JP2006083457A - Treatment method for zinc leach residue and the like - Google Patents
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Abstract
Description
本発明は,湿式亜鉛製錬において発生した亜鉛浸出残渣などといった少なくともInまたはSnを含む被処理物からInやSnを分離する方法に関する。 The present invention relates to a method for separating In and Sn from an object to be treated containing at least In or Sn such as zinc leaching residue generated in wet zinc smelting.
湿式亜鉛製錬においては,ZnS主体の亜鉛精鉱を焙焼して酸に可溶なZnOの形態に変え,これを硫酸で浸出し,得られたZnリッチの浸出尾液は電解工程へ供される。一方,硫酸浸出で生じた亜鉛浸出残渣は,SO2を用いた還元加圧浸出法を採用することにより,硫酸浸出だけでは回収できなかったフェライト系のZnやFe,レアメタルなどの有価金属を浸出させて回収している(特許文献1参照)。また,こうして有価金属を浸出回収した後の浸出残渣は,更に銀や鉛の原料として利用される(特許文献2参照)。 In hydro-zinc smelting, zinc concentrate mainly composed of ZnS is roasted into an acid-soluble form of ZnO, which is leached with sulfuric acid, and the resulting Zn-rich leaching tail solution is supplied to the electrolysis process. Is done. On the other hand, zinc leaching residue produced by sulfuric acid leaching uses a reduced pressure leaching method using SO 2 to leach valuable metals such as ferrite-based Zn, Fe, and rare metals that could not be recovered by sulfuric acid leaching alone. And collected (see Patent Document 1). Further, the leaching residue after leaching and recovering valuable metals is further used as a raw material for silver and lead (see Patent Document 2).
しかしながら,亜鉛浸出残渣をSO2で還元加圧浸出して有価金属を浸出回収した場合,残った浸出残渣中にはレアメタルがまだ相当量残されており,中でも付加価値の高いInのロスが大きい。例えば亜鉛浸出残渣をSO2で加圧浸出した場合,ZnやFeの浸出率が95%程度であるのに対して,Inの浸出率は88〜90%程度と低い。 However, when the zinc leaching residue is reduced and leached with SO 2 and valuable metals are leached and recovered, a considerable amount of rare metal is still left in the remaining leaching residue, and the loss of In, which has a high added value, is particularly large. . For example, when zinc leaching residue is pressure leached with SO 2 , the leaching rate of In is as low as 88 to 90% while the leaching rate of Zn or Fe is about 95%.
また優良な亜鉛鉱石の枯渇化により,今後は不純物としてSnを含有した高Sn品位の亜鉛精鉱の処理が必要となることが予想される。亜鉛浸出残渣をSO2で還元加圧浸出した場合,Sn浸出率は10%程度以下に過ぎない。Znその他の有価金属を回収した後の浸出残渣は,次に銀や鉛の精錬工程に送られるが,特にSnは,鉛電解において不純物として製品に混入し易いため,浸出残渣中のSn品位の更なる低減が望まれる。 In addition, due to the depletion of excellent zinc ore, it is expected that it will be necessary to treat high-grade zinc concentrate containing Sn as an impurity in the future. When the zinc leaching residue is reduced pressure leached with SO 2 , the Sn leaching rate is only about 10% or less. The leaching residue after recovering Zn and other valuable metals is then sent to the refining process for silver and lead. In particular, Sn is easily mixed into the product as an impurity in lead electrolysis. Further reduction is desired.
本発明の目的は,湿式亜鉛製錬において発生した亜鉛浸出残渣などといった少なくともInまたはSnを含む被処理物からSnとレアメタル(特にIn)を高い浸出率で浸出回収できる処理方法を提供することにある。 An object of the present invention is to provide a treatment method capable of leaching and recovering Sn and rare metals (particularly In) at a high leaching rate from an object to be treated containing at least In or Sn such as a zinc leaching residue generated in wet zinc smelting. is there.
