydrochloric acid: nitric acid=3:1, content of hydrochloric acid: analytical pure 36%～38%.Nitric acid content: analytical pure 68%～70%.Reaction formula is: Ag+HNO
3+ HCl=AgCl+NO
2↑+H
2O.
Its advantage is: chloroazotic acid and the silver efficient that is swift in response is high, and later collection silver is carried out place mat.
The 4th step: add 2 liters of hydrofluoric acid dips after the reaction and removed surperficial blue rete in 2～5 hours in chloroazotic acid, hydrofluoric acid refers to analytical pure content: 42%～50%.Reaction formula is: SiN
4+ 4HF+9H
2O=3H
2SiO
3↓+4NH4F.
Its advantage is: hydrofluoric acid to the fast efficient of silicon nitride reaction high and cell piece is surperficial mix under the mixed solution of chloroazotic acid and hydrofluoric acid, can process clean.
The 5th step: will move back and finally wait until clean fragment after cell piece behind the silver soaks with nitration mixture.Wherein, nitration mixture refers to: the mixing liquid of nitric acid and hydrofluoric acid, nitration mixture ratio are wherein 13 liters in nitric acid of nitric acid: hydrofluoric acid=1.3:1,10 liters in hydrofluoric acid.
The 6th step: the 1kg high-purity iron powder is put into wang aqueous solution stir, after reaction finishes silver powder is filtered, oven dry can obtain the higher silver ingot of quality after the batching melting.Reaction formula is: Fe+2Ag
+=Fe
2 ++ 2Ag.
Described high-purity iron powder refers to purity 〉=99%, and granularity is 150～500 μ m.
Show by 18 repetition tests: adopt the technology of the present invention, every 50kg cell piece can reclaim the silver about 0.6kg.
The above; be the specific embodiment of the present invention only, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Claims (4)
1. useless solar battery sheet moves back the silver recovery method, it is characterized in that comprising the steps: that a is with sun power waste battery sheet surface wash clean; Wherein, hydrochloric acid referred to that analytical pure content was 36%～38% to b usefulness salt acid soak with the removal of aluminium back surface field in 2～5 hours; Silicon chip after c aluminium back surface field is removed is clean with pure water rinsing, puts into chloroazotic acid and soaks 2～5 hours, removes silver electrode above the silicon chip; D adds HF in the ratio of chloroazotic acid and HF volume ratio 17～19:1 in chloroazotic acid, the silicon chip of removing silver electrode is inserted soaked 2～5 hours, removes the blue film of surface nitrogen SiClx, obtains the clean silver strip that moves back; Described HF refers to analytical pure HF content: 42%～50%; E move back silver strip clean with pure water rinsing after, soaked 4～6 hours with nitration mixture, clean and obtain clean fragment; Wherein, nitration mixture refers to: the mixing liquid of nitric acid and hydrofluoric acid, nitration mixture ratio are nitric acid: hydrofluoric acid=1.25～1.35:1; F throws in the ratio of 0.9～1.1kg high-purity iron powder in the cell piece of every 50kg, high-purity iron powder is put into the described chloroazotic acid hydrofluoric acid of d step mixing solutions stir, and described high-purity iron powder refers to purity 〉=99%, and granularity is 150～500 μ m; After reaction finishes, silver powder to be filtered, oven dry can obtain purity and be the silver ingot more than 90% after the batching melting.
2. useless solar battery sheet according to claim 1 moves back the silver recovery method, it is characterized in that comprising the steps: that a is with sun power waste battery sheet surface wash clean; Wherein, hydrochloric acid referred to that analytical pure content was 36%～38% to b usefulness salt acid soak with the removal of aluminium back surface field in 3～4 hours; Silicon chip after c aluminium back surface field is removed is clean with pure water rinsing, puts into chloroazotic acid and soaks 3～4 hours, removes silver electrode above the silicon chip; D adds HF in the ratio of chloroazotic acid and HF volume ratio 18:1 in chloroazotic acid, the silicon chip of removing silver electrode is inserted soaked 3～4 hours, removes the blue film of surface nitrogen SiClx, obtains the clean silver strip that moves back; Described HF refers to analytical pure HF content: 42%～50%; E move back silver strip clean with pure water rinsing after, soaked 4.5～5.5 hours with nitration mixture, clean and obtain clean fragment; Wherein, nitration mixture refers to: the mixing liquid of nitric acid and hydrofluoric acid, nitration mixture ratio are nitric acid: hydrofluoric acid=1.3:1; F throws in the ratio of 1kg high-purity iron powder in the cell piece of every 50kg, high-purity iron powder is put into the described chloroazotic acid hydrofluoric acid of d step mixing solutions stir, and described high-purity iron powder refers to purity 〉=99%, and granularity is 150～500 μ m; After reaction finishes, silver powder to be filtered, oven dry can obtain purity and be the silver ingot more than 90% after the batching melting.
