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US20120186397A1 - Reclaiming of lead in form of high purity lead compound from recovered electrode paste slime of dismissed lead batteries and/or of lead minerals - Google Patents

Reclaiming of lead in form of high purity lead compound from recovered electrode paste slime of dismissed lead batteries and/or of lead minerals Download PDF

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Publication number
US20120186397A1
US20120186397A1 US13/388,012 US200913388012A US2012186397A1 US 20120186397 A1 US20120186397 A1 US 20120186397A1 US 200913388012 A US200913388012 A US 200913388012A US 2012186397 A1 US2012186397 A1 US 2012186397A1
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United States
Prior art keywords
lead
sulphate
solution
acetate salt
salt
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US13/388,012
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English (en)
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Federica Martini
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Millbrook Lead Recycling Technologies Ltd
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Millbrook Lead Recycling Technologies Ltd
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Assigned to MILLBROOK LEAD RECYCLING TECHNOLOGIES LIMITED reassignment MILLBROOK LEAD RECYCLING TECHNOLOGIES LIMITED ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MARTINI, FEDERICA
Publication of US20120186397A1 publication Critical patent/US20120186397A1/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/54—Reclaiming serviceable parts of waste accumulators
    • 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
    • C22B13/00—Obtaining lead
    • C22B13/04—Obtaining lead by wet processes
    • C22B13/045—Recovery from waste materials
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • 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
    • 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
    • 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
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
    • 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
    • Y02W30/84—Recycling of batteries or fuel cells

Definitions

  • This disclosure relates to techniques for reclaiming high purity lead compound from impure mixtures, like recovered electrode paste slime of dismissed batteries or lead minerals.
  • the starting material in the form of electrode paste slime or finely ground and eventually pre-treated lead mineral is leached using an acid different from sulphuric, adding hydrogen peroxide or other reducing agent or lead dioxide that may be present in the starting material and sulphuric acid for converting all lead compounds to insoluble lead sulphate which is separated together with other insoluble substances and is thereafter selectively dissolved in an aqueous solution of a solubilizing compound.
  • a carbonate salt for precipitating carbonate/oxycarbonate of lead.
  • the acid leaching step of the impure starting material implies certain costs and treatment plant complexities.
  • the novel approach unexpectedly found outstandingly efficient consists in directly suspending the impure starting material in a lead sulphate dissolving aqueous solution of an acetate salt and adding thereto either hydrogen peroxide or a sulphite or alternatively bubbling sulphurous anidride through it, in a measure adapted to reduce any lead dioxide expected to be present in the impure starting material to lead oxide, and sulphuric acid in a measure adapted to convert all lead oxide to lead sulphate that remains dissolved in the selected dissolving salt solution.
  • a clear solution containing the dissolved lead sulphate may then be separated from a solid phase residue that includes all undissolved impurities contained in the impure starting material.
  • the hydroxide solution now containing the residual lead stripped from the previously separated solid phase of impurities may be introduced in the liquid acetate solution containing the lead sulphate in the vessel in which hydroxide of the same cation of the acetate salt is introduced for precipitating the lead contained as lead sulphate in the liquid acetate solution in form of lead oxide or hydroxide.
  • Precipitation of high purity lead compound from the clear lead sulphate solution may then by effected either by adding to the solution carbonate of the same cation of the acetate salt used for selectively dissolved lead sulphate for precipitating insoluble carbonate/oxycarbonate of lead, as contemplated in the process disclosed in said prior PCT patent application No.
  • the clear solution of acetate salt becomes progressively enriched of sulphate of the same cation of the acetate salt used for selectively dissolving lead sulphate, it may be recycled to the suspension step of the impure starting material for as long as the sodium sulphate concentration remains below saturation.
  • the solution may be cooled to about 10° C. for selectively crystallizing and precipitating solid phase constituted by sulphate of the cation of the acetate salt used, which is recovered by filtering.
  • the clear acetate salt solution freed of the sulphate salt may then be recycled to the suspension bath of the impure starting material.
  • the acetate solution is percolated through a column filled with chelating resin for sequestering any residual lead ions in the solution, before cooling the solution in order to produce lead-free sulphate salt, as a by-product, of broader market acceptance.
