WO2016132629A1 - Procédé d'extraction au solvant et procédé permettant d'empêcher la formation d'impuretés - Google Patents

Procédé d'extraction au solvant et procédé permettant d'empêcher la formation d'impuretés Download PDF

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WO2016132629A1
WO2016132629A1 PCT/JP2015/084423 JP2015084423W WO2016132629A1 WO 2016132629 A1 WO2016132629 A1 WO 2016132629A1 JP 2015084423 W JP2015084423 W JP 2015084423W WO 2016132629 A1 WO2016132629 A1 WO 2016132629A1
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solution
sulfuric acid
scandium
solvent extraction
treatment
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PCT/JP2015/084423
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English (en)
Japanese (ja)
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達也 檜垣
龍馬 山隈
秀昌 永井
小林　宙
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住友金属鉱山株式会社
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Priority to PH12017501508A priority Critical patent/PH12017501508B1/en

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • 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
    • 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
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
    • 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 solvent extraction method, and more particularly, to suppress the generation of clad in a metal solvent extraction process using an extraction starting solution composed of an aqueous metal sulfuric acid solution containing a flocculant and an organic solvent containing an extractant.
  • the present invention relates to a method for extracting a metal solvent.
  • HPAL process hydrometallurgical process in which nickel oxide ore is charged with sulfuric acid in a pressure vessel and heated to a high temperature of about 240 ° C to 260 ° C to separate it into a leachate containing nickel and leach residue. It has become.
  • a neutralizing agent is added to the obtained leachate to separate impurities, and then a sulfiding agent is added to recover nickel as nickel sulfide.
  • the obtained nickel sulfide is processed in an existing nickel smelting process to become electric nickel or a nickel salt compound (see, for example, Patent Document 1).
  • the generated slurry is often subjected to solid-liquid separation into a clarified liquid and a residue using a sedimentation method.
  • a coagulant such as a polymer coagulant is added to promote sedimentation of the residue. Therefore, in the process after the addition of the flocculant, there is a problem that the organic matter derived from the flocculant dissolves in the liquid and increases the TOC (total organic carbon) concentration in the liquid.
  • the third phase clad is generated in addition to the organic phase and the water phase due to the influence of the TOC in the liquid.
  • the generation of clad in the solvent extraction process causes loss of valuable metals caused by the metal component and organic solvent taken into the clad, and increases the cost of chemicals for the organic solvent. Furthermore, it leads to clogging of the equipment piping, and causes operability to deteriorate.
  • the present invention has been proposed in view of the above-described circumstances, and in the solvent extraction of a solution containing a polymer flocculant, the occurrence of cladding during the solvent extraction is efficiently prevented, and the valuable metal to be extracted It aims at providing the solvent extraction method which can suppress the loss of a component, the chemical
  • the present inventors have made extensive studies to solve the above-described problems.
  • an activated carbon treatment in which a solution containing a polymer flocculant is brought into contact with activated carbon, the concentration of TOC derived from the polymer flocculant can be effectively reduced, It has been found that the generation of clad during solvent extraction can be prevented, and the present invention has been completed. That is, the present invention provides the following.
  • a first aspect of the present invention is a solvent extraction method in which a sulfuric acid solution containing a polymer flocculant and an organic extractant are mixed to extract metal ions contained in the aqueous sulfuric acid solution into the organic extractant.
  • activated carbon is brought into contact with the aqueous sulfuric acid solution, and then the aqueous sulfuric acid solution and the organic extractant are mixed.
  • the third invention of the present invention is a solvent extraction method in which a sulfuric acid aqueous solution containing a polymer flocculant and an organic extractant are mixed to extract metal ions contained in the sulfuric acid aqueous solution into the organic extractant.
  • This is a method for preventing clad generation in which activated carbon is brought into contact with the sulfuric acid aqueous solution prior to solvent extraction by mixing the sulfuric acid aqueous solution and the organic extractant.
  • the solvent extraction method according to the present invention is a metal solvent extraction method in which a sulfuric acid aqueous solution containing a polymer flocculant and an organic extractant are mixed, and metal ions contained in the sulfuric acid aqueous solution are extracted into the organic extractant. is there.
  • activated carbon is brought into contact with a sulfuric acid aqueous solution containing metal ions, and then the sulfuric acid aqueous solution and the organic extractant are mixed. That is, it is characterized in that a treatment using activated carbon is performed as a pretreatment on a sulfuric acid aqueous solution which is a target solution for solvent extraction treatment.
  • the TOC concentration (total carbon concentration) in the solution to be subjected to solvent extraction can be reduced, and the generation of clad during solvent extraction can be effectively prevented. And thereby, the loss of the extractant and the recovery loss of the valuable metal extracted by being taken in by the clad can be suppressed.