従来は塩酸や塩化物塩を含む浸出元液は亜鉛製錬工程へCl−が混入すると,設備の腐食やメタル亜鉛の生産性及び品質の低下の原因となるため,使用されていなかった。本発明では,Cl−を含んだ液を亜鉛製錬本工程と切り離した別系統処理することにより解決した。即ち本発明によれば,湿式亜鉛製錬において発生した亜鉛浸出残渣をSO2を用いて還元加圧浸出することにより発生した浸出残渣などといった少なくともInまたはSnを含む被処理物を浸出原料とし,硫酸と塩酸との混合溶液,硫酸に塩化物塩を混合した混合溶液,または硫酸と塩酸に塩化物塩を混合した混合溶液の何れかを浸出元液として,温度60℃以上の条件で浸出処理することを特徴とする,亜鉛浸出残渣等の処理方法が提供される。 Conventional leaching source solution containing hydrochloric acid or chloride salt is Cl to zinc smelting process - when is mixed, it will cause corrosion of metal zinc productivity and decrease in quality of facilities, have not been used. In the present invention, the solution containing Cl − was solved by a separate system treatment separated from the zinc smelting process. That is, according to the present invention, the leaching raw material is an object to be treated containing at least In or Sn, such as a leaching residue generated by reducing pressure leaching of zinc leaching residue generated in wet zinc smelting using SO 2 . Leaching treatment is performed at a temperature of 60 ° C or higher using either a mixed solution of sulfuric acid and hydrochloric acid, a mixed solution of sulfuric acid mixed with chloride salt, or a mixed solution of sulfuric acid and hydrochloric acid mixed with chloride salt as the brewing source solution. A method for treating zinc leaching residue and the like is provided.
前記浸出元液における硫酸濃度は,100g/リットル以上であることが好ましい。また,前記浸出元液において混合された塩化物塩は,例えばNaCl,KClまたはCaClの1種以上である。また,前記浸出元液におけるCl−量は,前記浸出原料に含まれるSnの当量の1倍以上であり,かつ10等量以下であることが好ましい。 The sulfuric acid concentration in the leaching source solution is preferably 100 g / liter or more. Further, the chloride salt mixed in the leaching source liquid is, for example, one or more of NaCl, KCl, or CaCl. In addition, the Cl − amount in the leaching source solution is preferably at least 1 time the equivalent of Sn contained in the leaching raw material and at most 10 equivalents.
前記浸出原料を浸出処理した浸出尾液の一部または全部を,前記浸出元液として再利用することもできる。また,前記浸出原料を浸出処理した浸出尾液を,中和剤によりpH 4〜9に調整した後,沈澱物を回収しても良い。 A part or all of the leaching tail liquid obtained by leaching the leaching raw material can be reused as the leaching source liquid. The leaching tail liquid obtained by leaching the leaching raw material may be adjusted to pH 4-9 with a neutralizing agent, and the precipitate may be recovered.
本発明によれば,湿式亜鉛製錬において発生した亜鉛浸出残渣をSO2を用いて還元加圧浸出することにより発生した浸出残渣などといった少なくともInまたはSnを含む被処理物を浸出原料として,SnとIn等のレアメタルを高い浸出率で回収することが可能となる。これにより,Inロスが減少する。また,浸出残渣中のSn品位を低減することにより,後の銀や鉛の精錬工程における不純物の低減を図ることができるようになる。 According to the present invention, Sn to be treated as a leaching raw material is a material containing at least In or Sn, such as a leaching residue generated by reducing pressure leaching of zinc leaching residue generated in wet zinc smelting using SO 2. And rare metals such as In can be recovered at a high leaching rate. As a result, the In loss is reduced. Further, by reducing the Sn quality in the leaching residue, it becomes possible to reduce impurities in the subsequent silver and lead refining process.
