WO2012143394A1 - Procédé pour la récupération de thallium d'une solution aqueuse - Google Patents

Procédé pour la récupération de thallium d'une solution aqueuse Download PDF

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Publication number
WO2012143394A1
WO2012143394A1 PCT/EP2012/057079 EP2012057079W WO2012143394A1 WO 2012143394 A1 WO2012143394 A1 WO 2012143394A1 EP 2012057079 W EP2012057079 W EP 2012057079W WO 2012143394 A1 WO2012143394 A1 WO 2012143394A1
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WO
WIPO (PCT)
Prior art keywords
thallium
aqueous solution
resin
ppm
iminodiacetic
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/EP2012/057079
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English (en)
Inventor
Cédric HUMBLOT
Jean-Marie Blondel
Frédéric Nicolas
Francis Grosjean
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Solvay SA
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Solvay SA
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Filing date
Publication date
Application filed by Solvay SA filed Critical Solvay SA
Publication of WO2012143394A1 publication Critical patent/WO2012143394A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C22B61/00—Obtaining metals not elsewhere provided for in this subclass
    • 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
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • 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 relates to a method of removing impurities, especially thallium, from an aqueous solution from an industrial process, in particular, obtained from rice hull ashes, ashes of wood combustion plants, ashes of coal combustion plants, cement kiln residue, steel industry dust, or dust from iron sintering processes, preferably using an aminophosphonic or an industrial process, in particular, obtained from rice hull ashes, ashes of wood combustion plants, ashes of coal combustion plants, cement kiln residue, steel industry dust, or dust from iron sintering processes, preferably using an aminophosphonic or an industrial process, in particular, obtained from rice hull ashes, ashes of wood combustion plants, ashes of coal combustion plants, cement kiln residue, steel industry dust, or dust from iron sintering processes, preferably using an aminophosphonic or an industrial process, in particular, obtained from rice hull ashes, ashes of wood combustion plants, ashes of coal combustion plants, cement kiln residue, steel industry dust, or dust from iron sintering processes,
  • the present invention also provides a process of removing impurities, especially thallium, and recovering and recycling the insoluble or removed species.
  • alkaline earth metals and other heavy metals, especially barium, calcium, chromium, strontium, and thallium.
  • These metals often remain in the form of a mixture of different salts, for example, chloride, sulfate, hydroxide, or carbonate. Since these metals will have a bad effect on the usage, moreover these metals (especially thallium) can be very expensive, they are needed for removal, recovery, and recycle with high purity.
  • metals can be recovered from aqueous solutions electrolytically or by precipitation with precipitating agents, if necessary in the presence of bases like NaOH.
  • German patent application DEI 02009018959A describes brine comprising potassium chloride which contains dissolved thallium.
  • the content of thallium in the brine can be reduced.
  • This process has the disadvantages that valuable product, namely the potassium chloride with a high content of precipitated thallium is lost, and that the precipitated thallium has no real value because it is dissipated in a great amount of potassium chloride. A very high thallium recovery is therefore needed.
  • the present invention provides a high removal yield of thallium compared to other impurities, and thallium can be selectively removed from the residue, recovered, and reused.
  • thallium can be selectively removed from the residue, recovered, and reused.
  • resins for example, thiol-based resins disclosed in patent EP 442778 above, they have poor removal yield of thallium while eliminating most other metals, most of which are divalent or trivalent, so it is impossible to obtain thallium with high purity.
  • the present invention is directed to a simple method of removing impurities, especially thallium, from an aqueous solution, to obtain a purified aqueous solution with a very low concentration of thallium, especially preferably of about 0.1 ppm or less, and for recovery and recycling especially of the removed thallium content.
  • the method according to the invention includes a step of removing impurities, especially thallium, from an aqueous solution from an industrial process, using a chelating agent capable of complexing thallium ions, preferably an aminophosphonic or an iminodiacetic chelating resin, to obtain a purified aqueous solution.
  • a chelating agent capable of complexing thallium ions preferably an aminophosphonic or an iminodiacetic chelating resin
  • the present method works well with a starting aqueous solution which has a small amount of thallium, for example, about 2 ppm or less due to high removal efficiency.
  • the method of the invention can be performed, for example, to treat a solution comprising potassium chloride and Tl ions. Therefore, the resulting potassium chloride obtained by crystallization of the residue has a thallium content of 2 ppm or less, preferably equal to or less than 1 ppm, and even more preferably, equal to or lower than 0.5 ppm, which is suitable for most common applications.
