WO2015025304A2 - Procédé permettant la récupération d'un matériau à base d'étain à partir de déchets électroniques et matériau électrolytique à base d'étain obtenu à l'aide du procédé - Google Patents

Procédé permettant la récupération d'un matériau à base d'étain à partir de déchets électroniques et matériau électrolytique à base d'étain obtenu à l'aide du procédé Download PDF

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Publication number
WO2015025304A2
WO2015025304A2 PCT/IB2014/066555 IB2014066555W WO2015025304A2 WO 2015025304 A2 WO2015025304 A2 WO 2015025304A2 IB 2014066555 W IB2014066555 W IB 2014066555W WO 2015025304 A2 WO2015025304 A2 WO 2015025304A2
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WO
WIPO (PCT)
Prior art keywords
tin
solution
digestion
electrolysis
process according
Prior art date
Application number
PCT/IB2014/066555
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English (en)
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WO2015025304A3 (fr
Inventor
Marcin Arkadiusz ZGUTKA
Aleksander Jakub SZALECKI
Piotr Lukasz MIKOLAJCZYK
Artur MOLIK
Ryszard SWIETLIK
Jan SIWIEC
Marzena TROJANOWSKA
Original Assignee
Ecoback Sp. Z O.O.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ecoback Sp. Z O.O. filed Critical Ecoback Sp. Z O.O.
Publication of WO2015025304A2 publication Critical patent/WO2015025304A2/fr
Publication of WO2015025304A3 publication Critical patent/WO2015025304A3/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/14—Electrolytic production, recovery or refining of metals by electrolysis of solutions of tin
    • 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
    • C22B25/00—Obtaining tin
    • C22B25/06—Obtaining tin from scrap, especially tin scrap
    • 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