図1に示すように,湿式亜鉛製錬においては,亜鉛精鉱を焙焼して得たZnOを硫酸で浸出し,得られたZnリッチの浸出尾液は電解工程へ供される。一方,硫酸浸出で生じた亜鉛浸出残渣は,更にSO2を用いて還元加圧浸出され,浸出尾液は有価金属の回収工程へ供される。また有価金属を浸出回収した後の浸出残渣は,本発明における浸出原料となる。かような浸出原料は,鉛を主成分とし,Agなども含有するが,その他にInやSnもまだ少なからず含んでおり,そのまま鉛や銀の原料として利用したのでは,Inのロスを生じてしまう。またSn品位が高いと,銀や鉛の精錬工程において不純物として混入し易いため生産性を落すことになる。 As shown in FIG. 1, in wet zinc smelting, ZnO obtained by roasting zinc concentrate is leached with sulfuric acid, and the obtained Zn-rich leaching tail solution is subjected to an electrolysis process. On the other hand, the zinc leaching residue generated by sulfuric acid leaching is further subjected to reduction pressure leaching using SO 2 , and the leaching tail liquid is supplied to a valuable metal recovery step. Further, the leaching residue after leaching and recovering valuable metals becomes the leaching raw material in the present invention. Such a leaching material contains lead as a main component and also contains Ag and the like, but also contains a lot of In and Sn, and if used as it is as a raw material for lead and silver, loss of In occurs. End up. Moreover, when Sn grade is high, since it is easy to mix as an impurity in the refining process of silver or lead, productivity will fall.
そこで本発明では,このようにInやSnをまだ含んでいる浸出原料を,硫酸と塩酸との混合溶液,硫酸に塩化物塩を混合した混合溶液,または硫酸と塩酸に塩化物塩を混合した混合溶液の何れかを浸出元液として,更に浸出処理する。硫酸に塩化物塩を混合する場合,及び硫酸と塩酸に塩化物塩を混合する場合,混合する塩化物塩として,例えばNaCl,KClまたはCaClの1種以上を用いることができる。 Therefore, in the present invention, the leaching raw material that still contains In and Sn is mixed with sulfuric acid and hydrochloric acid, mixed solution of sulfuric acid with chloride salt, or mixed with sulfuric acid and hydrochloric acid with chloride salt. Further leaching is performed using any of the mixed solutions as a brewing source liquid. When a chloride salt is mixed with sulfuric acid, and when a chloride salt is mixed with sulfuric acid and hydrochloric acid, one or more of NaCl, KCl or CaCl can be used as the mixed chloride salt.
ここで,浸出原料を浸出処理する浸出元液にあっては,硫酸濃度が100g/リットル以上であることが好ましい。浸出元液における硫酸濃度が100g/リットル以下の場合,Snが殆ど浸出されないからである。 Here, in the brewing source liquid for leaching the leaching raw material, the sulfuric acid concentration is preferably 100 g / liter or more. This is because when the sulfuric acid concentration in the leaching source solution is 100 g / liter or less, Sn is hardly leached.
また浸出元液には,塩酸由来または塩化物塩由来のCl−が存在することになるが,浸出元液におけるCl−量は,Snを溶解させるのに最低必要な量(1倍当量)以上で,かつ10倍等量以下,好ましくは5倍等量以下が望ましい。Cl−を大量に添加しすぎる銀や鉛精錬用の銀や鉛まで浸出させることになってしまう。 In the leaching source solution, hydrochloric acid-derived or chloride salt-derived Cl − is present, but the amount of Cl − in the leaching source solution is more than the minimum necessary amount (1 equivalent) for dissolving Sn. And 10 times or less, preferably 5 times or less. Cl - becomes possible to leach up to large amounts of silver and lead for silver and lead smelting too much added.
また,かような浸出元液によって前記浸出原料を浸出処理するにあたり,温度は60℃以上とする。60℃以下では,Inの浸出が殆ど進まなくなってしまう。 Further, when the leaching raw material is leached with such a leaching source liquid, the temperature is set to 60 ° C. or higher. Below 60 ° C, In leaching hardly progresses.
こうして浸出処理することにより,前述の浸出原料中に存在していたSnの大部分を浸出させ,Inの殆ど全部を浸出させることが可能となる。そして,このように浸出原料を浸出処理したことによってZn,Feなどと共にSn,In等を含んだ浸出尾液を,中和剤によりpH 4〜9に調整した後,沈澱物を回収することにより,Inなどの有価金属を少ないロスで回収することができるようになる。 By performing the leaching process in this manner, it is possible to leach most of Sn existing in the aforementioned leaching raw material and to leach almost all of In. By leaching the leaching raw material in this way, the leaching tail liquid containing Sn, In, etc., together with Zn, Fe, etc. is adjusted to pH 4-9 with a neutralizing agent, and then the precipitate is recovered. , In and other valuable metals can be recovered with little loss.
