JP5291313B2 - Tin recovery method - Google Patents
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Description
本発明は、錫の回収方法に関し、特に、不純物としてアンチモンを含む錫含有塩基性溶液から錫を回収する方法に関する。 The present invention relates to a method for recovering tin, and more particularly to a method for recovering tin from a tin-containing basic solution containing antimony as an impurity.
錫（Ｓｎ）が溶解した苛性ソーダ水溶液のような錫含有塩基性溶液に不純物として数十〜２００ｍｇ／Ｌ程度のアンチモン（Ｓｂ）が溶解していると、その錫含有塩基性溶液を電解液として使用して電解採取を行っても、Ｓｎと共にＳｂも電着するため、純度の高いＳｎを得ることができない。例えば、ＪＩＳ１種で規格されているＳｂ２００ｐｐｍ以下のＳｎを得る場合には、電解液中のＳｎ濃度が５０ｇ／Ｌ程度であれば、電解液中のＳｂ濃度を１０ｍｇ／Ｌ程度、好ましくは５ｍｇ／Ｌ程度まで下げなければならない。 When several tens to 200 mg / L of antimony (Sb) is dissolved as an impurity in a tin-containing basic solution such as a caustic soda solution in which tin (Sn) is dissolved, the tin-containing basic solution is used as an electrolyte. Even if electrolytic collection is carried out, Sb is electrodeposited together with Sn, so that high purity Sn cannot be obtained. For example, when obtaining Sn of 200 ppm or less of Sb standardized by JIS class 1, if the Sn concentration in the electrolyte is about 50 g / L, the Sb concentration in the electrolyte is about 10 mg / L, preferably 5 mg / L. It must be lowered to about L.
不純物としてＳｂを含む錫含有塩基性溶液を室温で長時間放置すると、Ｓｂが徐々に沈澱して、Ｓｂ濃度が２０ｍｇ／Ｌ程度まで低下する。しかし、その沈澱には長時間を要し、また、電解採取の際に液温を８０℃程度まで上げる必要があるので、錫含有塩基性溶液中のＳｂ濃度を下げるために冷却するのは、エネルギー的にもロスが多い。 When a tin-containing basic solution containing Sb as an impurity is allowed to stand at room temperature for a long time, Sb gradually precipitates and the Sb concentration decreases to about 20 mg / L. However, the precipitation takes a long time, and since it is necessary to raise the liquid temperature to about 80 ° C. during electrowinning, cooling to lower the Sb concentration in the tin-containing basic solution There are many energy losses.
従来、不純物として錫以外の金属を含む錫含有塩基性溶液から錫を回収する方法として、不純物を含む錫含有塩基性溶液に、還元用金属を添加するとともに、再酸化防止剤としてチオ硫酸ナトリウムなどを添加して、液中の不純物を置換還元し、析出した不純物を濾過などによって除去した後に、錫を回収する方法が提案されている（例えば、特許文献１参照）。 Conventionally, as a method for recovering tin from a tin-containing basic solution containing a metal other than tin as an impurity, a reducing metal is added to the tin-containing basic solution containing an impurity, and sodium thiosulfate is used as a reoxidation inhibitor. A method is proposed in which tin is recovered after adding and reducing impurities in the liquid and removing the precipitated impurities by filtration or the like (see, for example, Patent Document 1).
しかし、特許文献１の方法では、不純物としてＳｂを含む錫含有塩基性溶液に、還元用金属を添加するとともに、再酸化防止剤としてチオ硫酸ナトリウムなどを添加しても、錫含有塩基性溶液中のＳｂ濃度を短時間で十分に低下させることができない場合がある。 However, in the method of Patent Document 1, even if a reducing metal is added to a tin-containing basic solution containing Sb as an impurity and sodium thiosulfate or the like is added as a reoxidation inhibitor, In some cases, the Sb concentration cannot be sufficiently reduced in a short time.
したがって、本発明は、このような従来の問題点に鑑み、不純物としてＳｂを含む錫含有塩基性溶液中のＳｂ濃度を短時間で十分に低下させて効率的に錫を回収することができる、錫の回収方法を提供することを目的とする。 Therefore, in view of such a conventional problem, the present invention can efficiently recover tin by sufficiently reducing the Sb concentration in a tin-containing basic solution containing Sb as an impurity in a short time. It aims at providing the recovery method of tin.
