CN108728654A - A kind of photovoltaic chip recovery method - Google Patents
A kind of photovoltaic chip recovery method Download PDFInfo
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- CN108728654A CN108728654A CN201810609552.0A CN201810609552A CN108728654A CN 108728654 A CN108728654 A CN 108728654A CN 201810609552 A CN201810609552 A CN 201810609552A CN 108728654 A CN108728654 A CN 108728654A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0086—Treating solutions by physical methods
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
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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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Abstract
The invention discloses a kind of photovoltaic chip recovery methods, fast and efficiently to recycle the metal in photovoltaic chip metal coating.The photovoltaic chip recovery method includes：Photovoltaic chip is placed in leachate and impregnates preset duration, the photovoltaic chip includes the coat of metal of substrate and the substrate surface, the leachate includes the first acid solution and the second acid solution than mixing by preset quality, the leachate makes the metal in the coat of metal form dissolving metal salts, and the substrate is made to be passivated；Photovoltaic chip is taken out, metal salt is obtained in the leachate after using；From obtaining the metal in the coat of metal in the metal salt.
Description
Technical field
The present invention relates to photovoltaic chip technology field, more particularly to a kind of photovoltaic chip recovery method.
Background technology
Copper-indium-galliun-selenium film solar cell is referred to as the since theoretical efficiency is high, material consumption is few, prepares that low energy consumption etc.
Two generation solar battery technologies.Because indium and gallium belong to dissipated metal, reserves and yield is all limited and value is higher, need by
Bad in production process and the valuable metal in the copper-indium-gallium-selenium photovoltaic chip scrapped are recycled, and are further followed with facilitating
Ring utilizes, to ensure the sustainable development of copper-indium-galliun-selenium film solar cell material.Copper-indium-gallium-selenium photovoltaic chip generally uses
Iron material matter substrate (include but not limited to stainless steel substrate) steams method by copper indium gallium selenide and other coats of metal by sputtering method or altogether
It is plated on iron material matter substrate, each coating and iron material matter substrate are tightly combined.
Dissolution method dissolves into iron material matter substrate and copper indium gallium selenide coating in oxidisability acid solution simultaneously, the content of iron in solution
Much larger than the content of copper indium gallium selenide, the metals such as copper indium gallium selenide can not be effectively recycled.Alkali solution technique by alkali soluble solution copper indium gallium selenide layer with
The connection molybdenum layer of substrate, dissolving molybdenum layer speed is slower, can not be used in routinely producing substantially.The method that freezing uses deep cooling
By the separation of substrate and copper indium gallium selenide coating, freezing processing procedure requires temperature relatively low, and process conditions require height, are shelled after deep cooling
It is difficult from more.
Invention content
The present invention provides a kind of photovoltaic chip recovery method, fast and efficiently to recycle in photovoltaic chip metal coating
Metal.
The present invention provides a kind of photovoltaic chip recovery method, including：
Photovoltaic chip is placed in leachate and impregnates preset duration, the photovoltaic chip includes substrate and the substrate surface
The coat of metal, the leachate includes that the first acid solution and the second acid solution than mixing, the leachate make institute by preset quality
The metal stated in the coat of metal forms dissolving metal salts, and the substrate is made to be passivated；
Photovoltaic chip is taken out, metal salt is obtained in the leachate after using；
From obtaining the metal in the coat of metal in the metal salt.
Optionally, when the coat of metal includes copper indium gallium selenide coating, and the substrate includes iron material matter substrate, described
One acid solution includes concentrated nitric acid, and second acid solution includes the concentrated sulfuric acid.
Optionally, the preset quality ratio of first acid solution and the second acid solution includes：5%：95% to 10%：90%.
Optionally, the method further includes：Photovoltaic chip is placed in when being impregnated in leachate, when the coat of metal stops
When dissolving, increase by first acid solution so that the coat of metal continues to dissolve.
Optionally, metal salt is obtained in the leachate after using, including：
Using obtaining metal salt in leachate of the embrane method acid recovery technology after using；Alternatively,
Sulfating roasting is carried out to the leachate after using and obtains metal salt.
Optionally, the method further includes：
Photovoltaic chip is placed in when being impregnated in leachate, the gas of generation is subjected to tail gas absorption.