Definitions

  • the present invention concerns a field of the recycling of electronic waste and recovery of valuable raw materials, in particular metals, to be reused from such waste. More particularly, the present invention concerns a process for the recovery of a tin material from electronic scrap and an electrolytic tin material obtained by the process.
  • solder not containing lead must be used in applications related to electronic equipment, except for that used in military, medical and aviation applications. Therefore, any new equipment other than that used in the fields specified above may not contain lead-containing solder. Nevertheless, a considerable quantity of devices containing lead solder were already manufactured and sold before 2002. Therefore, there is a problem of the recycling and treatment of electronic waste containing tin and lead solder.
  • the already known metal recycling and recovery methods are based on incineration.
  • electronic waste is fed into furnaces in which it is incinerated.
  • the resulting metallic material being a mixture of different metals, needs to be separated. Separation is carried out using metallurgical processes. Therefore, such methods are very expensive, because they are highly energy-consuming. Furthermore, they are very harmful to the environment due to emissions of noxious gases.
  • Present invention provides a process for the recovery of a tin material from electronic scrap, characterised in that the electronic scrap containing the tin material is provided, the tin material in the electronic scrap is digested using a digestion solution whereby an electrolysis solution and treated electronic scrap, substantially free from the tin material, are obtained, wherein the electronic scrap after digestion is used for further treatment, the electrolysis solution is subjected to electrolysis whereby a tin material and a spent electrolysis solution are obtained, and the tin material obtained electrolytically and the spent electrolysis solution are transferred for further processing.
  • the electronic scrap is preferably copper metal granulate.
  • the electronic scrap is preferably washed at least once using the spent electrolysis solution or at least once using a fresh digestion solution, wherein the solutions after washing the electronic scrap are combined with the electrolysis solution.
  • the spent solution is preferably regenerated whereby a regenerated digestion solution is obtained, to be used as the digestion solution in the step of tin material digestion.
  • the spent electrolysis solution is preferably recycled to electronic scrap digestion, and the solution is optionally regenerated.
  • the composition of the electrolysis solution is adjusted.
  • at least one operation is preferably carried out, the operation being selected from a group including, respectively, the addition of lead, addition of lead alloys, addition of lead compounds, precipitation of lead excess, precipitation of tin excess, tin oxidation to Sn ⁇ +4 >, or combinations thereof.
  • the digestion solution or the electrolysis solution or the spent electrolysis solution is preferably subjected to at least one operation, the operation being selected from a group including filtration, ultrafiltration, osmosis, electrodialysis, treatment with magnetic field, precipitation of low soluble compounds, freezing out, crystallisation, concentration, evaporation, extraction, ion exchange, chelation, selective oxidation and/or reduction, or combinations thereof.
  • Tin dioxide or lead sulphate are preferably added.
  • the tin material is preferably substantially pure tin or a tin and lead alloy.
  • the electrolytic tin material is preferably substantially pure electrolytic tin or electrolytic tin and lead alloys.
  • the digestion solution preferably contains 10 to 60% of an alkanesulphonic acid, 0.01 to 5% nitrate ions and water.
  • the digestion solution preferably also contains 0.001 to 1 5% of at least organic brightener, selected from a group including 0 to 10% of at least one aromatic amine selected from a group including benzotriazole, imidazole, and derivatives thereof, quinones, such as hydroquinone, pyrocatechol and derivatives thereof, and water soluble ethers, such as 1 -propoxyethanol, 2-propoxyethanol and derivatives thereof.
  • at least organic brightener selected from a group including 0 to 10% of at least one aromatic amine selected from a group including benzotriazole, imidazole, and derivatives thereof, quinones, such as hydroquinone, pyrocatechol and derivatives thereof, and water soluble ethers, such as 1 -propoxyethanol, 2-propoxyethanol and derivatives thereof.
  • the alkanesulphonic acid is preferably selected from a group including methanesulphonic acid, ethanesulphonic acid and mixtures thereof.
  • the electrolytic tin material of the invention is obtained using the process of the invention.
  • the electrolytic tin material of the invention is preferably substantially pure electrolytic tin or an electrolytic tin and lead alloy.
  • solder containing tin or tin and lead is removed from electronic scrap.
  • Industrially important materials are obtained, such as pure tin, tin and lead alloys, tin compounds, such as tin dioxide, tin carbonate, lead compounds, such as lead sulphate.
  • practically pure copper is recovered to be industrially reused.
  • the proposed process of the invention is inexpensive, because no furnace processes are used. Furthermore, the process of the invention is less harmful to the environment, because there are no noxious emissions, such as those from furnace processes, or harmful liquid waste, such as acidic leaching waste, electrolysis waste, etc.
  • the copper metal granulate was found to be effective to be used in the process for the recovery of the tin material from electronic scrap.