  • ppm denotes ppm by weight unless other wise indicated.
  • the present inventors discovered that especially an aminophosphonic or an iminodiacetic chelating resin is very useful in the treatment of an aqueous solution, especially for selective removal of thallium. It is therefore possible to recover thallium at a lower concentration when sludge recovered during regeneration of the aminophosphonic or the iminodiacetic resin is treated.
  • the present invention provides : (1) a purification method of thallium from an aqueous solution using an aminophosphonic or an iminodiacetic chelating resin, (2) a recovery method of the adsorbed thallium onto the an aminophosphonic or an iminodiacetic chelating resin ; and (3) a recycling method of the recovered thallium.
  • one of the essential features of the invention resides in a method of removing impurities, especially thallium from an aqueous solution from an industrial process, preferaby using an aminophosphonic or an
  • the iminodiacetic chelating resin more preferably an iminodiacetic resin to obtain a purified aqueous solution.
  • the aqueous solution may, in particular, contain potassium chloride, which will be purified by this process and used for other processes.
  • one or more other ingredients which are selected from alkali metals, alkali earth metals, or other heavy metals, as well as thallium, are removed from the aqueous solution.
  • the other ingredients are selected from one or more of barium, calcium, chromium, lithium, silicon or strontium, especially barium, calcium, lithium, or strontium. It is clear for the expert that commonly, those other ingredients are present in the form of salts, e.g. in the form of the chlorides.
  • the method of the invention may further comprise one or more steps of removing one or more other ingredients before the removal of thallium.
  • the aqueous solution is subjected to pre-treatment, one or more times, to remove one or more other ingredients.
  • the aqueous solution contains 2 ppm or less of thallium and 30 weight % or more of other ingredients based on the total weight of aqueous solution.
  • monovalent thallium ions are removed from the aqueous solution along with trivalent thallium ions.
  • the resulting aqueous solution contains less thallium than before the purification treatment.
  • the resulting purified aqueous Osolution contains 2 ppm or less, preferably 0.1 ppm or less, more preferably 0.02 ppm or less of thallium ions.
  • the content of thallium dropped to at least 0.4 ppm.
  • removal efficiency is much lower than that using the present method.
  • the starting aqueous solution has a small amount of thallium, for example, about 2 ppm, the prior methods do not work well. However, with the present method, even a small amount of thallium can be removed from the aqueous solution.
  • the pH of the aqueous solution is at least 9, preferably at least 10, more preferably at least 1 1.
  • the term "at least” denotes "equal to or higher than”.
  • the process temperature is between 10 and 80°C, preferably between 40 and 80°C, still more preferably between 45 and 55°C, and most preferably about 50°C.
  • the method preferably further comprises one or more steps of recovering thallium from the chelating agent, especially from the aminophosphonic chelating resin or from the iminodiacetic chelating resin.
  • an acid is used in the recovery steps.
  • Said method further comprises one or more steps of precipitating and isolating thallium from the acid.
  • the recovery steps may comprise :
  • the aminophosphonic or the iminodiacetic chelating resin is reused after removing adsorbed ingredients.
  • the purified solution is subjected to one or more further processes, such as crystallization or electrolysis.
  • the iminodiacetic groups of a chelating resin only make complexes with multivalent metals. These complexes are very stable. Therefore, these resins have high selectivity and are capable of removing metals from a solution selectively.
  • the residue, an aqueous extract solution of which is purified according to the process of the present invention, is obtained by, for example, treating byproducts from metallurgical manufacture, preferably from steel manufacture, or by treating cement kiln dust from cement production.
  • Cement kiln dust (CKD) is preferably a fine-grained, solid, highly alkali metal waste removed from cement kiln exhaust gas by air pollution control devices.
  • Other residues from industrial processes of rice hull ashes, ashes of wood combustion plants, ashes of coal combustion plants, cement kiln residue, steel industry dust, or dust from iron sintering processes can be purified using the present process.
  • a suitable treatment may comprise, for example, contacting the residue with an aqueous solution to provide a suspension of solids in a solution of water soluble impurities.
  • the method according to the invention makes it possible to remove impurities contained in a residue, especially thallium, resulting in a purified aqueous solution having high purity and a very low concentration of thallium.
  • the residue may contain various impurities, including polyvalent metals, inorganic compounds, and/or organic compounds, as well as thallium.
  • Said residue may contain impurities from 10000 ppm to 0.001 ppm, preferably from 100 ppm to 0.001 ppm, more preferably from 1 to 0.001 ppm by weight of the residue.