  • FIG. 1 is a flow diagram of a scandium recovery process for recovering scandium as scandium oxide from a scandium-containing solution (hereinafter also referred to as “scandium-containing solution”) through an ion exchange step and a solvent extraction step.
  • scandium-containing solution a scandium-containing solution
  • the solvent extraction method according to the present invention can be applied, for example, to a process in a solvent extraction step in the process shown in FIG.
  • the present embodiment a specific embodiment of the solvent extraction method according to the present invention (hereinafter referred to as “the present embodiment”) will be described by taking the process shown in FIG. 1 as an example.
  • the process shown in FIG. 1 shows a flow of recovering scandium from a scandium-containing solution through a solvent extraction process, but the metal to be extracted is not limited to scandium, and naturally other metals may be used.
  • Embodiment in Scandium Recovery Process As a scandium-containing solution, nickel oxide ore is leached with sulfuric acid under high temperature and high pressure, and the obtained leachate is subjected to neutralization treatment and sulfidation treatment to obtain a post-sulfurization solution ( Using a sulfuric acid aqueous solution containing scandium as a metal, scandium is recovered from this solution.
  • the scandium recovery process includes a nickel oxide ore hydrometallurgical process S1, an ion exchange process S2, a solvent extraction process S3, and a roasting process S4.
  • a nickel oxide ore hydrometallurgical process S1 an ion exchange process S2, a solvent extraction process S3, and a roasting process S4.
  • each process is demonstrated in order.
  • the nickel oxide ore hydrometallurgy step S1 the nickel oxide ore is subjected to a leaching treatment, and the obtained leachate is subjected to neutralization treatment and sulfidation treatment to obtain a sulfidized solution.
  • the hydrometallurgy step S1 of nickel oxide ore includes a leaching step S11 in which nickel oxide ore is leached with sulfuric acid under high temperature and high pressure to obtain a leaching slurry, and a leachate from the leaching slurry.
  • Leaching step S11 for example, using a high-temperature pressurized container (autoclave) or the like, sulfuric acid is added to the nickel oxide ore slurry and high-pressure steam and high-pressure air are supplied.
  • This is a step of performing a stirring treatment at a temperature to generate a leaching slurry comprising a leaching solution containing nickel or scandium and a leaching residue containing hematite.
  • the nickel oxide ore include so-called laterite ores such as limonite ore and saprolite ore. These nickel oxide ores contain scandium.
  • Solid-liquid separation step S12 the leaching slurry generated in the leaching step S11 is washed in multiple stages to separate the leaching solution containing nickel and scandium from the leaching residue that is hematite.
  • the leaching slurry is mixed with the cleaning liquid, and then subjected to a solid-liquid separation process using a solid-liquid separation device such as a thickener. Specifically, the slurry is first diluted with a cleaning solution and then the leach residue in the slurry is concentrated as a thickener sediment.
  • a polymer flocculant is added to the slurry to promote sedimentation of the leaching residue.
  • the polymer flocculant is not particularly limited, but anionic carboxylic acid-based and sulfonic acid-based materials including acrylic acid, nonionic materials including acrylamide, and dimethylaminoethyl methacrylate are included. Cationic methacrylic acid esters and acrylate esters are used, and are easily available as commercial products.
  • Neutralization process S13 is a process which adjusts pH by adding a neutralizing agent to a leaching solution, and obtains the neutralized starch containing an impurity element, and the liquid after neutralization.
  • valuable metals such as nickel, cobalt, and scandium are included in the post-neutralization solution, and most of impurities including aluminum become neutralized starch.
  • a polymer flocculant or the like is added to the slurry composed of the neutralized starch and the post-neutralized solution to perform solid-liquid separation treatment, and the subsequent treatment in the sulfurization step S14 is performed. Collect the neutralized solution provided.
  • Sulfurization step Sulfurization step S14 is a step of adding a sulfide such as hydrogen sulfide gas to the obtained post-neutralization liquid to obtain nickel sulfide and post-sulfurization liquid.
  • a sulfide such as hydrogen sulfide gas
  • nickel, cobalt, zinc and the like are recovered as sulfides, and scandium and the like remain in the liquid after sulfiding. Therefore, nickel and scandium can be effectively separated by the sulfidation treatment in the nickel oxide ore hydrometallurgical process.
  • the nickel sulfide slurry obtained by the sulfidation process is separated using a sedimentation separator such as a thickener, and the nickel sulfide is separated and recovered from the bottom of the thickener, while the post-sulfurization solution as an aqueous solution component is Collect by overflowing.
  • a polymer flocculant or the like can be added to the slurry to promote the sedimentation of the sulfide.
  • a post-sulfurization solution that is a sulfuric acid acid solution obtained through such a hydrometallurgical step of nickel oxide ore is recovered, and the post-sulfurization solution is recovered.
  • Scandium is recovered by performing an ion exchange treatment and a solvent extraction treatment described later.
  • the post-sulfurization solution (sulfuric acid solution containing scandium) obtained by the hydrometallurgy step S1 of nickel oxide ore is subjected to an ion exchange treatment, whereby impurities such as aluminum and Chromium is removed to concentrate scandium in the solution. Thereby, highly pure scandium can be collect
  • the ion exchange process using chelate resin is mentioned.