  • Digestion solution for the tin material in the copper metal material Digestion solution for the tin material in the copper metal material. Considering the complex composition and grain size of the fractions, digestion experiments were carried out using electronic scrap as provided. The first experiments were performed using FF Concentrate. Bath concentration was calculated based on the Material Safety Data Sheet and the Processing Manual for Stripper L80. The experiments were unsuccessful. Concentrated methanesulphonic acid (MSA) in the form of FF Concentrate and its aqueous solutions digested tin to a minor extent and very slowly.
  • MSA Concentrated methanesulphonic acid
  • the optimum concentration of the nitrate anion added should be no more than 2 to 3%. When concentration is higher than that, no further effect on the tin digestion process is seen. 3% of the anion added was used in further experiments.
  • the maximum digestion solution capacity is 1 03.7 g per dm 3 of the digestion bath.
  • the concentration of FF Concentrate in the bath should be between 30 and 50%.
  • FF Concentrate diluted in a 1 :1 ratio was used, which corresponds to 40 weight % concentration of MSA (5 mol/dm 3 ).
  • Tin digestion process A catalyst was selected which considerably accelerates the process of tin digestion in electronic scrap.
  • a bath with the following composition is used in the experiments: 50% FF Concentrate, 47% water and 3% nitrate anion.
  • Scrap digestion time is 30 min.
  • Experiments are under way to obtain selective tin digestion. This would make easier the electrolysis process, affected by metals digested with tin.
  • experiments with digesting pure metals were carried out with aluminium, lead, zinc, copper and iron. Aluminium was not digested, zinc, copper and iron were slightly digested, and lead was digested as required.
  • the composition of the digested solution was also determined. Unfortunately, the composition of each resulting fraction varied; therefore, the digestion process required permanent analytical surveillance.
  • Example composition of a solution following the digestion of fraction A1 determined using FAAS is shown in Table 6.
  • Electrodes Selection of electrodes. Graphite and platinum-iridium anodes with high chemical resistance were initially used. Platinum gauze anodes were more promising, while graphite electrodes generated slime thus fouling the bath, even though filtration fabric bags were used. Copper and tin foil cathodes were used. The suggested electrode set is a copper or tin foil cathode, and the anode should be made of platinum or a platinum-iridium alloy.
  • Tin bath modification additives Baths prepared based on tin electrolyte without brightening additives were used in the initial experiments with tin separation. Even though no impurities were present, tin deposition from such simplest baths did not yield satisfactory results: coatings were black, spongy and with poor adhesion. Therefore, commercial brighteners used in electroplating and masking products which reduce co- deposition of other metals were used in further experiments. JIW INWEX products were used, intended for sulphate baths for tin plating : Inwexlux 9 (25 - 30 g/dm 3 ), Inwexlux 1 0 (2 - 5 g/dm 3 ), Niwelator ACA (1 - 2 g/dm 3 ). The additives were used in quantities as suggested by the manufacturer. Electrolysis with bath additives used gave promising results. The deposited tin coat was fine crystalline, bright and compact.
  • Electrolytic tin separation A unit with power supply, a magnetic stirrer and electrolyser for testing baths with a volume of 500 cm 3 was prepared for the experiments.
  • glossy coats were obtained for high current densities (5-6 A/dm 2 ).
  • an area of good quality coats was found at low current densities (0.5-1 .5 A/dm 2 ).
  • the resulting coats were black and loose in the whole range of current densities.
  • a probable cause was tin chloride complexes formed from which tin cannot be electroplated.
  • Electrolytic tin separation from solution after electronic scrap digestion A filtered solution directly after electronic scrap digestion was subjected to electrolysis. An insoluble platinum gauze anode was used, and copper foil was the cathode. The parameters of electrolysis are shown in Table 7.
  • the resulting coating was subjected to quantitative analysis using a scanning electron microscope with an X- ray microanalyser (type: Quanta 250 FEG , FEI Company). With the EDS detector fitted in the microscope, quantitative analysis of the resulting coating was performed ; for results, see Table 8.
  • the coating was also analysed at a 20377 magnification.
  • the quantitative analysis was performed at two magnifications, in different spots of the resulting tin coat. Tin content in the coat was 75%.
  • the resulting surface was not uniform , with spots where tin was not deposited.
  • deposited crystals are clearly seen (irregular, of various sizes).
  • Electrolytic tin separation from diluted solution after electronic scrap digestion A filtered solution after electronic scrap digestion, diluted so that tin concentration was 20 g/dm 3 (typical tin concentration in acidic tin plating baths), was subjected to electrolysis. A platinum gauze anode was used, and copper foil was the cathode. The parameters of electrolysis are shown in Table 9.
  • the resulting coating was subjected to quantitative analysis using a scanning electron microscope with an X-ray microanalyser (type: Quanta 250 19FEG , FEI Company). The coating seen at a 1395 magnification showed that the resulting surface started to be discontinuous and blisters started to appear.
  • Table 1 Results of quantitative analysis of coating obtained from diluted bath after electronic scrap digestion.
  • the coating was also analysed at a 1 1673 magnification.
  • Table 1 1 Parameters of electrolysis.
  • the resulting coating was subjected to quantitative analysis using a scanning electron microscope with an X- ray microanalyser (type: Quanta 250 FEG, FEI Company).
  • the resulting surface was uniform, without blisters or dendrites.
  • the quantitative analysis was performed at two magnifications, in different spots of the resulting tin coat. Tin content in the coat was 96%. The resulting coat was uniform, without spots where tin was not deposited. At a 12088 magnification, distinct metal crystals were seen occupying the whole cathode surface.