本発明者らは、上記課題を解決するために鋭意研究した結果、不純物としてＳｂを含む錫含有塩基性溶液に、酸化数（−２）の硫黄を含むイオンが存在する状態で、アルカリ領域においてＳｂより卑な金属を添加し、Ｓｂを沈澱させて除去することによって、不純物としてＳｂを含む錫含有塩基性溶液中のＳｂ濃度を短時間で十分に低下させて効率的に錫を回収することができることを見出し、本発明を完成するに至った。 As a result of diligent research to solve the above problems, the present inventors have found that in an alkaline region, a tin-containing basic solution containing Sb as an impurity contains ions containing sulfur having an oxidation number (-2). By adding a metal lower than Sb and precipitating and removing Sb, the Sb concentration in the tin-containing basic solution containing Sb as an impurity can be sufficiently reduced in a short time to efficiently recover tin. As a result, the present invention has been completed.
すなわち、本発明による錫の回収方法は、不純物としてアンチモンを含む錫含有塩基性溶液に、酸化数（−２）の硫黄を含むイオンが存在する状態で、アルカリ領域においてアンチモンより卑な金属を添加し、アンチモンを沈澱させて除去した後、錫を回収することを特徴とする。 That is, the method for recovering tin according to the present invention adds a base metal more than antimony in an alkaline region in the presence of ions containing sulfur having an oxidation number (−2) in a tin-containing basic solution containing antimony as an impurity. The tin is recovered after the antimony is precipitated and removed.
この錫の回収方法において、酸化数（−２）の硫黄を含むイオンが、硫黄イオン（Ｓ２−）、チオ錫酸イオン（ＳｎＳ３ ２−）およびチオアンチモン酸（ＳｂＳ４ ２−）からなる群から選ばれる一種以上のイオンであるのが好ましい。また、錫含有塩基性溶液に、硫化ナトリウム、硫化錫および硫化アンチモンからなる群から選ばれる一種以上の化合物を添加することにより、酸化数（−２）の硫黄を含むイオンが存在する状態にするのが好ましい。また、錫含有塩基性溶液に、硫化アルカリ、水硫化アルカリ、チオ錫酸アルカリおよび金属硫化物からなる群から選ばれる一種以上の化合物を添加することにより、酸化数（−２）の硫黄を含むイオンが存在する状態にしてもよい。さらに、錫含有塩基性溶液に硫黄を添加することにより、酸化数（−２）の硫黄を含むイオンが存在する状態にしてもよい。 In this method for recovering tin, ions containing sulfur having an oxidation number (−2) are composed of sulfur ions (S 2− ), thiostannate ions (SnS 3 2− ), and thioantimonic acid (SbS 4 2− ). It is preferably one or more ions selected from the group. In addition, by adding one or more compounds selected from the group consisting of sodium sulfide, tin sulfide and antimony sulfide to the tin-containing basic solution, ions containing sulfur having an oxidation number (-2) are present. Is preferred. Further, by adding one or more compounds selected from the group consisting of alkali sulfide, alkali hydrosulfide, alkali thiostannate and metal sulfide to the tin-containing basic solution, sulfur containing an oxidation number (−2) is contained. An ion may be present. Furthermore, you may make it the state in which the ion containing sulfur of oxidation number (-2) exists by adding sulfur to a tin containing basic solution.
また、上記の錫の回収方法において、アルカリ領域においてアンチモンより卑な金属が、錫、亜鉛およびアルミニウムからなる群から選ばれる一種以上の金属であるのが好ましい。また、アンチモンを沈澱させて除去した後、得られた溶液を電解液として使用して電解採取により錫を回収するのが好ましい。さらに、アルカリ領域においてアンチモンより卑な金属を添加する際に、錫含有塩基性溶液の温度を７０℃以上にするのが好ましい。 In the above tin recovery method, it is preferable that the base metal in the alkaline region than antimony is one or more metals selected from the group consisting of tin, zinc and aluminum. Further, after antimony is precipitated and removed, it is preferable to recover tin by electrolytic collection using the obtained solution as an electrolytic solution. Furthermore, it is preferable that the temperature of the tin-containing basic solution is set to 70 ° C. or higher when adding a metal that is lower than antimony in the alkaline region.
本発明によれば、不純物としてＳｂを含む錫含有塩基性溶液中のＳｂ濃度を短時間で十分に低下させて効率的に錫を回収することができる。特に、不純物としてＳｂを含む錫含有塩基性溶液が酸化した場合であっても、溶液中のＳｂ濃度を短時間で十分に低下させて効率的に錫を回収することができる。 According to the present invention, tin can be efficiently recovered by sufficiently reducing the Sb concentration in a tin-containing basic solution containing Sb as an impurity in a short time. In particular, even if a tin-containing basic solution containing Sb as an impurity is oxidized, tin can be efficiently recovered by sufficiently reducing the Sb concentration in the solution in a short time.
