WO2010023942A1 - タリウム及び硝酸カリウムの回収方法及び回収装置 - Google Patents

タリウム及び硝酸カリウムの回収方法及び回収装置 Download PDF

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Publication number
WO2010023942A1
WO2010023942A1 PCT/JP2009/004216 JP2009004216W WO2010023942A1 WO 2010023942 A1 WO2010023942 A1 WO 2010023942A1 JP 2009004216 W JP2009004216 W JP 2009004216W WO 2010023942 A1 WO2010023942 A1 WO 2010023942A1
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Prior art keywords
thallium
potassium nitrate
aqueous solution
dissolved
recovering
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English (en)
French (fr)
Japanese (ja)
Inventor
小西正芳
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Sumitomo Osaka Cement Co Ltd
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Sumitomo Osaka Cement Co Ltd
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Priority to CN200980129855.1A priority Critical patent/CN102112662B/zh
Priority to KR1020117002509A priority patent/KR101542287B1/ko
Publication of WO2010023942A1 publication Critical patent/WO2010023942A1/ja
Anticipated expiration legal-status Critical
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    • 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
    • C25C1/22—Electrolytic production, recovery or refining of metals by electrolysis of solutions of metals not provided for in groups C25C1/02 - C25C1/20
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
    • B01D61/025—Reverse osmosis; Hyperfiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/147—Microfiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
    • B01D61/422—Electrodialysis
    • B01D61/423—Electrodialysis comprising multiple electrodialysis steps
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
    • C23G5/04—Apparatus
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals

Definitions

  • the present invention relates to a thallium and potassium nitrate recovery method and recovery apparatus, and more particularly, recovers and effectively uses thallium (Tl), which is a rare metal, from thallium-containing potassium nitrate, and recovers and effectively uses potassium nitrate (KNO 3 ).
  • Tl thallium
  • KNO 3 potassium nitrate
  • the present invention relates to a thallium and potassium nitrate recovery method and recovery apparatus suitable for use at the time.
  • a chlorine bypass device is installed to remove volatile components such as chlorine contained in industrial waste.
  • the chlorine bypass dust discharged from this chlorine bypass device contains useful heavy metals such as thallium. Therefore, in order to reuse it as a cement raw material again, these chlorine compounds are removed and useful as thallium and the like. Heavy metals need to be recovered.
  • Patent Document 3 A method in which a metal dissolved in the waste water is precipitated as an oxide by applying a direct current to the waste water, and the metal oxide is separated from the waste water. According to this metal removal method, the metal contained in the wastewater can be efficiently removed, and the metal concentration in the wastewater can be significantly reduced. Therefore, there is an effect that the quality of the waste water can be improved to a state that sufficiently meets the waste water standard.
  • the present invention was made in order to solve the above-mentioned problem, and without using the thallium-containing potassium nitrate as a waste, recovering and effectively using thallium, which is a rare metal contained in the thallium-containing potassium nitrate, It is an object of the present invention to provide a thallium and potassium nitrate recovery method and recovery apparatus that can recover and effectively use potassium nitrate contained in this thallium-containing potassium nitrate.
  • the present invention provides the following thallium and potassium nitrate recovery method and recovery apparatus. That is, the method for recovering thallium and potassium nitrate according to the present invention is a method for recovering thallium and potassium nitrate from thallium-containing potassium nitrate, wherein the thallium-containing potassium nitrate is dissolved in water to form an aqueous solution, and a direct current is passed through the aqueous solution.
  • the thallium dissolved in the aqueous solution is precipitated as metal thallium or thallium oxide, and the thallium recovery step for recovering the metal thallium or thallium oxide and the aqueous solution from which the thallium has been removed are concentrated to dissolve in the aqueous solution.
  • thallium and potassium nitrate recovery method by applying a direct current to an aqueous solution containing thallium-containing potassium nitrate, thallium dissolved in the aqueous solution is precipitated as metal thallium or thallium oxide, and this metal thallium or thallium oxide is recovered. Thereafter, by concentrating the aqueous solution from which the thallium has been removed, potassium nitrate dissolved in the aqueous solution is precipitated as crystals, and the potassium nitrate crystals are recovered. Thereby, thallium and potassium nitrate contained in thallium-containing potassium nitrate can be efficiently recovered, and the recovered thallium and potassium nitrate can be effectively used.
  • thallium dissolved in the aqueous solution as metallic thallium by maintaining the hydrogen ion concentration of the aqueous solution in which the thallium-containing potassium nitrate is dissolved to be less than 7. It is preferable to deposit thallium dissolved in the aqueous solution as thallium oxide by adding potassium halide to the aqueous solution in which the thallium-containing potassium nitrate is dissolved.
  • the concentration is preferably performed using one or more of heating means, reverse osmosis membrane, and electrodialysis.
  • the thallium and potassium nitrate recovery device of the present invention is a device for recovering thallium and potassium nitrate from thallium-containing potassium nitrate, wherein the thallium-containing potassium nitrate is dissolved in water to form an aqueous solution, and a direct current is passed through the aqueous solution.
  • the electrolysis tank for depositing thallium dissolved in the aqueous solution as metal thallium or thallium oxide, the first separation and recovery means for separating and recovering the deposited metal thallium or thallium oxide, and the thallium were removed. It comprises a precipitation means for concentrating the aqueous solution and precipitating potassium nitrate dissolved in the aqueous solution as crystals, and a second separation and recovery means for separating and recovering the potassium nitrate crystals.
  • the thallium-containing potassium nitrate aqueous solution obtained in the dissolution tank is put into an electrolysis tank, and a direct current is passed through the aqueous solution in the electrolysis tank, so that thallium dissolved in the aqueous solution is converted into metal thallium or It is deposited as thallium oxide, and the deposited metal thallium or thallium oxide is separated and recovered by the first separation and recovery means.
  • the aqueous solution from which thallium has been removed is concentrated by a precipitation means, whereby potassium nitrate dissolved in the aqueous solution is precipitated as crystals, and the precipitated potassium nitrate crystals are separated and recovered by a second separation and recovery means.
  • the precipitation means preferably includes any one or more of a heating means, a reverse osmosis membrane, and electrodialysis.
  • thallium-containing potassium nitrate is dissolved in water to form an aqueous solution, and a direct current is applied to the aqueous solution to precipitate thallium dissolved in the aqueous solution as metal thallium or thallium oxide.
  • the thallium and potassium nitrate recovery apparatus of the present invention by dissolving a thallium-containing potassium nitrate in water to form an aqueous solution, and by applying a direct current to the aqueous solution, the thallium dissolved in the aqueous solution is converted into metal thallium or Electrolysis tank for depositing as thallium oxide, first separation and recovery means for separating and recovering this deposited metal thallium or thallium oxide, and concentrating the aqueous solution from which this thallium has been removed, and using potassium nitrate dissolved in this aqueous solution as crystals Since the precipitation means for precipitating and the second separation and recovery means for separating and recovering the potassium nitrate crystals are provided, thallium and potassium nitrate contained in the thallium-containing potassium nitrate can be efficiently recovered with a simple device. Therefore, thallium and potassium nitrate recovered from thallium-containing potassium nitrate can be