Optionally, the method further includes：
The photovoltaic chip of taking-up is cleaned, remaining dissolving metal salts on the substrate of photovoltaic chip are made；
From obtaining the metal in the coat of metal in the solution after cleaning.
Optionally, the preset duration includes：1 to 10 minute.
Optionally, described from obtaining the metal in the coat of metal in the metal salt, including：
Combination using one or more of mode is from obtaining the metal in the coat of metal in the metal salt：In
With the precipitation method, displacement method, extraction, reduction method, ion-exchange and electrolysis.
The technical solution that the embodiment of the present invention provides can include the following benefits：By using two in the present embodiment
Nitration mixture is made in the different acid solution of kind, can dissolve the coat of metal using the nitration mixture and make the characteristic of substrate passivation so that metal-plated
Layer can be quickly dissolved in leachate, and substrate will not dissolve, and metal salt is then obtained from leachate, finally from metal salt
In obtain metal, realize the coat of metal and substrate it is quick, efficiently separate, efficient recycling has been carried out to photovoltaic chip.
Other features and advantages of the present invention will be illustrated in the following description, also, partly becomes from specification
It obtains it is clear that understand through the implementation of the invention.The purpose of the present invention and other advantages can be by the explanations write
Specifically noted structure is realized and is obtained in book, claims and attached drawing.
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
Description of the drawings
Attached drawing is used to provide further understanding of the present invention, and a part for constitution instruction, the reality with the present invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the flow chart of photovoltaic chip recovery method in the embodiment of the present invention.
Fig. 2 is the flow chart of photovoltaic chip recovery method in the embodiment of the present invention.
Specific implementation mode
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
In the related technology, when recycling photovoltaic chip, dissolution method is since the content of iron in solution is much larger than copper indium gallium selenide
Content can not effectively recycle the metals such as copper indium gallium selenide；Alkali solution technique dissolving molybdenum coating speeds are slower, substantially can not be in routinely producing
It uses；Freezing processing procedure requires temperature relatively low, and process conditions require height, and coat of metal stripping is difficult after deep cooling.
To solve the above problems, the present embodiment impregnates photovoltaic chip using nitration mixture as leachate, base in soaking process
Plate is passivated, and coated metal then forms metal salt and enters solution, therefore realizes that fast and effectively photovoltaic chip recycles.
Referring to Fig. 1, photovoltaic chip recovery method includes in the present embodiment：
Step 101：Photovoltaic chip is placed in leachate and impregnates preset duration, photovoltaic chip includes substrate and substrate surface
The coat of metal, leachate includes that the first acid solution and the second acid solution than mixing, the leachate make the coat of metal by preset quality
In metal form dissolving metal salts, and substrate is made to be passivated.
Step 102：Photovoltaic chip is taken out, metal salt is obtained in the leachate after using.
Step 103：From the metal obtained in metal salt in the coat of metal.
Leachate is made using two kinds of different acid solutions in the present embodiment, using the leachate can dissolve the coat of metal,
And the characteristic for making substrate be passivated so that the coat of metal can be quickly dissolved in leachate, and substrate will not dissolve, so as to
Obtain metal salt from leachate, metal finally obtained from dissolving metal salts, realize substrate and the coat of metal it is quick, have
Effect separation, efficient recycling has been carried out to photovoltaic chip.
In an embodiment of the present invention, when the coat of metal includes copper indium gallium selenide coating, the first acid solution includes concentrated nitric acid；When
When substrate includes iron material matter substrate, the second acid solution includes the concentrated sulfuric acid.Wherein, concentrated nitric acid for example may include mass fraction be more than or
Nitric acid equal to 68%.The concentrated sulfuric acid for example may include the sulfuric acid that mass fraction is greater than or equal to 95%.
In the present embodiment, for the copper indium gallium selenide coating in photovoltaic chip, it can use and copper indium gallium selenide fast reaction shape
At metal salt, to make the rapidly-soluble concentrated nitric acid of copper indium gallium selenide that can be used for iron material matter substrate as the first acid solution
Make the concentrated sulfuric acid that iron is passivated as the second acid solution under room temperature.