  • FIG. 1 is a flow sheet of the main steps of the process of this disclosure for reclaiming high purity lead oxide from dismissed battery electrode slime or lead minerals, alternatively for producing pure lead carbonate/oxycarbonate or pure lead oxide/hydroxide.
  • FIG. 2 is a simplified diagram of a plant for reclaiming highly pure lead compound from dismissed battery electrode slime or lead minerals, alternatively as pure lead carbonate/oxycarbonate or pure lead oxide/hydroxide, according to the alternative process flows of FIG. 1 .
  • the impure starting solid material is suspended in an aqueous solution of a salt capable of dissolving lead sulphate, such as for example an acetate salt of sodium, ammonium, potassium, urea, mono-, di- or tri-ethanolamine.
  • a salt capable of dissolving lead sulphate such as for example an acetate salt of sodium, ammonium, potassium, urea, mono-, di- or tri-ethanolamine.
  • sulphuric acid in an amount necessary to convert all oxides present in the starting material to sulphate, and a reducing agent chosen among hydrogen peroxide, a sulphite salt and sulphurous anhydride, is gradually added or bubbled through the suspension bath in an amount necessary to reduce any lead dioxide that may be contained in the starting material (as would be the case with slime from discarded lead batteries) to lead oxide.
  • a reducing agent chosen among hydrogen peroxide, a sulphite salt and sulphurous anhydride
  • Step ( 1 ) of the process flow sheet of FIG. 1 in the suspension bath of the starting material take place the chemical reactions that are formally described herein below in view of the fact that they take place simultaneously, causing the conversion of all lead compounds to sulphate that dissolves in the aqueous solution containing the specific dissolving salt mentioned above.
  • the following reactions relate to an exemplary embodiment of reclaiming high purity lead compound from electrode paste slime of dismissed batteries in which lead sulphate is present as measure component (close to about 60% by weight) in the impure starting material and dissolved in the aqueous solution of sodium acetate.
  • an aqueous solution of tri-hydrated sodium acetate dissolved in water in a concentration comprised between 37.5 and 54.5% by weight can be satisfactorily used.
  • Sulphuric acid is added in an amount corresponding to or just exceeding the stoichiometric requirement for converting all lead oxides to lead sulphate as pre-evaluated for the impure starting material to be processed.
  • hydrogen peroxide the amount of which may also be pre-calculated in terms of the stoichiometric requirement for reducing the lead dioxide contained in the starting material.
  • the amount of electrode paste that can be treated in a certain volume of solution depends on the solubilizing capacity of the lead sulphate in the solution of the selected acetate salt and of the added amount of sulphuric acid.
  • the ability of dissolve lead sulphate of the acetate salt solution depends from its salt concentration. By way of example, one liter of aqueous solution with a concentration of 37.5% by weight of sodium acetate is able to dissolve 100 g of lead sulphate. By increasing the concentration of the acetate salt, the amount of lead sulphate that can be dissolved increases proportionally.
  • the temperature at which the above described reactions can be carried out in the suspension bath may be comprised between about 10° C. up to boiling point.
  • the suspension may be stirred with a pails or turbine mixer in order to favor breaking down of lead compound aggregates.
  • the combination of the chosen operating conditions (type and fineness of the starting solid material, type and concentration of the lead sulphate dissolving salt solution, eventual lead dioxide reducing agent addition, temperature, stirring mode) will influence the time needed for completing this first step ( 1 ) of the all-wet reclaiming process.
  • the sulphuric acid used for the sulphation of all the lead oxide in the solution should preferably have a high concentration in order not to excessively dilute the lead sulphate dissolving solution.
  • a limpid acetate solution containing lead sulphate may be separated from the solid phase residues, for example by filtration. All insoluble impurities and substances are therefore separated from the solution (Step 2 of the flow sheet of FIG. 1 ).
  • the critical temperature is in the vicinity of 70° C., therefore the precipitation may be carried out at about 72-73° C. (unless for some reason one should prefer to recover a highly purified lead hydroxide, thermally convertible to lead oxide eventually).