  • the concentration of thallium in undisturbed natural soil is 2.2 to 29 ppm ⁇ See Xiao, "Environmental impact of thallium related to the mercury-thallium- gold mineralization in southwest Guizhouzhou Province, China," Chicoutimi, Universit du Qu bee Chicoutimi, 2001).
  • the thallium containing aqueous solution to be purified by the present invention has a concentration of thallium from 0.001 ppm to 100 ppm preferably from 0.1 ppm to 10 ppm, more preferably from 0.5 ppm to 2 ppm by weight of the total solution.
  • the preferred resin which can be used in the present invention can be any aminophosphonic-based or iminodiacetic-based resin.
  • the appropriate resins, identified by tests by inventors, include, but are not limited to,
  • LEWATIT ® TP 260 or LEWATIT ® TP208 (available from LANXESS SA), which are weakly acidic, macroporous cation exchange resins with chelating respectively aminophosphonic or iminodiacetic groups. It comprises
  • Lanxess offer the same type of resins like Dow Chemicals (Amberlite ® IRC747 and Amberlite ® IRC748), Mitsubishi
  • the aqueous solution may be pre-treated with any one of known methods in this field.
  • the residue can be pre-treated with, but is not limited to, iron salts and carbonates, especially FeCl 2 and Na 2 C0 3 .
  • This pre-treatment can decrease the other elements by precipitation, filtration, and/or decantation.
  • the aqueous solution is pretreated.
  • This preferred pretreatment serves to remove metal ions which might interfere with the method of the present invention to remove and, especially, to remove and recover thallium ions selectively, or which are undesired because they may contaminate the recovered thallium which desiredly should be pure.
  • alkaline earth metals and heavy metal cations such as the ions of Cd are removed in a pretreatment step.
  • This pretreatment step can be performed, for example, with an aminophosphonic acid resin.
  • the pretreated aqueous solution then contains essentially only monovalent cations, e.g. potassium ions in the form of potassium chloride, and thallium ions.
  • the thallium ions are then selectively removed from the pretreated solution, especially by contacting the solution with aminophosphonic-based or, especially, with iminodiacetic-based resin.
  • the present method works well when the pH of the aqueous solution to be purified is at least 9, preferably at least 10, more preferably at least 11, and the process temperature is between 10 and 80°C, preferably between 40 and 80°C, still more preferably between 45 and 55°C, and most preferably around 50°C.
  • the resin may be mixed with the aqueous solution in various ways, such as blending or stirring. After adsorption of thallium onto the resin, the adsorbed thallium can be separated from the resin for recycling. Any separating means in the field can be used.
  • the used resin can be recycled by a method where the removed impurities, especially thallium from an aqueous solution from an industrial process, are isolated as follows : (a) regenerating the resin as recommended by the producer (generally by countercurrent flow with water, an acid such as HC1, water, a base such as NaOH, and then water again, (b) adjusting the pH of the sludge recovered during the regeneration of the resin and oxidize the sludge with an appropriate oxidant, such as sodium hypochlorite or peroxide salt ; and (c) filtrating and washing of the precipitate, which is thallium trihydroxide
  • aminophosphonic resin can also be used in the previous treatment of the aqueous solution.
  • the method of the invention allows for the removal especially of thallium from an aqueous solution from an industrial process, in particular, obtained from rice hull ashes, ashes of wood combustion plants, ashes of coal combustion plants, cement kiln residue, steel industry dust, or dust from iron sintering processes. It is principally possible to remove and recover the thallium content of any residue where the removal of thallium is desirable.
  • earth contaminated with thallium or fertilizer mainly potassium chloride
  • the residue is extracted with water to obtain an aqueous solution containing thallium, and then, the method of the invention is performed.
  • a residue containing even low amounts of thallium e.g. less than 30 ppm, and even less than 2 ppm, can be treated efficiently.
  • the thallium content removed can be recovered in the form of a very pure thallium salt which is a further advantage.
  • the purified aqueous solution can be further treated to recover the remaining contents of other salts present, for example, to recover potassium chloride with an extremely low content of thallium.
  • Lewatit TP208 stirred during 1 h in a reactor at 50°C.
  • Duolite GT73 stirred during 50 min in a reactor at 50°C.
  • the amount of thallium remaining in the solution is 0.46 mg/kg for iminodiacetic-based resin, which is much less than 1.5 mg/kg for the thiol-based resin.
  • Lewatit TP208 stirred during 60 min in a reactor at 50°C.
  • the amount of thallium remaining in the solution is 0.46 mg/kg for iminodiacetic-based resin, which is much less than 1.2 mg/kg for the thiol-based resin.
  • Example 3 Influence of oxidation and pH
  • thallium By oxidation and pH adjustment of the initial solution, thallium can efficiently be removed from the solution and a precipitate of thallium hydroxide can be recovered.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