Wherein, the reaction equation of chemical reaction generation metal salt occurs for the copper in the coat of metal, indium, gallium, selenium and leachate such as
Under：
Se+4HNO3=H2SeO2+4NO2↑+H2O
Cu+H2SO4+2HN23=CuSO4+2NO2↑+2H2O
2In+3H2SO4+6HNO2=In2(SO4)3+6NO2↑+6H2O
2Ga+3H2SO4+6HNO2=Ga2(SO4)3+6NO2↑+6H2O
Since the metal in the coat of metal is slower with strong sulfuric acid response at normal temperatures, so, copper indium gallium selenide mainly with leaching
Concentrated nitric acid in liquid is reacted.Concentrated nitric acid in leachate keeps metal rapidly-soluble simultaneously, the concentrated sulfuric acid master in leachate
It is used for passivated iron.The concentrated sulfuric acid is reacted with iron at normal temperatures, in the oxidation film of the Surface Creation densification of iron, to make iron be passivated.
In an embodiment of the present invention, the preset quality of the first acid solution and the second acid solution ratio includes：5%：95% to 10%：
90%.
It is considered in the present embodiment and preferably impregnates effect.In nitration mixture, the ratio of the first acid solution should not be too large, the first acid
The proportional region of liquid is advisable in the copper indium gallium selenide being completely dissolved just in the coat of metal, so that there is no concentration to be lower
The first acid solution go influence iron material matter substrate in iron passivation.
In an embodiment of the present invention, when photovoltaic chip is placed in and is impregnated in leachate by above-mentioned steps 101, photovoltaic chip
Recovery method can also include the following steps：When the coat of metal stops dissolving, increase by the first acid solution so that the coat of metal continues
Dissolving.
In the present embodiment, it can be made by increasing by the first acid solution when leachate is insufficient to allow the coat of metal all to dissolve
It obtains the coat of metal to continue to dissolve, to ensure to impregnate effect.
In an embodiment of the present invention, when photovoltaic chip is placed in and is impregnated in leachate by above-mentioned steps 101, photovoltaic chip
Absorption method can also include the following steps：The gas of generation is subjected to tail gas absorption.
In the present embodiment, can generated gas when being chemically reacted in soaking process be subjected to tail gas absorption, with
Exempt to pollute environment.
In an embodiment of the present invention, as shown in Fig. 2, after above-mentioned steps 102 take out photovoltaic chip, photovoltaic chip returns
Receiving method can also include the following steps：
Step 104：The photovoltaic chip of taking-up is cleaned, remaining dissolving metal salts on the substrate of photovoltaic chip are made.
Step 105：The metal in the coat of metal is obtained from the solution after cleaning.
It should be noted that step 104-105 can be performed simultaneously with step 102-103.
In the present embodiment, it can be recycled to remaining in the metal on substrate after immersion, to further increase metal
The rate of recovery.
In an embodiment of the present invention, from the metal obtained in metal salt in the coat of metal, including：
Using obtaining metal salt in leachate of the embrane method acid recovery technology after using；Alternatively,
Sulfating roasting is carried out to the leachate after using, obtains metal salt.
In the present embodiment, different technological means can be used, metal salt is obtained in the leachate after using.
In an embodiment of the present invention, from the metal obtained in metal salt in the coat of metal, including：Using following a kind of or
The combination of various ways is from the metal obtained in metal salt in the coat of metal：Neutralization precipitation method, displacement method, extraction, reduction method,
Ion-exchange and electrolysis.
Wherein, neutralization precipitation method carries out neutralization precipitation by the way that lime, NaOH and KOH and metal ion is added, and is then dehydrated
After roasted to obtain metal oxide.Displacement method is referred to utilizing the active sex differernce of metal, be incited somebody to action using the strong metal of activity
Metal target cements out the method to form metal simple-substance from solution.Extraction handles mutual not phase therewith using fluid extractant
The bi-component or Multi component of appearance realize the mass transfer separation process of component separation.Reduction method refers to using metal A (or its alloy)
Make method of the reducing agent at high temperature by the reduction of the compound of another metal B to produce metal B (or its alloy).Ion exchange
Method is to utilize ion exchange resin or fiber-reactive gene attachment exchange ion, and acid group example or metal are exchanged from waste acid liquor
Example realizes the method that detaches between different acid and metal salts.Electrolysis obtains metal by being electrolysed to metal salt solution
Simple substance.
Realization process is discussed in detail below by specific embodiment.