本発明による錫の回収方法の実施の形態では、Ｓｎの他に不純物としてＳｂを含む苛性ソーダ水溶液のような錫含有塩基性溶液に、酸化数（−２）の硫黄を含むイオンが存在する状態で、アルカリ領域においてＳｂより卑な金属を添加し、７０℃以上の温度で緩やかに攪拌して置換反応によりＳｂを沈澱させ、濾過によりＳｂを除去した後、得られた溶液を電解液として使用して電解採取によりＳｎを回収する。 In the embodiment of the method for recovering tin according to the present invention, a tin-containing basic solution such as a caustic soda aqueous solution containing Sb as an impurity in addition to Sn contains ions containing sulfur having an oxidation number (-2). In the alkaline region, a metal lower than Sb is added, gently stirred at a temperature of 70 ° C. or more to precipitate Sb by a substitution reaction, Sb is removed by filtration, and the resulting solution is used as an electrolyte. Then, Sn is collected by electrolytic collection.
酸化数（−２）の硫黄を含むイオンとしては、硫黄イオン（Ｓ２−）、チオ錫酸イオン（ＳｎＳ３ ２−）、チオアンチモン酸（ＳｂＳ４ ２−）などが挙げられる。また、酸化数（−２）の硫黄を含むイオンが存在する状態にするために、錫含有塩基性溶液に、硫化アルカリ、水硫化アルカリ、チオ錫酸アルカリおよび金属硫化物からなる群から選ばれる一種以上の化合物を添加することができ、硫化ナトリウム、硫化錫および硫化アンチモンからなる群から選ばれる一種以上の化合物を添加するのが好ましい。 Examples of ions containing sulfur having an oxidation number (-2) include sulfur ions (S 2− ), thiostannate ions (SnS 3 2− ), and thioantimonic acid (SbS 4 2− ). Further, in order to obtain a state in which ions containing sulfur with an oxidation number (-2) are present, the tin-containing basic solution is selected from the group consisting of alkali sulfide, alkali hydrosulfide, alkali thiostannate, and metal sulfide. One or more compounds can be added, and it is preferable to add one or more compounds selected from the group consisting of sodium sulfide, tin sulfide and antimony sulfide.
アルカリ領域においてＳｂより卑な金属としては、Ｓｎ、Ｚｎ、Ａｌなどを使用することができ、粒状、粉状または板状のＳｎを使用するのが好ましい。 Sn, Zn, Al, etc. can be used as the base metal in the alkaline region, and it is preferable to use granular, powdery or plate-like Sn.
なお、濾過によりＳｂを除去した液は、２価のＳｎ（Ｓｎ２＋）が存在すると、電着するＳｎがスポンジ状になるため、電解採取前に液中に酸素を吹き込むなどによって酸化して４価のＳｎ（Ｓｎ４＋）にするのが好ましい。このような処理を電解採取前に行うと、平滑な電着錫を得ることができる。 In addition, when divalent Sn (Sn 2+ ) is present in the liquid from which Sb has been removed by filtration, Sn to be electrodeposited becomes a spongy form, so that it is oxidized by blowing oxygen into the liquid before electrolytic collection, etc. It is preferable to use Sn (Sn 4+ ). If such treatment is performed before electrolytic collection, smooth electrodeposited tin can be obtained.
以下、本発明による錫の回収方法の実施例について詳細に説明する。 Examples of the method for recovering tin according to the present invention will be described in detail below.
［実施例１］
不純物としてＳｂを含む錫含有塩基性溶液として、ＮａＯＨ濃度１００ｇ／Ｌの水溶液に３０ｇ／ＬのＳｎと１００ｍｇ／ＬのＳｂを溶解した水溶液３００ｍＬを用意した。この水溶液に硫化ナトリウム（Ｎａ２Ｓ）１ｇを添加して９０℃に加温した後、粒径１．５ｍｍ程度の９９．９％のＳｎ粒１０ｇを添加して、攪拌羽根で緩やかに攪拌し、経過時間毎の水溶液中のＳｂ濃度を測定した。その結果を図１に示す。
[Example 1]
As a tin-containing basic solution containing Sb as an impurity, 300 mL of an aqueous solution prepared by dissolving 30 g / L Sn and 100 mg / L Sb in an aqueous solution having a NaOH concentration of 100 g / L was prepared. After adding 1 g of sodium sulfide (Na 2 S) to this aqueous solution and heating to 90 ° C., add 10 g of 99.9% Sn particles having a particle size of about 1.5 mm and gently stirring with a stirring blade. The Sb concentration in the aqueous solution for each elapsed time was measured. The result is shown in FIG.