La présente invention porte sur un procédé d'enlèvement d'impuretés, en particulier de thallium, à partir d'une solution aqueuse provenant d'un procédé industriel, à l'aide d'un agent chélateur, en particulier d'une résine chélatrice aminophosphonique ou iminodiacétique. Selon le présent procédé, les ions thallium monovalents et trivalents, qui étaient difficiles à enlever dans un seul procédé avant la présente invention, peuvent être enlevés simplement en un seul procédé. De plus, la présente invention est très utile pour le traitement d'une solution aqueuse contenant une faible concentration de thallium et une concentration élevée d'autres ingrédients en raison de son rendement d'enlèvement élevé. La solution aqueuse purifiée ainsi obtenue traitée par le présent procédé contient de préférence moins de 0,1 ppm de thallium. Après enlèvement du thallium de la solution, le thallium peut être récupéré sélectivement sous forme de précipité de trihydroxyde de thallium par oxydation et ajustement du pH des boues de régénération de résine, et ensuite il peut être réutilisé dans d'autres procédés.
PCT/EP2012/057079 2011-04-20 2012-04-18 Procédé pour la récupération de thallium d'une solution aqueuse Ceased WO2012143394A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP11163265 2011-04-20
EP11163265.9 2011-04-20

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WO2012143394A1 true WO2012143394A1 (fr) 2012-10-26

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017127650A1 (fr) * 2016-01-21 2017-07-27 Archer Daniels Midland Company Procédés de récupération de catalyseurs
CN109811128A (zh) * 2019-02-14 2019-05-28 广州大学 一种从冶炼酸性废水回收铊及制备碘化亚铊的方法
CN115432854A (zh) * 2022-09-06 2022-12-06 水口山有色金属有限责任公司 一种高卤素污酸优先富集除铊的方法
CN115652114A (zh) * 2022-12-28 2023-01-31 长沙华时捷环保科技发展股份有限公司 一种含铊溶液中铊的资源化回收工艺