  • the depleted bath was reused for electronic scrap digestion. 4% potassium nitrate was added to the depleted bath and electronic scrap was digested again. Tin content increased to 47.5 g/dm 3 .
  • the depleted bath directly after electrolysis can be reused for electronic scrap digestion. Bath composition after reuse for electronic scrap digestion is shown in Table 1 5.
  • electronic scrap is used as a granulate.
  • it may have any form, such as pellets, granules, etc., or be non-agglomerated, for example in the form of flakes, chips, etc. , resulting directly from processes for scrap recovery from electronic waste.
  • the processes for scrap recovery from electronic waste are known and will not be discussed here.
  • digested scrap is obtained which is practically free from any tin material, that is, tin or tin and lead, being predominantly copper.
  • the copper is a valuable raw material used for processing to obtain pure copper.
  • certain electrodes are listed.
  • the cathodes may be made from any metal or metal alloy, preferably from tin foil.
  • any conductive material resistant to the electrolyte which does not separate into layers during electrolysis may be used, such as tantalum, titanium with platinum metal layers and compounds thereof. Electrolysis is conducted in conventional electrolysers which will not be discussed in detail here.
  • lead as metal or alloys or compounds increases current densities during electrolysis.
  • electrolysis may be conducted at higher current densities, such as 5-6 A dm 2 , whereby a tin and lead alloy is obtained.
  • baths without lead electrolysis is conducted at current densities of 0.5-1 .5 A/dm 2 , whereby substantially pure tin is deposited. Therefore, it may be preferable to add lead considering the increased speed of electronic scrap processing.
  • the solution obtained in electronic scrap digestion is an electrolysis solution also called an electrolysis bath.
  • the solution may be adjusted before electrolysis. This means that composition thereof may be modified or controlled accordingly to obtain an electrolytic material with desired composition after electrolysis.
  • the electrolysis solution is adjusted as early as at the step of scrap digestion with a leaching solution by adding lead, its alloys or compounds. If so, electrolytic tin and lead alloys are obtained in electrolysis.
  • electrolytic tin and lead alloys with special composition may be obtained.
  • the lead compounds added are for example lead carbonate, lead oxide or lead hydroxide. Tin compounds may be added to the electrolysis solution or to the digestion solution, such as tin carbonate, to maintain specific composition of the electrode material obtained in the process.
  • Excess tin may be precipitated from the electrolysis solution in the form of barely soluble compounds, such as tin oxalate.
  • Excess lead may also be precipitated as lead sulphate, for example.
  • Tin may also be oxidised to tin 4+ using hydrogen peroxide or another oxidiser to precipitate metastannic acid which gradually loses water and transforms into tin dioxide.
  • the processes discussed above may as well be conducted during electrolysis and during electronic scrap digestion. Materials important in technology are recovered in such processes, such as tin dioxide, lead sulphate, lead carbonate, tin carbonate, phosphates, etc.
  • the s, p, d and f block elements and their compounds may pass to the solution with tin.
  • the elements or their compounds accumulate, which has an adverse effect on the electrolysis process. Therefore, such elements or their compounds are removed from the solution.
  • the elements or their compounds may be removed at any time: they may be removed from the digestion solution, from the electrolysis solution immediately before electrolysis, during electrolysis or after electrolysis.
  • the electrolysis solution When the electrolysis solution is recycled after electrolysis has ended (the spent electrolysis solution), it may be regenerated as discussed above.
  • the regeneration involves restoring digestion properties of the spent electrolysis solution, for example by supplementing the alkanesulphonic acid, nitrate ions or additives to the electrolysis solution, as listed in the aforementioned example.
  • the regenerated electrolysis solution is recycled to the process as the digestion solution.
  • the processes for the removal of the s, p, d and f block elements and their compounds and regeneration include filtration, ultrafiltration , osmosis, electrodialysis, treatment with magnetic field, precipitation of compounds having low solubility, freezing out, crystallisation, concentration, evaporation, extraction, ion exchange, chelation, selective oxidation or reduction, or combinations thereof.
  • the processes are known to one skilled in the art and will not be discussed here.
  • a spent electrolysis solution which contains alkanesulphonic acid and nitrate ions.
  • the spent electrolysis solution is preferably recycled to the process, optionally following treatment, such as filtration, regeneration, removal of components with adverse effect on digestion and electrolysis. If so, little waste is generated in the process, to be disposed off accordingly. If not, the spent solution is fed to the process as waste. Being biodegradable, the waste is much less harmful to the environment than conventional digestion solutions based on strong inorganic acids.
  • the waste may be used for processing to recover desired components, such as the alkanesulphonic acid.
  • a tin material is obtained as a result of electrolysis, being substantially pure tin or a tin and lead alloy. Such materials are important for technology and used in further processing. They are used for the manufacture of bearing metals, type metals, alloys for precision casts, low melting alloys (Wood alloys), new soldering alloys, ceramics, glass pigments and many others.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