［比較例１〜３］
比較例１では硫化ナトリウムを添加しなかった、比較例２では硫化ナトリウムの代わりに硫酸ナトリウム（Ｎａ２ＳＯ４）３ｇを添加した、比較例３では硫化ナトリウムの代わりにチオ硫酸ナトリウム５水和物（Ｎａ２Ｓ２Ｏ３・５Ｈ２Ｏ）０．６ｇを添加した以外は、実施例１と同様の操作を行い、経過時間毎の水溶液中のＳｂ濃度を測定した。その結果を図１に示す。
[Comparative Examples 1-3]
In Comparative Example 1, sodium sulfide was not added. In Comparative Example 2, 3 g of sodium sulfate (Na 2 SO 4 ) was added instead of sodium sulfide. In Comparative Example 3, sodium thiosulfate pentahydrate was used instead of sodium sulfide. Except for adding 0.6 g of (Na 2 S 2 O 3 .5H 2 O), the same operation as in Example 1 was performed, and the Sb concentration in the aqueous solution at each elapsed time was measured. The result is shown in FIG.
図１に示すように、硫化ナトリウムを添加した実施例１では、約３０分経過後に水溶液中のＳｂ濃度が０ｍｇ／Ｌ程度まで低下しているが、硫化ナトリウムを添加しなかった比較例１や硫酸ナトリウムを添加した比較例２では、１時間以上経過しても水溶液中のＳｂ濃度が５０ｍｇ／Ｌ程度までしか低下することができなかった。この結果から、硫化ナトリウムの代わりに硫酸ナトリウム（硫酸イオンＳＯ４ −）を添加しても、水溶液中のＳｂ濃度を低下させる効果がないのがわかる。また、図１に示すように、硫化ナトリウムの代わりにチオ硫酸ナトリウムを添加した比較例３では、水溶液中のＳｂ濃度が０ｍｇ／Ｌ程度まで低下するまでに１時間程度を要し、実施例１のように短時間でＳｂ濃度を十分に低下させることができないことがわかる。 As shown in FIG. 1, in Example 1 in which sodium sulfide was added, the Sb concentration in the aqueous solution decreased to about 0 mg / L after about 30 minutes, but Comparative Example 1 in which sodium sulfide was not added In Comparative Example 2 in which sodium sulfate was added, the Sb concentration in the aqueous solution could only be reduced to about 50 mg / L even after 1 hour or more had elapsed. From this result, it can be seen that even if sodium sulfate (sulfate ion SO 4 − ) is added instead of sodium sulfide, there is no effect of reducing the Sb concentration in the aqueous solution. Further, as shown in FIG. 1, in Comparative Example 3 in which sodium thiosulfate was added instead of sodium sulfide, it took about 1 hour until the Sb concentration in the aqueous solution decreased to about 0 mg / L. It can be seen that the Sb concentration cannot be sufficiently reduced in a short time.
［実施例２］
不純物としてＳｂを含む錫含有塩基性溶液として、ＮａＯＨ濃度１００ｇ／Ｌの水溶液に１０ｇ／ＬのＳｎを溶解させた後、Ｓｂメタルを溶解させ、溶け残りを濾過により除去した水溶液を用意した。この水溶液に過酸化水素を添加して酸化（３価のＳｂを５価のＳｂに酸化）し、残存する過酸化水素をＳｎで分解し、室温で１０時間放置した後、濾過した。
[Example 2]
As a tin-containing basic solution containing Sb as an impurity, 10 g / L Sn was dissolved in an aqueous solution having a NaOH concentration of 100 g / L, and then an Sb metal was dissolved and an undissolved residue was removed by filtration. Hydrogen peroxide was added to this aqueous solution for oxidation (trivalent Sb was oxidized to pentavalent Sb), and the remaining hydrogen peroxide was decomposed with Sn, allowed to stand at room temperature for 10 hours, and then filtered.