  • Step 3 of the flow chart of FIG. 1 consists in adding to the liquid acetate solution containing substantially all the lead content of the starting material in the form of lead sulphate, instead of a hydroxide, a carbonate of the same cation of the selected acetate salt (i.e. either sodium, potassium or ammonium), which produces a selective precipitation of lead carbonate or a mixture of lead carbonate and oxycarbonate, because of their much lower solubility than that of lead sulphate.
  • precipitation may be conducted at any temperature comprised between ambient temperature up to boiling point.
  • Step 4 of the flow chart of FIG. 1 the precipitated lead oxide or hydroxide or carbonate/oxycarbonate is separated by filtration (Step 4 of the flow chart of FIG. 1 ) from the solution while sulphate of the cation of the hydroxide or carbonate used for precipitating the lead as insoluble oxide (or hydroxide) or carbonate (and/or oxycarbonate) remains in the solution.
  • the limpid acetate solution now containing also the sulphate of the same cation of the acetate salt, can be integrally recycled to the suspension bath of selective dissolution of the lead sulphate (Step 1 ) of the process, for as long as the content of sulphate remains below saturation (this limit depends primarily on the type of dissolving salt solution of the lead sulphate and processing conditions).
  • Step 8 of the flow sheet of FIG. 1 This may be easily done by exploiting the different solubilities at different temperatures of the sulphate salt (i.e. of sodium, potassium or ammonium sulphate) from that of the corresponding acetate salt for selectively crystallizing the sulphate and separating it from the acetate solution.
  • the sulphate salt i.e. of sodium, potassium or ammonium sulphate
  • the concentration of the aqueous solubilizing salt solution and the temperature at which lead sulphate dissolution in it is carried out are not essential parameters because they simply influence the time necessary for completing the reactions discussed above and the quantity of lead sulphate that may be dissolved in the solution.
  • the solubilizing solution after precipitation of the dissolved lead as oxide or hydroxide or carbonate/oxycarbonate, is recycled back and therefore one's operates with a recycled solution, more and more recycles may be necessary to complete dissolution of a given quantity of lead sulphate.
  • novel approach of this disclosure has proved itself outstandingly suitable to process electrode paste slimes where the amounts of the three main lead compounds, namely lead sulphate, lead oxide and lead dioxide, oscillate in the vicinity of a mean value by a range of variability of about 2% by weight and this may in practice impede to calculate exactly the quantity of sulphuric acid solution for converting to sulphate all lead oxides present in the impure starting material.
  • the amounts of the three main lead compounds namely lead sulphate, lead oxide and lead dioxide
  • the solution is preferably percolated through a column filled with chelating resin for sequestering any residual lead ions in the solution (Step 5 of the flow sheet of FIG. 1 ), before cooling the solution to about 10° C. for precipitating a crystalline solid phase (Step 6 of the flow sheet of FIG. 1 ), constituted by sulphate of the cation of the acetate salt used, which is recovered by filtering (Step 7 of the flow sheet of FIG. 1 ).
  • the clear acetate salt solution freed of the sulphate salt may then be recycled to the suspension bath of the impure starting material while the lead-free sulphate salt constitutes a marketable by-product.
  • 80 g of recovered dried electrode paste having a lead content, expressed as metal equivalent, of 72% was treated under stirring with 1000 ml aqueous solution of tri-hydrated sodium acetate at 37.5% by weight, with the addition of g 12.2 of concentrated sulphuric acid at 94-96% by weight, at the temperature of 83° C. Successively, hydrogen peroxide at 32% by weight was slowly added to the suspension (dropwise for about 10 minutes) until no further clarification of the suspension was observed.
  • the hot suspension was then filtered and the separated solid phase was constituted by insoluble lead compounds and lead compound concretions, electrode grid fragments and various additives used for making the electrode paste such as carbon black, barium sulphate, fibers, etc. and impurities such as sand, plastic materials, etc.
  • the amount of this dark grey solid phase was about 4-12% by weight of the solid mass of the dry electrode paste.