  • XRD powder X-ray-diffraction
  • FIG. 1 is a schematic diagram showing a thallium and potassium nitrate recovery device according to an embodiment of the present invention, which is an example of a device for recovering thallium (Tl) and potassium nitrate (KNO 3 ) from thallium-containing potassium nitrate.
  • This thallium and potassium nitrate recovery device is a dissolution tank 1 in which thallium-containing potassium nitrate is dissolved in water to form an aqueous solution, and high-temperature water vapor of 100 ° C. or higher is supplied to the water in order to heat the water in the dissolution tank 1
  • the high-temperature steam supply pipe 2 to be stored, the electrolytic solution 3 for storing the aqueous solution, and applying a direct current to the aqueous solution to precipitate thallium dissolved in the aqueous solution as metal thallium or thallium oxide, and the electrolysis
  • a direct current stabilizing power source 4 for supplying direct current to the aqueous solution in the tank 3, a solid-liquid separator (first separation and recovery means) 5 for separating and recovering metal thallium or thallium oxide deposited from the aqueous solution, and the thallium removed.
  • the solid-liquid separator 5 may be anything as long as it can separate and recover metal thallium or thallium oxide. Examples thereof include a microfiltration device equipped with a microfiltration membrane (MF), a centrifugal separator, and the like.
  • the crystal can 6 may be any means as long as it can precipitate the potassium nitrate dissolved in the aqueous solution by concentrating the aqueous solution from which thallium has been removed, and is therefore a means for concentrating the aqueous solution by heating.
  • the high-temperature steam supply pipe 7 can be replaced with a reverse osmosis membrane or electrodialysis for concentrating the aqueous solution.
  • the solid-liquid separator 8 may be any one that can separate and recover potassium nitrate, and examples thereof include a microfiltration device and a centrifugal separator.
  • thallium and potassium nitrate recovery method of the present invention (hereinafter simply referred to as “recovery method”) will be described with reference to FIG.
  • recovery method of the present embodiment thallium-containing potassium nitrate is dissolved in water to form an aqueous solution, and a direct current is passed through the aqueous solution to precipitate thallium dissolved in the aqueous solution as metal thallium or thallium oxide.
  • Thallium-containing potassium nitrate used in this recovery method is a nitrate containing 0.2 to 3 mass% of thallium in potassium nitrate, and the purity of potassium nitrate is generally 97 to 99.8 mass%.
  • This potassium nitrate contains Na, Pb, Ca, Fe and the like as impurities.
  • the amount of water input is limited as described above is that it is in a range sufficient to effectively precipitate thallium dissolved in the aqueous solution as metal thallium or thallium oxide when a direct current is applied to the aqueous solution. Because. Note that if the amount of water input is less than 2 times the mass of thallium-containing potassium nitrate, depending on the temperature, the entire amount of potassium nitrate may not dissolve, and the viscosity of the resulting aqueous solution increases, leading to the subsequent steps. This is not preferable because it is difficult to pump.
  • Electrolysis of aqueous potassium nitrate containing thallium A potassium nitrate aqueous solution containing thallium is pumped from the dissolution tank 1 to the electrolysis tank 3, and the electrolysis tank 3 is electrolyzed by applying a direct current to the aqueous solution from the DC stabilizing power source 4 and dissolved in this aqueous solution.
  • the thallium is deposited as metal thallium or thallium oxide.
  • an acid such as hydrochloric acid, nitric acid, sulfuric acid or the like is added to the aqueous solution, and the pH (hydrogen ion concentration) of the aqueous solution is less than 7, preferably 4 or more and less than 7.
  • the thallium dissolved in this aqueous solution can be deposited as metallic thallium.
  • potassium halide such as potassium chloride
  • thallium dissolved in the aqueous solution can be precipitated as thallium oxide.
  • thallium dissolved in the aqueous solution can be precipitated in a state of either metal thallium or thallium oxide.
  • Solid-liquid separation of thallium The aqueous solution in which the metal thallium or thallium oxide is precipitated is pumped to a solid-liquid separator (first separation and recovery means) 5, and the precipitated metal thallium or thallium oxide is separated from the aqueous solution and recovered.
  • the purity of the metal thallium recovered here is about 97% by mass, and the purity of thallium oxide is about 97% by mass.
  • Solid-liquid separation of potassium nitrate The aqueous solution in which the potassium nitrate is precipitated is pumped to a solid-liquid separator (second separation / recovery means) 8, and the precipitated potassium nitrate is separated from the aqueous solution and recovered.
  • the purity of the potassium nitrate recovered here is about 97% by mass and contains about 0.05% by mass of metal thallium or thallium oxide.
  • the waste water discharged from the solid-liquid separator 8 is sent to the crystal can 6 and reused, but may be discharged to the outside after performing a predetermined waste water treatment.
  • thallium-containing potassium nitrate is dissolved in water to form an aqueous solution, and a direct current is passed through the aqueous solution, whereby thallium dissolved in the aqueous solution is obtained.
  • the aqueous solution from which the thallium has been removed is concentrated to precipitate and recover potassium nitrate dissolved in the aqueous solution as crystals, so that thallium contained in thallium-containing potassium nitrate and Potassium nitrate can be recovered efficiently by a simple operation individually.
  • thallium and potassium nitrate can be individually recovered from thallium-containing potassium nitrate, and these can be effectively used again.