L'invention concerne un procédé permettant la récupération d'un matériau à base d'étain à partir de déchets électroniques, les déchets électroniques contenant le matériau à base d'étain étant fournis, le matériau à base d'étain présents dans les déchets électroniques étant digéré à l'aide d'une solution de digestion de telle sorte qu'une solution d'électrolyse et des déchets électroniques traités, sensiblement dépourvus d'un matériau à base d'étain soient obtenus, les déchets électroniques après la digestion étant utilisés pour un autre traitement, la solution d'électrolyse étant soumise à une électrolyse de telle sorte qu'un matériau à base d'étain et une solution d'électrolyse utilisée soient obtenus et le matériau à base d'étain obtenu par électrolyse et la solution d'électrolyse utilisée étant transférés vers un autre traitement. L'invention concerne également un matériau à base d'étain obtenu par électrolyse à l'aide du procédé de l'invention.
PCT/IB2014/066555 2014-06-26 2014-12-03 Procédé permettant la récupération d'un matériau à base d'étain à partir de déchets électroniques et matériau électrolytique à base d'étain obtenu à l'aide du procédé WO2015025304A2 (fr)

Applications Claiming Priority (2)

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PL408674A PL408674A1 (pl) 2014-06-26 2014-06-26 Sposób odzyskiwania materiału cynowego ze złomu elektronicznego i elektrolityczny materiał cynowy otrzymywany tym sposobem
PLPL408674 2014-06-26

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WO2015025304A3 WO2015025304A3 (fr) 2015-07-16

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108300872A (zh) * 2018-04-28 2018-07-20 昆山雅鑫化工有限公司 用于电路板回收锡的装置及其方法
CN113046564A (zh) * 2021-03-23 2021-06-29 江苏净拓环保科技有限公司 一种废退锡水回收与再生方法
CN114759182A (zh) * 2022-05-25 2022-07-15 昆明理工大学 石墨烯包覆草酸锡负极材料及其制备方法、电池
JP7324912B2 (ja) 2016-12-19 2023-08-10 ヴェオリア エンバイロメント－ブイイー 電気伝導性混合物中に含有されるスズ及び／又は鉛を抽出するための電解法

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JP2671276B2 (ja) * 1986-08-29 1997-10-29 日鉱金属 株式会社 銅系スクラツプの処理方法
US4944851A (en) * 1989-06-05 1990-07-31 Macdermid, Incorporated Electrolytic method for regenerating tin or tin-lead alloy stripping compositions
US4921571A (en) * 1989-07-28 1990-05-01 Macdermid, Incorporated Inhibited composition and method for stripping tin, lead or tin-lead alloy from copper surfaces
CN102330112A (zh) * 2011-08-18 2012-01-25 华星集团环保产业发展有限公司 一种从废旧电路板中回收锡和铅的方法及其所用的装置
KR20130125590A (ko) * 2012-05-09 2013-11-19 고등기술연구원연구조합 폐 리드프레임 스크랩으로부터의 주석 회수 방법

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7324912B2 (ja) 2016-12-19 2023-08-10 ヴェオリア エンバイロメント－ブイイー 電気伝導性混合物中に含有されるスズ及び／又は鉛を抽出するための電解法
CN108300872A (zh) * 2018-04-28 2018-07-20 昆山雅鑫化工有限公司 用于电路板回收锡的装置及其方法
CN113046564A (zh) * 2021-03-23 2021-06-29 江苏净拓环保科技有限公司 一种废退锡水回收与再生方法
CN114759182A (zh) * 2022-05-25 2022-07-15 昆明理工大学 石墨烯包覆草酸锡负极材料及其制备方法、电池

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PL408674A1 (pl) 2016-01-04

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