  • the filtered limpid solution containing lead sulphate was stirred at 83° C. adding thereto sodium hydroxide until reaching a practically complete precipitation of the lead in the form of lead oxide.
  • the suspension was thereafter filtered separating the precipitate from the solubilizing solution of sodium acetate now enriched of sodium sulphate that was recycled to the stirred lead sulphate dissolution vessel for as long as the content of sodium sulphate in the solution remained below saturation.
  • the purified sulphate solution (practically lead-free) was slowly cooled to 10° C., under slow stirring, for precipitating a crystalline solid phase constituted by sodium sulphate that was then recovered by filtering the suspension, while the clear solution was recycled to the dissolution vessel of the lead sulphate.
  • the filtered lead oxide accurately rinsed with de-ionized water was dried at 160° C. for as long as reaching constancy of weight.
  • the separated dark grey solid phase was suspended in sodium hydroxide at 40% by weight, at 50° C. for 15 minutes.
  • the separated limpid liquid phase was introduced into the limpid acetate solution containing also the lead sulphate, as part of the required amount of sodium hydroxide for precipitating all lead in solution as lead oxide or hydroxide (according to a preferred embodiment) in consideration of the fact that also the lead present in the solution as sodium plumbite converts itself to lead oxide (or hydroxide).
  • the calculated maximum quantity of recoverable lead oxide was of 62.05 g while the quantity of lead oxide effectively recovered was of 62.03 g for a recovery yield of 99.96%.
  • the lead oxide (whether directly produced by the all-wet process or obtained by heating lead carbonate/oxycarbonate produced by the all-wet process) is perfectly suitable for preparing electrode pastes for new batteries.
  • a mineral or a mixture of minerals of lead may be substantially similar to the above described embodiments, an essential pre-step being that of converting as much as possible any different salt of lead present in the mineral to either lead sulphate or to lead oxide.
  • the mineral in case of galena, the most common lead mineral, the mineral should be heated in air, according to common roasting techniques, until oxidizing the lead sulphite to sulphate.
  • the other common mineral anglesite does not need any prior treatment being itself already constituted by lead sulphate.
  • the mineral(s) should be finely ground for facilitating their processing.
  • FIG. 2 is a schematic diagram of possible embodiments for an industrial plant for reclaiming variable lead in form of high purity compounds from recovered electrode paste of dismissed lead batteries and/or finally ground led minerals, eventually pretreated for converting as much of the lead compounds to lead sulphate.
  • the scheme of FIG. 2 provides a multi-embodiment illustration of the discussed processing alternatives (though sodium is indicated as the exemplary selected cation of both the acetate salt and of the alternatively added compounds for precipitating the desired pure compound of lead, according to the various alternatives).
  • a first reactor RAC ( 1 ) in which the impure material is suspended in an aqueous acetate salt solution, is associated a first solid-liquid separator F( 1 ) for separating the lead sulphate containing solution from the solid phase constituted by insoluble impurities of the impure starting material.
  • a second reactor for precipitating the desired lead compound of high purity that in the multiple alternative scheme of FIG. 2 is anyone of the reactors RAC ( 2 ), RAC ( 3 ) and RAC ( 4 ), is associated a second solid-liquid separator, that is the related one F( 2 ), F( 3 ) and F( 4 ).
  • the third and last reactor RAC ( 5 ) and associated third and last solid-liquid separator F( 5 ) are required for at least periodically (or more preferably continuously) treating the recycling acetate salt solution and to recycle it to the first sulphate dissolving reactor RAC ( 1 ).
  • the treatment consists of selectively crystallizing by virtue of the significantly different solubilities of the acetate salt and of the sulphate of the same cation of the acetate salt, introduced in the second reactor for precipitating the desired lead compound, and removing it from the system.
  • This step must be performed (continuously or intermittently) in order to prevent saturating the recycling acetate salt solution with the sulphate of the same cation, which if let to occur would cause co-precipitation of this salt together with the lead sulphate (making vain the purification process).
  • the plant may include an exchange resin column C( 1 ) filled with an appropriate chelating resin, through which the solution, when directed to the selective sulphate crystallization reactor RAC ( 5 ) (whether continuously or periodically) passes, for sequestering residual lead ions that may be present in the solution.