  • the thallium recovery step and the potassium nitrate recovery step can be performed continuously, the cost and time for recovering thallium and potassium nitrate can be kept low.
  • a dissolution tank 1 for producing a thallium-containing potassium nitrate aqueous solution, a high-temperature steam supply pipe 2, and an electrolysis tank 3 for depositing metal thallium or thallium oxide from the aqueous solution; , DC stabilized power supply 4, solid-liquid separator 5 for separating and recovering metal thallium or thallium oxide, crystal can 6 for precipitating potassium nitrate in aqueous solution as crystals, high-temperature steam supply pipe 7, and potassium nitrate crystals are separated Since it comprises the solid-liquid separator 8 to be recovered, thallium and potassium nitrate contained in the thallium-containing potassium nitrate can be efficiently recovered with a simple device. Therefore, thallium and potassium nitrate recovered from thallium-containing potassium nitrate can be effectively used again. Moreover, since the structure of the apparatus is simple, the cost for recovering thallium and
  • Example 1 1 kg of thallium-containing potassium nitrate containing 7210 mg / kg of thallium was added to 5 kg of water so that the mass ratio of thallium-containing potassium nitrate to water was 1: 5, and stirred to obtain a thallium-containing potassium nitrate aqueous solution.
  • FIG. 2 shows a powder X-ray diffraction (XRD) pattern of the precipitate of Example 1.
  • the aqueous solution from which the metal thallium had been removed was put into the crystal can 6 and heated with high-temperature steam at 100 ° C. for 60 minutes to evaporate water, and concentrated until the volume of this aqueous solution became 1/10. Thereby, brown white fine crystals were precipitated in the aqueous solution.
  • the aqueous solution in which the microcrystals were precipitated was subjected to solid-liquid separation using the solid-liquid separator 8, and the precipitated microcrystals were separated from the aqueous solution and collected.
  • FIG. 3 shows a powder X-ray diffraction (XRD) pattern of the microcrystals of Example 1.
  • XRD powder X-ray diffraction
  • Example 2 1 kg of thallium-containing potassium nitrate containing 7210 mg / kg of thallium was added to 5 kg of water so that the mass ratio of thallium-containing potassium nitrate to water was 1: 5, and stirred to obtain a thallium-containing potassium nitrate aqueous solution.
  • hydrochloric acid was added to this aqueous solution of potassium nitrate containing thallium to maintain the pH of this aqueous solution at 5, and when this aqueous solution was electrolyzed by applying a direct current of 500 mA through a platinum electrode, a silver-colored precipitate was obtained. A product was formed. Next, the precipitate was recovered, and the precipitate was identified by powder X-ray diffraction (XRD), and was confirmed to be metal thallium.
  • XRD powder X-ray diffraction
  • the aqueous solution from which the metal thallium had been removed was put into the crystal can 6 and heated with high-temperature steam at 100 ° C. for 60 minutes to evaporate water, and concentrated until the volume of this aqueous solution became 1/10. Thereby, brown white fine crystals were precipitated in the aqueous solution.
  • the aqueous solution in which the microcrystals were precipitated was subjected to solid-liquid separation using the solid-liquid separator 8, and the precipitated microcrystals were separated from the aqueous solution and collected.
  • the microcrystal was identified by powder X-ray diffraction (XRD), it was confirmed that the crystallite had good crystallinity.
  • XRD powder X-ray diffraction
  • the thallium content in the microcrystals was analyzed by IPC-AES, it was 965 mg / kg, and it was found that the thallium content was about 1/8 of the original thallium-containing potassium nitrate.
  • Example 3 1 kg of thallium-containing potassium nitrate containing 7210 mg / kg of thallium was added to 5 kg of water so that the mass ratio of thallium-containing potassium nitrate to water was 1: 5, and stirred to obtain a thallium-containing potassium nitrate aqueous solution.
  • FIG. 4 shows a powder X-ray diffraction (XRD) pattern of the precipitate of Example 3.
  • the aqueous solution from which thallium oxide had been removed was put into the crystal can 6 and heated with high-temperature steam at 100 ° C. for 60 minutes to evaporate water, and concentrated until the volume of this aqueous solution became 1/10. Thereby, brown white fine crystals were precipitated in the aqueous solution.
  • the aqueous solution in which the microcrystals were precipitated was subjected to solid-liquid separation using the solid-liquid separator 8, and the precipitated microcrystals were separated from the aqueous solution and collected.
  • the microcrystal was identified by powder X-ray diffraction (XRD), it was confirmed that the crystallite had good crystallinity.
  • XRD powder X-ray diffraction
  • the thallium content in the microcrystals was analyzed by IPC-AES, it was 755 mg / kg, and it was found that the thallium content was about 1/10 compared to the original thallium-containing potassium nitrate.
  • FIG. 5 is a diagram showing a change in the concentration of thallium according to the energization amount (C / L).
  • A indicates electrolysis only by energization, and since electrolysis only by energization was performed without any particular action, the pH changed to acid over time, and thallium in the aqueous solution was inversely proportional to the energization amount. The concentration is decreasing.
  • B shows electrolysis when potassium hydroxide is added during energization to maintain the pH at a weak alkali. Like A, the thallium concentration in the aqueous solution decreases in inverse proportion to the energization amount.
  • C shows electrolysis when potassium chloride is added at the time of energization, no precipitation on the electrode is observed, and precipitation of brown tantalum oxide is observed.
  • the aqueous solution is inversely proportional to the energization amount.
  • the thallium concentration in the inside is decreasing.
  • the thallium concentration in the aqueous solution decreases with increasing energization amount (C / L) in both cases of energization only, potassium hydroxide addition, and potassium chloride addition.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
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  • Inorganic Chemistry (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrolytic Production Of Metals (AREA)
PCT/JP2009/004216 2008-08-29 2009-08-28 タリウム及び硝酸カリウムの回収方法及び回収装置 Ceased WO2010023942A1 (ja)