また,このように浸出原料を浸出処理した後の浸出尾液は,高い濃度の硫酸およびCl−イオンを含んでおり,その一部または全部を浸出原料を浸出処理するための浸出元液として再利用することもできる。その場合,浸出原料を浸出処理した後の浸出尾液の一部を抜き出して浸出原料を浸出処理するための浸出元液として再利用し,残りは中和剤によりpH 4〜9に調整した後,沈澱物を回収することにより,Inなどの有価金属を回収しても良い。なお中和後の液は,有価金属および重金属が殆ど入っていていないため,廃水処理施設へ送られ処理される。 In addition, the leaching tail liquid after leaching treatment of the leaching raw material contains high concentrations of sulfuric acid and Cl − ions, and a part or all of the leaching tail liquid is reused as a leaching source liquid for leaching the leaching raw material. It can also be used. In that case, a part of the leaching tail liquid after leaching the leaching raw material is extracted and reused as a brewing source liquid for leaching the leaching raw material, and the remainder is adjusted to pH 4-9 with a neutralizing agent. , Valuable metals such as In may be recovered by recovering the precipitate. The neutralized solution contains almost no valuable metals or heavy metals and is sent to a wastewater treatment facility for processing.
一方,浸出原料を浸出処理した後の浸出残渣は,更に銀や鉛の原料として利用される。本発明によれば,このようにInなどの有価金属の回収ロスを低減できることに加え,浸出残渣中のSn品位を低減することにより,後の銀や鉛の精錬工程における不純物処理の負荷軽減を図ることができるようになる。 On the other hand, the leaching residue after leaching treatment of the leaching raw material is further used as a raw material for silver or lead. According to the present invention, in addition to reducing the recovery loss of valuable metals such as In as described above, by reducing the Sn quality in the leaching residue, it is possible to reduce the load of impurity treatment in the subsequent silver and lead refining process. It becomes possible to plan.
なお,以上では湿式亜鉛製錬においてZnOを硫酸浸出して生じた亜鉛浸出残渣を更にSO2で還元加圧浸出した後の浸出残渣を浸出原料とした例を説明したが,本発明では,亜鉛精鉱を酸素とFe3+を用いて直接浸出することにより発生した浸出残渣を浸出原料とすることもできる。また亜鉛精鉱を直接浸出する場合,高圧の酸素と150℃以上の温度で行う加圧浸出法を用いても良い。 In the above, an example in which the leaching residue obtained by further reducing and leaching the zinc leaching residue generated by sulfuric acid leaching of ZnO in wet zinc smelting with SO 2 was described as a leaching raw material. The leaching residue generated by directly leaching the concentrate using oxygen and Fe 3+ can be used as a leaching raw material. When zinc concentrate is leached directly, a pressure leaching method in which high pressure oxygen and a temperature of 150 ° C. or higher are used may be used.
亜鉛精鉱を焙焼したZnOを硫酸浸出して得た亜鉛浸出残渣を更にSO2で加圧浸出して有価金属を浸出回収した後の浸出残渣を浸出原料とした。表1に実施例の浸出原料とした浸出残渣の品位と対鉱石での浸出率を示す。 Zinc leaching residue obtained by leaching ZnO obtained by roasting zinc concentrate by sulfuric acid was further leached under pressure with SO 2 to leach and collect valuable metals, and the leaching residue was used as the leaching raw material. Table 1 shows the quality of the leaching residue used as the leaching raw material in the examples and the leaching rate against ore.