  • an exchange resin column C( 1 ) filled with an appropriate chelating resin, through which the solution, when directed to the selective sulphate crystallization reactor RAC ( 5 ) (whether continuously or periodically) passes, for sequestering residual lead ions that may be present in the solution.
  • the chelating resin filler will gradually loose its activity and periodically a stripping of sequestered lead ions must be carried out by circulating through the column (C 1 ) acetic acid for a certain period of time.
  • the lead ridden stripping solution of acetic acid used for this periodical re-activation of the exchange resin, now containing lead acetate, may be “disposed of” by simply introducing it into the first reactor RAC ( 1 ), as shown by the relative line.
  • the multi-embodiment plant diagram of FIG. 2 illustrates also the optional reactor RAC (2bis) in which, if desirable, in consideration of the composition of the impure starting material to be processed, residual amount of lead that may remain associated with the separated solid phase of impurities, in form of compounds or concretions that could not be dissolved during the treatment of the impure material in the first reactor RAC ( 1 ).
  • the separated solid phase is suspended in hot concentrated solution of hydroxide of the same cation of the selected acetate salt for dissolving also these compounds of lead or concretions thereof.
  • the associated liquid-solid separator F (2bis) permits to separate all non-lead impurities from a liquor of hydroxide containing sodium plumbite dissolved in it which may be conveniently used as part of hydroxide addition in a second reactor RAC ( 2 ) or RAC ( 3 ) that may be used for precipitating all the lead in the solution as lead oxide or lead hydroxide, according to a preferred embodiment.

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US13/388,012 2009-07-30 2009-07-30 Reclaiming of lead in form of high purity lead compound from recovered electrode paste slime of dismissed lead batteries and/or of lead minerals Abandoned US20120186397A1 (en)

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PCT/IT2009/000344 WO2011013149A1 (fr) 2009-07-30 2009-07-30 Récupération de plomb sous forme de composé de plomb de haute pureté à partir de boue ou pâte d'électrode récupérée de batteries au plomb mises au rebut et/ou de minerais de plomb

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US (1) US20120186397A1 (fr)
EP (1) EP2460220A1 (fr)
JP (1) JP2013500566A (fr)
CN (1) CN102576918A (fr)
AU (1) AU2009350377A1 (fr)
CA (1) CA2769175A1 (fr)
IN (1) IN2012DN01754A (fr)
MX (1) MX2012001350A (fr)
RU (1) RU2012107523A (fr)
TW (1) TW201119946A (fr)
UA (1) UA100651C2 (fr)
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US20160308261A1 (en) * 2013-12-03 2016-10-20 Verdeen Chemicals, Inc. Zero lead pollution process for recycling used lead acid batteries
US9670565B2 (en) 2014-06-20 2017-06-06 Johnson Controls Technology Company Systems and methods for the hydrometallurgical recovery of lead from spent lead-acid batteries and the preparation of lead oxide for use in new lead-acid batteries
US10062933B2 (en) 2015-12-14 2018-08-28 Johnson Controls Technology Company Hydrometallurgical electrowinning of lead from spent lead-acid batteries
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JP6550582B1 (ja) * 2018-11-27 2019-07-31 株式会社ジェーエフシーテック 鉛の製造方法および製造設備
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US20160308261A1 (en) * 2013-12-03 2016-10-20 Verdeen Chemicals, Inc. Zero lead pollution process for recycling used lead acid batteries
US10122052B2 (en) 2014-06-20 2018-11-06 Johnson Controls Technology Company Systems and methods for purifying and recycling lead from spent lead-acid batteries
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CA2769175A1 (fr) 2011-02-03
MX2012001350A (es) 2012-02-22
TW201119946A (en) 2011-06-16
RU2012107523A (ru) 2013-09-10
EP2460220A1 (fr) 2012-06-06
WO2011013149A1 (fr) 2011-02-03
UA100651C2 (ru) 2013-01-10
IN2012DN01754A (fr) 2015-06-05
AU2009350377A1 (en) 2012-03-08
CN102576918A (zh) 2012-07-11

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