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CN200980129855.1A CN102112662B (zh) 2008-08-29 2009-08-28 铊及硝酸钾的回收方法以及回收装置
KR1020117002509A KR101542287B1 (ko) 2008-08-29 2009-08-28 탈륨 및 질산칼륨의 회수방법 및 회수장치

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CN105217659B (zh) * 2015-10-28 2017-01-11 天脊煤化工集团股份有限公司 一种生产硝酸钾的方法及其系统
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JPS5693887A (en) * 1979-12-27 1981-07-29 Nippon Mining Co Ltd Pecovery of tallium from lead electrolyte

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JP3508554B2 (ja) 1998-07-02 2004-03-22 三菱マテリアル株式会社 高純度ヨウ化タリウムの製造方法および球状高純度ヨウ化タリウム
JP4446426B2 (ja) 2003-01-30 2010-04-07 株式会社タクマ タリウム含有液処理方法と処理設備
FI115537B (fi) * 2003-03-14 2005-05-31 Outokumpu Oy Menetelmä talliumin poistamiseksi sinkkipitoisesta liuoksesta
CN1317205C (zh) * 2005-05-30 2007-05-23 广州大学 含铊废水的处理方法

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Publication number Priority date Publication date Assignee Title
JPS5693887A (en) * 1979-12-27 1981-07-29 Nippon Mining Co Ltd Pecovery of tallium from lead electrolyte

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JP2010053416A (ja) 2010-03-11
KR101542287B1 (ko) 2015-08-06
JP5293005B2 (ja) 2013-09-18
CN102112662B (zh) 2013-02-13
KR20110044859A (ko) 2011-05-02

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