このようにして得られた濾液３００ｍＬに硫化ナトリウム０．５ｇ（Ｓ量換算０．２０５）を添加して８０℃に加温した後、粒径１．５ｍｍ程度の９９．９％のＳｎ粒１０ｇを添加して、攪拌羽で緩やかに攪拌し、経過時間毎の水溶液中のＳｂ濃度を測定した。その結果を図２に示す。 After adding sodium sulfide 0.5g (S amount conversion 0.205) to 300 mL of the filtrate thus obtained and heating to 80 ° C., 10 g of 99.9% Sn particles having a particle diameter of about 1.5 mm are obtained. Was added and stirred gently with a stirring blade, and the Sb concentration in the aqueous solution was measured for each elapsed time. The result is shown in FIG.
［実施例３、４、比較例４、５］
実施例３では硫化ナトリウムの代わりに硫化錫（ＳｎＳ２）０．５８ｇ（Ｓ量換算０．２０４）を添加した、実施例４では硫化ナトリウムの代わりに硫化アンチモン（Ｓｂ２Ｓ５）０．１ｇ（Ｓ量換算０．０４０）を添加した、比較例４では硫化ナトリウムを添加しなかった（Ｓ量換算０）、比較例５では硫化ナトリウムの代わりにチオ硫酸ナトリウム５水和物（Ｎａ２Ｓ２Ｏ３・５Ｈ２Ｏ）１．５９ｇ（Ｓ量換算０．４１０）を添加した以外は、実施例２と同様の操作を行い、経過時間毎の水溶液中のＳｂ濃度を測定した。その結果を図２に示す。
[Examples 3 and 4, Comparative Examples 4 and 5]
In Example 3, 0.58 g of tin sulfide (SnS 2 ) (0.204 conversion in terms of S) was added instead of sodium sulfide, and in Example 4, 0.1 g of antimony sulfide (Sb 2 S 5 ) instead of sodium sulfide. In Comparative Example 4 to which (S amount conversion 0.040) was added, sodium sulfide was not added (S amount conversion 0). In Comparative Example 5, sodium thiosulfate pentahydrate (Na 2 S) was used instead of sodium sulfide. except that the addition of 2 O 3 · 5H 2 O) 1.59g (S amount in terms 0.410), the procedure of example 2 was measured Sb concentration in the aqueous solution for each elapsed time. The result is shown in FIG.
図２に示すように、硫化ナトリウムを添加した実施例２と硫化錫を添加した実施例３では、約３０分経過後に水溶液中のＳｂ濃度が０ｍｇ／Ｌ程度まで低下し、硫化アンチモンを添加した実施例４では、約９０分経過後に水溶液中のＳｂ濃度が０ｍｇ／Ｌ程度まで低下しているが、硫化ナトリウムを添加しなかった比較例４やチオ硫酸ナトリウムを添加した比較例５では、水溶液中のＳｂ濃度を全く低下させることができなかった。この結果から、不純物としてＳｂを含む錫含有塩基性溶液が酸化した場合には、硫化ナトリウムの代わりにチオ硫酸ナトリウムを添加しても、水溶液中のＳｂ濃度を低下させる効果がないのがわかる。 As shown in FIG. 2, in Example 2 in which sodium sulfide was added and Example 3 in which tin sulfide was added, the Sb concentration in the aqueous solution dropped to about 0 mg / L after about 30 minutes, and antimony sulfide was added. In Example 4, the Sb concentration in the aqueous solution decreased to about 0 mg / L after about 90 minutes. In Comparative Example 4 in which sodium sulfide was not added and in Comparative Example 5 in which sodium thiosulfate was added, the aqueous solution The Sb concentration therein could not be reduced at all. From this result, it is understood that when a tin-containing basic solution containing Sb as an impurity is oxidized, even if sodium thiosulfate is added instead of sodium sulfide, there is no effect of reducing the Sb concentration in the aqueous solution.
Claims (8)
The method for recovering tin according to any one of claims 1 to 7, wherein a temperature of the tin-containing basic solution is set to 70 ° C or higher when adding a metal that is lower than antimony in the alkaline region. .
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| KR101272102B1 (en) * | 2011-06-16 | 2013-06-07 | 한국지질자원연구원 | Method for electrolytic dissociating tin from used metal using alkali solution |
| JP2019173134A (en) * | 2018-03-29 | 2019-10-10 | Ｊｘ金属株式会社 | MANUFACTURING METHOD OF Sn |
| CN115404484B (en) * | 2022-09-24 | 2023-06-27 | 宁波金田铜业(集团)股份有限公司 | De-tin agent for tin-plated copper alloy |
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| JPH06145828A (en) * | 1992-11-16 | 1994-05-27 | Mitsui Kinzoku Shigen Kaihatsu Kk | Method for recovering gold and silver |
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