(実施例1)
先ず,この浸出原料(wet状態)386gに濃度500g/リットルの希硫酸1リットルを加え,更にNaCl 29gを添加し,リパルプした。こうして得たスラリーを大気圧下で,温度90℃,2hrの加熱を行った。所定の時期にスラリーの一部を取り出してろ過,洗浄した残渣から浸出率を測定した結果を図2に示す。60,120minを経過した時点におけるSn及びInの浸出率は各々85%と90%,鉱石から換算した総合浸出率は各々86%,99%であった。
Example 1
First, 1 liter of dilute sulfuric acid having a concentration of 500 g / liter was added to 386 g of this leaching raw material (wet state), and 29 g of NaCl was further added, followed by repulping. The slurry thus obtained was heated at 90 ° C. for 2 hours under atmospheric pressure. FIG. 2 shows the results of measuring the leaching rate from a residue obtained by taking out a portion of the slurry at a predetermined time, filtering and washing. The leaching rates of Sn and In after 60 and 120 min passed were 85% and 90%, respectively, and the total leaching rates converted from ore were 86% and 99%, respectively.
(実施例2)
実施例1と同じ浸出原料(wet状態)386gに濃度500g/リットルの希硫酸1リットルを加え,更にNaCl 5gを添加してリパルプした。こうして得たスラリーを大気圧下で,温度90℃,2hrの加熱を行った。所定の時期にスラリーの一部を取り出してろ過,洗浄した残渣から浸出率を測定した結果を図3に示す。60,120minを経過した時点におけるSn及びInの浸出率は各々35%(総合3%),62%(総合96%)であった。
(Example 2)
1 liter of dilute sulfuric acid having a concentration of 500 g / liter was added to 386 g of the same leaching raw material (wet state) as in Example 1, and 5 g of NaCl was further added for repulping. The slurry thus obtained was heated at 90 ° C. for 2 hours under atmospheric pressure. FIG. 3 shows the result of measuring the leaching rate from a residue obtained by removing a portion of the slurry at a predetermined time, filtering and washing. The leaching rates of Sn and In after 60 and 120 min were 35% (total 3%) and 62% (total 96%), respectively.
(比較例)
実施例1と同じ浸出原料(wet状態)386gに濃度500g/リットルの希硫酸1リットルを加えリパルプした。こうして得たスラリーを大気圧下で,温度90℃,2hrの加熱を行った。所定の時期にスラリーの一部を取り出してろ過,洗浄した残渣から浸出率を測定した結果を図4に示す。60,120minを経過した時点におけるSn及びInの浸出率は各々15%(総合20%),35%(総合93%)であった。
(Comparative example)
1 liter of dilute sulfuric acid with a concentration of 500 g / liter was added to 386 g of the same leaching raw material (wet state) as in Example 1 and repulped. The slurry thus obtained was heated at 90 ° C. for 2 hours under atmospheric pressure. FIG. 4 shows the result of measuring the leaching rate from a residue obtained by removing a part of the slurry at a predetermined time, filtering and washing. The leaching rates of Sn and In after 60 and 120 minutes were 15% (20% overall) and 35% (93% overall), respectively.
(実施例3)
実施例1と同じ浸出原料(wet状態)386gに所定濃度の希硫酸1リットルを加え,更にNaCl29g添加してリパルプした。こうして得たスラリーを大気圧下,温度40,60,90℃の各温度でそれぞれ2hr浸出後にろ過,洗浄した残渣から浸出率を測定した。各浸出温度に対する浸出率は図5のようになった。浸出温度40℃ではSnおよびInの浸出率は10%以下であった。
(Example 3)
1 liter of dilute sulfuric acid with a predetermined concentration was added to 386 g of the same leaching raw material (wet state) as in Example 1, and 29 g of NaCl was further added for repulping. The leaching rate was measured from the residue obtained by leaching the slurry thus obtained at a temperature of 40, 60, and 90 ° C. under atmospheric pressure for 2 hours, followed by filtration and washing. The leaching rate with respect to each leaching temperature is as shown in FIG. At a leaching temperature of 40 ° C., the leaching rate of Sn and In was 10% or less.