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2632763A (en) * 1948-05-25 1953-03-24 French T Hagemann Separation process for actinium
JPS5669226A (en) * 1979-11-09 1981-06-10 Agency Of Ind Science & Technol Purification of cadmium
EP0224209A2 (fr) * 1985-11-21 1987-06-03 Sumitomo Chemical Company, Limited Procédé pour la récupération de terres rares
EP0442778A1 (fr) 1990-02-05 1991-08-21 Metaleurop S.A. Procédé d'extraction de thallium
EP1116326A1 (fr) 1999-07-23 2001-07-18 Koninklijke Philips Electronics N.V. Element conducteur
DE102009018959A1 (de) 2009-04-25 2010-10-28 K-Utec Ag Salt Technologies Methode zur Reduzierung der Thalliumkonzentration in Mineralsalzlösungen
FR2951383A1 (fr) 2009-10-20 2011-04-22 Solvay Procede pour la valorisation conjointe de sels solubles contenus dans un residu d'un procede industriel

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2632763A (en) * 1948-05-25 1953-03-24 French T Hagemann Separation process for actinium
JPS5669226A (en) * 1979-11-09 1981-06-10 Agency Of Ind Science & Technol Purification of cadmium
EP0224209A2 (fr) * 1985-11-21 1987-06-03 Sumitomo Chemical Company, Limited Procédé pour la récupération de terres rares
EP0442778A1 (fr) 1990-02-05 1991-08-21 Metaleurop S.A. Procédé d'extraction de thallium
US5296204A (en) * 1990-02-05 1994-03-22 Metaleurop S.A. Thallium extraction process
EP1116326A1 (fr) 1999-07-23 2001-07-18 Koninklijke Philips Electronics N.V. Element conducteur
DE102009018959A1 (de) 2009-04-25 2010-10-28 K-Utec Ag Salt Technologies Methode zur Reduzierung der Thalliumkonzentration in Mineralsalzlösungen
FR2951383A1 (fr) 2009-10-20 2011-04-22 Solvay Procede pour la valorisation conjointe de sels solubles contenus dans un residu d'un procede industriel
WO2011048135A1 (fr) 2009-10-20 2011-04-28 Solvay Sa Procédé pour la régénération combinée de sels solubles contenus dans un résidu d'un procédé industriel

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
MIKROCHIMICA ACTA, vol. 96, no. 1-6, January 1988 (1988-01-01), pages 341 - 347
RILEY J P ET AL: "Chelating resins for the concentration of trace elements from sea water and their analytical use in conjunction with atomic absorption spectrophotometry", ANALYTICA CHIMICA ACTA, ELSEVIER, AMSTERDAM, NL, vol. 40, 1 January 1968 (1968-01-01), pages 479 - 485, XP026730637, ISSN: 0003-2670, [retrieved on 19680101], DOI: DOI:10.1016/S0003-2670(00)86764-1 *
TSISIN, G.I.; MALOFEEVA, G.I.; PETRUKHIN, O.M.; ZOLOTOV, Y.A.: "Vemadsky Institute of Geochemistry and Analytical Chemistry", USSR ACADEMY OF SCIENCES
XIAO: "Environmental impact of thallium related to the mercury-thallium- gold mineralization in southwest Guizhou Province, China", CHICOUTIMI, UNIVERSIT DU QU BEE CHICOUTIMI, 2001

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017127650A1 (fr) * 2016-01-21 2017-07-27 Archer Daniels Midland Company Procédés de récupération de catalyseurs
CN109811128A (zh) * 2019-02-14 2019-05-28 广州大学 一种从冶炼酸性废水回收铊及制备碘化亚铊的方法
CN115432854A (zh) * 2022-09-06 2022-12-06 水口山有色金属有限责任公司 一种高卤素污酸优先富集除铊的方法
CN115652114A (zh) * 2022-12-28 2023-01-31 长沙华时捷环保科技发展股份有限公司 一种含铊溶液中铊的资源化回收工艺

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