  • the ion exchange step S2 shown in FIG. 1 an ion exchange process using a chelate resin is performed. That is, by contacting the obtained post-sulfurized solution with the chelate resin, the scandium in the post-sulfurized solution is adsorbed on the chelate resin to obtain a scandium (Sc) eluent. More specifically, the ion exchange step S2 includes an adsorption step S21 in which the post-sulfurization solution is brought into contact with the chelate resin to adsorb scandium to the chelate resin, and sulfuric acid is brought into contact with the chelate resin to remove aluminum adsorbed on the chelate resin.
  • ion exchange process S2 it is not limited to this.
  • the post-sulfurized solution is brought into contact with the chelate resin to adsorb scandium to the chelate resin.
  • the chelate resin for example, a resin having iminodiacetic acid as a functional group can be used.
  • Aluminum removal step S22 0.1N or less sulfuric acid is brought into contact with the chelate resin adsorbing scandium to remove aluminum adsorbed on the chelate resin.
  • Chromium removal step S24 3N or more sulfuric acid is brought into contact with the chelate resin that has undergone the scandium elution step S23 to remove chromium adsorbed on the chelate resin.
  • the normality of sulfuric acid used in the eluent is less than 3N, it is not preferable because chromium is not properly removed from the chelate resin.
  • the scandium eluent (sulfuric acid aqueous solution containing scandium and a trace amount of impurities) obtained through the treatment in the ion exchange step S2 is brought into contact with the extractant, and impurities contained in a trace amount in the scandium eluate are extracted.
  • a back extract containing impurities is obtained by adding a back extractant to the resulting extract and separating it from scandium.
  • this solvent extraction step S3 an extraction process (solvent extraction) in which a solution (a sulfuric acid solution containing a polymer flocculant) and an organic solvent (an organic extractant) containing an extractant are mixed.
  • a solution a sulfuric acid solution containing a polymer flocculant
  • an organic solvent an organic extractant containing an extractant
  • activated carbon treatment is performed in which the solution is brought into contact with activated carbon.
  • the solvent extraction step S3 is a pretreatment step S31 in which a solution in which scandium is concentrated through the ion exchange step S2 (a sulfuric acid solution containing a polymer flocculant) is brought into contact with activated carbon to perform activated carbon treatment.
  • an extraction step S32 in which the extracted solution is extracted by mixing the solution after the activated carbon treatment and the organic extractant to extract impurities, and an acidic solution is mixed with the organic solvent after the extraction.
  • the scrubbing step S33 in which scandium extracted into the extractant is extracted and separated from the organic solvent to obtain the organic solvent after washing, and the back extraction starter is mixed with the washed organic solvent, and the impurity element is removed from the organic solvent after washing.
  • Pretreatment process activated carbon treatment process
  • the activated carbon treatment is performed by bringing the solution enriched in scandium through the ion exchange step S2 into contact with the activated carbon.
  • the scandium concentrate to be treated is derived from, for example, a solution obtained through the nickel oxide ore hydrometallurgical process S1, and is obtained by the solid-liquid separation process in the hydrometallurgical process S1. Contains the polymer flocculant used. The polymer flocculant is dissolved in the solution, and the TOC concentration in the solution is high based on the organic substance derived from the flocculant.
  • an activated carbon treatment in which activated carbon is brought into contact with a high TOC concentration solution derived from such a polymer flocculant, the carbon component is decomposed in the solution, and the TOC concentration can be effectively reduced. it can.
  • the type of activated carbon is not particularly limited.
  • raw materials such as coconut shells, coal, coke, and pitch are carbonized and activated, and pulverized to obtain a desired shape (average particle diameter, specific surface area, pores). What was prepared in the volume etc.) can be used.
  • coconut shell activated carbon using coconut shell as a raw material can be preferably used.
  • the shape of the activated carbon specifically, the average particle diameter, specific surface area, pore volume, etc. of the activated carbon is not particularly limited.
  • the average particle diameter is about 0.1 to 50 ⁇ m
  • the specific surface area is A BET value of about 300 to 2000 m 2 / g and a pore volume of about 0.1 ml / g or more can be used.
  • the activated carbon treatment method is not particularly limited.
  • activated carbon such as coconut shell activated carbon is packed in a predetermined column, and a solution (sulfuric acid solution containing a polymer flocculant) to be subjected to solvent extraction treatment is passed through the column. It can be performed by letting it liquid. By bringing the solution into contact with activated carbon in this manner, the TOC concentration in the solution can be reduced by a simple operation.
  • Conditions such as the treatment time of the activated carbon treatment are not particularly limited, but are preferably carried out until the TOC concentration in the solution is reduced to 0.04 g / l or less, and are carried out until it is reduced to 0.03 g / l or less. Is more preferable. Thus, it can prevent more effectively that a clad generate
  • extraction step S32 the solution subjected to the activated carbon treatment in contact with the activated carbon in the pretreatment step S31 and the organic solvent (organic extractant) containing the extractant are mixed to perform the extraction treatment. More specifically, a solution containing scandium after activated carbon treatment and an organic solvent containing an extractant are mixed to selectively extract an impurity element other than scandium, and an organic solvent after extraction containing the impurity element; , And the extraction liquid with increased scandium purity.