3. useless solar battery sheet according to claim 1 and 2 moves back the silver recovery method, it is characterized in that: described chloroazotic acid refers to that its ratio of mixed solution of hydrochloric acid and nitric acid is hydrochloric acid: nitric acid=3:1, wherein, content of hydrochloric acid: analytical pure 36%～38%, nitric acid content: analytical pure 68%～70%.
4. useless solar battery sheet according to claim 1 and 2 moves back the silver recovery method, it is characterized in that: described pure water refers to: pure water is the deionization pure water, and resistivity is that 10 megaohm mommes are to 18 megaohm mommes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102841483A CN102851506A (en) | 2012-08-12 | 2012-08-12 | Method for extracting and recovering silver from waste solar cell |
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|---|---|---|---|
| CN2012102841483A CN102851506A (en) | 2012-08-12 | 2012-08-12 | Method for extracting and recovering silver from waste solar cell |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103779441A (en) * | 2013-11-13 | 2014-05-07 | 河南科技学院 | Cleaning recovery treatment process of solar cell sheet |
| CN103920698A (en) * | 2014-05-08 | 2014-07-16 | 刘景洋 | Method for recycling resources in waste crystal solar silicon cell piece in classified mode |
| CN105347379A (en) * | 2015-12-14 | 2016-02-24 | 常州天合光能有限公司 | Method for recycling aluminum and silver from waste crystalline silicon solar cell |
| FR3028433A1 (en) * | 2014-11-18 | 2016-05-20 | Commissariat Energie Atomique | PROCESS FOR RECOVERING METALS CONTAINED IN A SILICON SUBSTRATE |
| EP3178576A1 (en) | 2015-12-11 | 2017-06-14 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Method for recycling the silver contained in a photovoltaic cell |
| CN107393813A (en) * | 2017-09-08 | 2017-11-24 | 如皋市下原科技创业服务有限公司 | A kind of acid cleaning process of diode chip for backlight unit |
| CN109576495A (en) * | 2018-12-03 | 2019-04-05 | 乐山新天源太阳能科技有限公司 | A kind of solar battery sheet recovery and treatment method |
| CN113846232A (en) * | 2021-10-22 | 2021-12-28 | 紫金矿业集团黄金珠宝有限公司 | Method for extracting noble metal from waste blue membrane for semiconductor to prepare high-purity gold and platinum |
| CN115138657A (en) * | 2022-05-24 | 2022-10-04 | 大连理工大学 | Method for preparing photocatalytic material by utilizing waste crystalline silicon solar cells |
| WO2023199270A1 (en) * | 2022-04-14 | 2023-10-19 | Coby Tao | Circular electrochemical metal recovery |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103779441A (en) * | 2013-11-13 | 2014-05-07 | 河南科技学院 | Cleaning recovery treatment process of solar cell sheet |
| CN103920698A (en) * | 2014-05-08 | 2014-07-16 | 刘景洋 | Method for recycling resources in waste crystal solar silicon cell piece in classified mode |
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| EP3178576A1 (en) | 2015-12-11 | 2017-06-14 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Method for recycling the silver contained in a photovoltaic cell |
| CN105347379A (en) * | 2015-12-14 | 2016-02-24 | 常州天合光能有限公司 | Method for recycling aluminum and silver from waste crystalline silicon solar cell |
| CN107393813A (en) * | 2017-09-08 | 2017-11-24 | 如皋市下原科技创业服务有限公司 | A kind of acid cleaning process of diode chip for backlight unit |
| CN109576495A (en) * | 2018-12-03 | 2019-04-05 | 乐山新天源太阳能科技有限公司 | A kind of solar battery sheet recovery and treatment method |
| CN113846232A (en) * | 2021-10-22 | 2021-12-28 | 紫金矿业集团黄金珠宝有限公司 | Method for extracting noble metal from waste blue membrane for semiconductor to prepare high-purity gold and platinum |
| CN113846232B (en) * | 2021-10-22 | 2022-09-02 | 紫金矿业集团黄金珠宝有限公司 | Method for extracting precious metal from waste blue membrane for semiconductor to prepare high-purity gold and platinum |
| WO2023199270A1 (en) * | 2022-04-14 | 2023-10-19 | Coby Tao | Circular electrochemical metal recovery |
| CN115138657A (en) * | 2022-05-24 | 2022-10-04 | 大连理工大学 | Method for preparing photocatalytic material by utilizing waste crystalline silicon solar cells |
| CN115138657B (en) * | 2022-05-24 | 2023-08-25 | 大连理工大学 | Method for preparing photocatalytic material by using waste crystalline silicon solar cell |
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Application publication date: 20130102 |