(実施例4)
実施例1と同じ浸出原料(wet状態)386gに濃度70,100,200,500g/リットルの各希硫酸1リットルをそれぞれ加え,更にNaCl29g添加してリパルプした。こうして得た各スラリーを大気圧下,温度90℃でそれぞれ2hr浸出後にろ過,洗浄した残渣から浸出率を測定した。各硫酸濃度に対する浸出率は図6のようになった。硫酸濃度100g/リットルでのSn及びInの浸出率は各々20%(総合25%),42%(総合94%)であった。浸出原料を浸出処理する浸出元液にあっては,硫酸濃度が100g/リットル以上であることが好ましい。浸出元液における硫酸濃度が100g/リットル未満の場合,Snが殆ど浸出されない。
Example 4
1 liter of each diluted sulfuric acid having a concentration of 70, 100, 200, and 500 g / liter was added to 386 g of the same leaching raw material (wet state) as in Example 1, and 29 g of NaCl was further added for repulping. Each slurry thus obtained was leached for 2 hours at 90 ° C. under atmospheric pressure and then filtered and washed, and the leaching rate was measured. The leaching rate for each sulfuric acid concentration was as shown in FIG. The leaching rates of Sn and In at a sulfuric acid concentration of 100 g / liter were 20% (total 25%) and 42% (total 94%), respectively. In the leaching source liquid for leaching the leaching raw material, the sulfuric acid concentration is preferably 100 g / liter or more. When the sulfuric acid concentration in the leaching source solution is less than 100 g / liter, Sn is hardly leached.
本発明は,湿式亜鉛製錬において発生する亜鉛浸出残渣の処理などに利用される。 The present invention is used for treatment of zinc leaching residue generated in wet zinc smelting.
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Cited By (7)
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WO2006080565A1 (en) * | 2005-01-31 | 2006-08-03 | Dowa Metals & Mining Co., Ltd. | Method for recovering indium |
JP2009155717A (en) * | 2007-12-28 | 2009-07-16 | Dowa Eco-System Co Ltd | Method for recovering indium |
US8992759B1 (en) | 2014-02-20 | 2015-03-31 | Honeywell International Inc. | Metal refining process using mixed electrolyte |
CN105907978A (en) * | 2016-04-20 | 2016-08-31 | 武汉长海高新技术有限公司 | Method of recycling indium from indium-containing smoke dust |
CN109628746A (en) * | 2019-01-03 | 2019-04-16 | 江西铜业技术研究院有限公司 | The extracting method of tin in a kind of silver separating residues |
CN110016547A (en) * | 2019-04-23 | 2019-07-16 | 王柯娜 | A kind of method of comprehensive utilization using sodium jarosite |
CN115896487A (en) * | 2022-11-25 | 2023-04-04 | 沈阳有色金属研究院有限公司 | Method for enriching and extracting indium from tin smelting smoke dust |
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2004
- 2004-09-17 JP JP2004271891A patent/JP2006083457A/en active Pending
Cited By (10)
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WO2006080565A1 (en) * | 2005-01-31 | 2006-08-03 | Dowa Metals & Mining Co., Ltd. | Method for recovering indium |
JP2009155717A (en) * | 2007-12-28 | 2009-07-16 | Dowa Eco-System Co Ltd | Method for recovering indium |
US8992759B1 (en) | 2014-02-20 | 2015-03-31 | Honeywell International Inc. | Metal refining process using mixed electrolyte |
CN105907978A (en) * | 2016-04-20 | 2016-08-31 | 武汉长海高新技术有限公司 | Method of recycling indium from indium-containing smoke dust |
CN105907978B (en) * | 2016-04-20 | 2018-06-29 | 武汉长海高新技术有限公司 | A kind of method of recovery indium in flue dust containing indium |
CN109628746A (en) * | 2019-01-03 | 2019-04-16 | 江西铜业技术研究院有限公司 | The extracting method of tin in a kind of silver separating residues |
CN109628746B (en) * | 2019-01-03 | 2021-02-26 | 江西铜业技术研究院有限公司 | Method for extracting tin from silver separating slag |
CN110016547A (en) * | 2019-04-23 | 2019-07-16 | 王柯娜 | A kind of method of comprehensive utilization using sodium jarosite |
CN110016547B (en) * | 2019-04-23 | 2020-11-13 | 王柯娜 | Comprehensive utilization method of jarosite slag |
CN115896487A (en) * | 2022-11-25 | 2023-04-04 | 沈阳有色金属研究院有限公司 | Method for enriching and extracting indium from tin smelting smoke dust |
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