  • extraction agents are known and are not particularly limited, but are preferably determined appropriately from the viewpoint of selectivity with the metal contained in the extraction target solution.
  • amine-based extraction agents can be used.
  • the amine-based extractant has characteristics such as low selectivity with scandium and no need for a neutralizing agent at the time of extraction.
  • PrimeneJM-T which is a primary amine, secondary amine.
  • An amine-based extractant known under a trade name such as LA-1, a tertiary amine TNOA (Tri-n-octylamine), TIOA (Tri-i-octylamine), or the like can be used.
  • the concentration of the amine-based extractant in the organic solvent is not particularly limited, but in consideration of phase separation during extraction and back-extraction described later, 1 volume % To about 10% by volume or less, and more preferably about 5% by volume.
  • the TOC concentration in the solution is effectively reduced by performing the pretreatment of bringing the solution into contact with activated carbon prior to the solvent extraction treatment.
  • This can prevent generation of clad derived from the TOC even during solvent extraction.
  • an amine-based extractant is used as an extractant in the extraction process, adverse effects due to the generated clad are likely to occur, but it is contained in the extraction residual liquid by performing the pretreatment prior to the extraction process in this way. Loss of a target metal (for example, scandium) to be obtained and an increase in drug cost such as an extractant can be suppressed.
  • a target metal for example, scandium
  • an acidic solution such as a hydrochloric acid solution, a sulfuric acid solution, or a nitric acid solution can be used.
  • a hydrochloric acid solution a concentration range of 2.0 mol / L or more and 9.0 mol / L or less is preferable, and when using a sulfuric acid solution, a concentration range of 3.5 mol / L or more and 9.0 mol / L or less is preferable.
  • a concentration range of 2.0 mol / L or more and 5.0 mol / L or less is preferable.
  • the impurity element is back extracted from the organic solvent from which the impurity element has been extracted.
  • this back-extraction step S34 by mixing water or a low-concentration acid solution as a back-extraction solution (back-extraction starting solution) with an organic solvent, the reaction opposite to the reaction at the time of extraction proceeds and the impurity element Is back-extracted to obtain a back-extracted solution (back extract) containing the impurity element.
  • the back extraction starting solution may be water, but phase separation from the organic phase may be poor. Therefore, it is preferable to use a low-concentration acid solution as the back extraction start solution.
  • a sulfuric acid solution having a concentration of less than about 3.5 mol / L is used.
  • extractant recovered after the back extraction process in the back extraction step S34 can be repeatedly used as the extractant in the solvent extraction process in the extraction step S32.
  • ⁇ Roasting process> In the roasting step S4, scandium is converted into oxalate (scandium oxalate) by using the extraction residual liquid containing scandium obtained through the solvent extraction step S3, and the scandium is converted into scandium by roasting it. to recover.
  • scandium as an oxalate, handling properties such as filterability can be improved, and scandium can be efficiently recovered.
  • the scandium recovery method is not limited to such treatment.
  • the roasting step S4 includes an oxalate oxidation step S41 in which scandium is oxalate precipitate (scandium oxalate), and roasting the obtained scandium oxalate into scandium oxide. And firing step S42.
  • the pH of the solution is preferably 0 or more and 0.5 or less. If the pH is too low, the solubility of scandium oxalate increases and the scandium recovery rate decreases.On the other hand, if the pH is too high, impurities contained in the solution are precipitated and the scandium purity is lowered. Absent. Moreover, it is preferable that the addition amount of an oxalic acid solution is 1.05 times or more and 1.2 times or less of an equivalent required in order to precipitate scandium as an oxalate.
  • the scandium oxalate crystallized in this manner can be recovered by filtration and washing treatment.
  • roasting step S42 scandium oxide is obtained by roasting the crystals of scandium oxalate obtained by the oxidation treatment.
  • the roasting process is a process in which the obtained scandium oxalate crystals are washed with water and dried, followed by roasting. By undergoing this roasting treatment, scandium can be recovered as scandium oxide.
  • the conditions for the roasting treatment are not particularly limited.
  • the baking may be performed in a tubular furnace at about 900 ° C. for about 2 hours.
  • a continuous furnace such as a rotary kiln because drying and roasting can be performed in the same apparatus.
  • Example 1 The nickel oxide ore slurry is charged into an autoclave, and sulfuric acid is added to perform leaching treatment. The resulting leachate is subjected to neutralization treatment and sulfidation treatment to obtain a post-sulfurization solution containing nickel sulfide and scandium. Got. Furthermore, a scandium concentrate was obtained by subjecting the post-sulfurization solution to known ion exchange treatment and concentration treatment.
  • 7.5 ml of an amine extractant (Primene JM-T: 5% by volume, Shellsol A150: 95% by volume) is added to 30 ml of each post-flowing solution and mixed to perform solvent extraction. did.
  • Table 1 shows the evaluation of clad generation after solvent extraction for each sample. In the evaluation, “ ⁇ ” indicates that no cladding was observed, and “ ⁇ ” indicates that a small amount of cladding was observed (in the comparative example described later, the occurrence of cladding was observed). (“X”)).
  • FIG. 2 is a graph which shows the result in Example 1, and is a graph which shows transition of the TOC density
  • FIG. 3 is a photographic diagram showing how clad is generated in Comparative Example 1.