Embodiment 1
Photovoltaic chip recovery method includes in the present embodiment：
Step A：It is 5% to prepare mass ratio：The leachate that 95% concentrated nitric acid is mixed with the concentrated sulfuric acid.Measure 20 liters of leachates
It is injected into 50 liters of leaching tanks, copper indium gallium selenide flexible photovoltaic chip is integrally put in leaching tanks, is taken out after ten minutes, can be shown
Copper indium gallium selenide assembly surface black is decorporated, and the iron material matter substrate of grey is remained, and the coat of metal is efficiently separated with substrate.Gold
Belong to the NO generated when coating dissolving2Equal toxic gases, which are passed through in 40% sodium hydroxide solution, carries out absorption processing.
Step B：Photovoltaic chip after immersion is taken out, is cleaned using 1L water, makes to remain on the substrate of photovoltaic chip
Dissolving metal salts.
Step C：The leachate after using is handled using embrane method acid recovery technology, obtain metal-free acid solution and
Metal salt solution, and the wash water in above-mentioned steps is mixed with metal salt solution, and by conventional smelting process from the gold
Belong to and detaches copper indium gallium selenide metal in salting liquid.
By the copper indium gallium selenide content in the copper indium gallium selenide metal and metal salt solution in detection chip, the invention pair can be obtained
Metal recovery rate is up to 99.99% or more in copper-indium-gallium-selenium photovoltaic chip.
Embodiment 2：
Photovoltaic chip recovery method includes in the present embodiment：
Step A：It is 10% to prepare mass ratio：The leachate that 90% concentrated nitric acid is mixed with the concentrated sulfuric acid.Measure 15 liters of leachings
Liquid is injected into 30 liters of leaching tanks, and copper indium gallium selenide flexible photovoltaic chip is integrally put in leaching tanks, is taken out after 8 minutes, can be shown
Show that copper indium gallium selenide assembly surface black is decorporated, remains the iron material matter substrate of grey.The coat of metal is efficiently separated with substrate.
The NO that the coat of metal generates when dissolving2Equal toxic gases, which are passed through in 40% sodium hydroxide solution, carries out absorption processing.
Step B：Photovoltaic chip after immersion is taken out, is cleaned using 1L water, makes to remain on the substrate of photovoltaic chip
Dissolving metal salts.
Step C：The leachate after using is handled using embrane method acid recovery technology, obtain metal-free acid solution and
Metal salt solution, and the wash water in above-mentioned steps is mixed with metal salt solution, and by conventional smelting process from the gold
Belong to and detaches copper indium gallium selenide metal in salting liquid.
By the copper indium gallium selenide content in the copper indium gallium selenide metal and metal salt solution in detection chip, the invention pair can be obtained
Metal recovery rate is up to 99.99% or more in copper-indium-gallium-selenium photovoltaic chip.
Embodiment 3：
Photovoltaic chip recovery method includes in the present embodiment：
Step A：It is 8% to prepare mass ratio：The leachate that 92% concentrated nitric acid is mixed with the concentrated sulfuric acid.Measure 5 liters of leachates
It is injected into 10 liters of leaching tanks, copper indium gallium selenide flexible photovoltaic chip is integrally put in leaching tanks, is taken out after 1 minute, can be shown
Copper indium gallium selenide assembly surface black is decorporated, and the iron material matter substrate of grey is remained, and the coat of metal is efficiently separated with substrate.Gold
Belong to the NO generated when coating dissolving2Equal toxic gases, which are passed through in 40% sodium hydroxide solution, carries out absorption processing.
Step B：Photovoltaic chip after immersion is taken out, is cleaned using 1L water, makes to remain on the substrate of photovoltaic chip
Dissolving metal salts, and using the wash water as the dissolving raw material of subsequent sulphuric acid roasting material.
Step C：To the leachate cooperation copper indium gallium selenide chamber material after using, (copper indium gallium selenide chamber material is identical as useless chip
Producing line on defective products, recovery process need to abolish selenizing structure using sulfating roasting) carry out sulfating roasting, obtain copper and indium
The metal sulfate of gallium and restore to obtain impure selenium from flue gas, metal sulfate is detached after water dissolution using conventional smelting process
To copper indium gallium selenide metal.