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Abstract

L'invention concerne un procédé d'extraction au solvant dans lequel, lorsqu'une solution contenant un coagulant polymère est soumise à une extraction au solvant, la formation d'impuretés pendant l'extraction au solvant peut être efficacement empêchée pour réduire la perte de constituants métalliques de valeur à extraire et pour éviter que le coût des produits chimiques concernant les solvants organiques n'augmente. Le procédé d'extraction au solvant selon la présente invention comprend le mélange d'une solution d'acide sulfurique contenant un coagulant polymère avec un agent d'extraction organique pour extraire les ions métalliques contenus dans la solution d'acide sulfurique avec l'agent d'extraction organique et est caractérisé en ce que la solution d'acide sulfurique est mise en contact avec du charbon actif avant d'être mélangée avec l'agent d'extraction organique.
PCT/JP2015/084423 2015-02-20 2015-12-08 Procédé d'extraction au solvant et procédé permettant d'empêcher la formation d'impuretés WO2016132629A1 (fr)

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PH12017501508A PH12017501508B1 (en) 2015-02-20 2017-08-18 Solvent extraction method, and method for preventing crud formation

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JP2015031782A JP6032303B2 (ja) 2015-02-20 2015-02-20 溶媒抽出方法、クラッド発生防止方法
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JP2019000834A (ja) * 2017-06-20 2019-01-10 住友金属鉱山株式会社 ニッケル高圧浸出残渣の固液分離方法

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JP7039936B2 (ja) * 2017-11-07 2022-03-23 住友金属鉱山株式会社 ニッケル高圧浸出残渣の固液分離方法
JP7463181B2 (ja) 2020-04-22 2024-04-08 Ｊｘ金属株式会社 レアメタルの回収方法

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JP2000119761A (ja) * 1998-10-16 2000-04-25 Unitika Ltd 飛灰の再資源化方法
JP2003220302A (ja) * 2002-01-31 2003-08-05 Kaigai Uran Shigen Kaihatsu Kk 鉱石の溶解および元素回収方法
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PH12017501508A1 (en) 2018-02-05
PH12017501508B1 (en) 2018-02-05
JP2016153520A (ja) 2016-08-25

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