Using the leachate after using as the raw material of sulfating roasting in the present embodiment, in conjunction with needing to carry out sulfating roasting
Copper indium gallium selenide chamber material, the sulfuric acid in leachate can be made full use of and consume, to obtain metal salt.
In the present invention, leachate uses room temperature nitration mixture, and process conditions require low compared with freezing；Immersion treatment needs
1-10 minutes are wanted, processing speed is fast compared with alkali solution technique.And metal values, which are directly transferred in solution to have to utilize, subsequently to be made
It is recycled with conventional method.Integrated artistic is simple, and speed is fast, is suitble to large-scale production.
Those skilled in the art after considering the specification and implementing the invention disclosed here, will readily occur to its of the present invention
Its embodiment.This application is intended to cover the present invention any variations, uses, or adaptations, these modifications, purposes or
Person's adaptive change follows the general principle of the present invention and includes undocumented common knowledge in the art of the invention
Or conventional techniques.The description and examples are only to be considered as illustrative, and true scope and spirit of the invention are by following
Claim is pointed out.
It should be understood that the invention is not limited in the precision architectures for being described above and being shown in the accompanying drawings, and
And various modifications and changes may be made without departing from the scope thereof.The scope of the present invention is limited only by the attached claims.
Claims (10)
1. a kind of photovoltaic chip recovery method, which is characterized in that the method includes：
Photovoltaic chip is placed in leachate and impregnates preset duration, the photovoltaic chip includes the gold of substrate and the substrate surface
Belong to coating, the leachate includes that the first acid solution and the second acid solution than mixing, the leachate make the gold by preset quality
The metal belonged in coating forms dissolving metal salts, and the substrate is made to be passivated；
Photovoltaic chip is taken out, metal salt is obtained in the leachate after using；
From obtaining the metal in the coat of metal in the metal salt.
2. photovoltaic chip recovery method as described in claim 1, which is characterized in that
When the coat of metal includes copper indium gallium selenide coating, and the substrate includes iron material matter substrate, first acid solution includes
Concentrated nitric acid, second acid solution includes the concentrated sulfuric acid.
3. photovoltaic chip recovery method as claimed in claim 2, which is characterized in that
The preset quality ratio of first acid solution and the second acid solution includes：5%：95% to 10%：90%.
4. photovoltaic chip recovery method as claimed in claim 2, which is characterized in that
The method further includes：Photovoltaic chip is placed in when being impregnated in leachate, when the coat of metal stops dissolving, is increased
First acid solution is so that the coat of metal continues to dissolve.
5. the photovoltaic chip recovery method as described in any one of claim 1-4, which is characterized in that the leaching after using
Go out and obtains metal salt in liquid, including：
Using obtaining metal salt in leachate of the embrane method acid recovery technology after using；Alternatively,
Sulfating roasting is carried out to the leachate after using, obtains metal salt.
6. the photovoltaic chip recovery method as described in any one of claim 1-4, which is characterized in that
The method further includes：
Photovoltaic chip is placed in when being impregnated in leachate, the gas of generation is subjected to tail gas absorption.
7. the photovoltaic chip recovery method as described in any one of claim 1-4, which is characterized in that
The method further includes：
The photovoltaic chip of taking-up is cleaned, remaining dissolving metal salts on the substrate of photovoltaic chip are made；
From obtaining the metal in the coat of metal in the solution after cleaning.
8. the photovoltaic chip recovery method as described in any one of claim 1-4, which is characterized in that
The preset duration includes：1 to 10 minute.
9. the photovoltaic chip recovery method as described in any one of claim 1-4, which is characterized in that
The method further includes：
Acid solution is obtained in leachate after using.
10. the photovoltaic chip recovery method as described in any one of claim 1-4, which is characterized in that
It is described from obtaining the metal in the coat of metal in the metal salt, including：
Combination using one or more of mode is from obtaining the metal in the coat of metal in the metal salt：It is heavy to neutralize
Shallow lake method, displacement method, extraction, reduction method, ion-exchange and electrolysis.
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| CN106029573A (en) * | 2014-02-26 | 2016-10-12 | 格林里昂集团有限公司 | Recovery of gold and/or silver from scrap |
| CN105087935A (en) * | 2014-05-22 | 2015-11-25 | 汉能新材料科技有限公司 | Method for recycling copper, indium and gallium from waste copper-indium-gallium target |
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