JP7146175B2 - How to collect gold - Google Patents
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- JP7146175B2 JP7146175B2 JP2019028873A JP2019028873A JP7146175B2 JP 7146175 B2 JP7146175 B2 JP 7146175B2 JP 2019028873 A JP2019028873 A JP 2019028873A JP 2019028873 A JP2019028873 A JP 2019028873A JP 7146175 B2 JP7146175 B2 JP 7146175B2
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Description
本発明は、溶媒抽出された金を還元して回収する方法に関する。 The present invention relates to a method for reducing and recovering solvent-extracted gold.
金は工業的には非鉄金属の副産物や廃電子基板などから回収されている。例えば、非鉄金属の副産物として、銅電解精製工程において電解槽内に沈積する銅電解スライムは、銅と共に金、銀、白金族元素などの様々な貴金属を含んでおり、金や白金族元素などの回収の原料として利用されている。これらの銅電解スライムなどから得られる処理滓から金を還元して回収する方法が従来から知られている。 Industrially, gold is recovered from by-products of non-ferrous metals, waste electronic substrates, and the like. For example, as a by-product of non-ferrous metals, the electrolytic copper slime deposited in the electrolytic bath in the copper electrolytic refining process contains various precious metals such as gold, silver, and platinum group elements along with copper. It is used as a raw material for recovery. A method for recovering gold by reducing it from the treated slag obtained from such copper electrolytic slime has been conventionally known.
例えば、特許文献１（特開平１１－３３５７４９号公報）には、銅電解スライム等から得られる金と白金族元素を含む処理滓に、シュウ酸を加えて金の浸出を抑制しつつ、塩酸を加えて白金族元素を浸出させて分離し、この溶解滓を塩素化溶解して金を浸出させ、この金浸出液のｐＨを約０.５～約２に調整して還元剤を加え、金を還元析出させる方法が記載されている。 For example, in Patent Document 1 (Japanese Patent Application Laid-Open No. 11-335749), oxalic acid is added to treatment slag containing gold and platinum group elements obtained from copper electrolytic slime or the like to suppress leaching of gold, while hydrochloric acid is added. In addition, the platinum group elements are leached and separated, the slag is chlorinated and dissolved to leached gold, the pH of the gold leaching solution is adjusted to about 0.5 to about 2, a reducing agent is added, and gold is leached. A method for reductive deposition is described.
また、特許文献２（特開２０１１－１３２５５２号公報）には、ジブチルカルビトール（以下、ＤＢＣと表記する）を用いて溶媒抽出した金イオンを含む溶液に還元剤を加えて金イオンを還元析出する方法において、還元剤としてシュウ酸カリウムを用い、還元時のｐＨを２.５～６.５に調整して金を還元析出させる方法が記載されている。 Further, in Patent Document 2 (Japanese Patent Application Laid-Open No. 2011-132552), a reducing agent is added to a solution containing gold ions that has been solvent-extracted using dibutyl carbitol (hereinafter referred to as DBC) to reduce and precipitate gold ions. In this method, gold is reduced and precipitated by using potassium oxalate as a reducing agent and adjusting the pH at the time of reduction to 2.5 to 6.5.
特許文献１の回収方法では、金の還元速度が遅く、水相に金が滞留する問題がある。また、特許文献２の回収方法では、還元剤としてシュウ酸カリウムを用いているので、高価であり、しかも金還元時のｐＨを２.５～６.５に調整しているので、金の還元率が低いと云う問題がある。また、シュウ酸カリウムは水に対する溶解熱が水酸化ナトリウムよりも高いので、スケールアップした際の取り扱いが難しくなる。 In the recovery method of Patent Document 1, the reduction rate of gold is slow, and there is a problem that gold stays in the aqueous phase. Further, in the recovery method of Patent Document 2, potassium oxalate is used as a reducing agent, which is expensive. There is the problem of low rates. Also, since potassium oxalate has a higher heat of dissolution in water than sodium hydroxide, it becomes difficult to handle when scaled up.
本発明は従来の金回収方法における上記問題を解決した方法を提供する。具体的には、本発明は、ｐＨ調整が容易であって、金の還元率が高く、金を効率よく還元析出することができる金回収方法を提供する。 The present invention provides a method that overcomes the above problems in conventional gold recovery methods. Specifically, the present invention provides a method for recovering gold that facilitates pH adjustment, has a high reduction rate of gold, and is capable of efficiently reducing and depositing gold.
本発明の金回収方法は以下の構成を有する。
〔１〕有機溶媒を用いて抽出した金イオンを含む溶液に還元剤を加えて金を還元析出させる金の回収方法において、水酸化ナトリウムとシュウ酸の混合溶液を還元剤として用い、該混合溶液の水酸化ナトリウムとシュウ酸のモル比（ＮａＯＨ／シュウ酸モル比）が２.１～２.５であって、還元時のｐＨが１０～１３であることを特徴とする金の回収方法。
〔２〕金の還元率が９６％以上であって、還元金に含まれるパラジウムが６ppm未満およびスズが２０ppm以下である上記[１]に記載する金の回収方法。
The gold recovery method of the present invention has the following configuration.
[1] In a method for recovering gold by adding a reducing agent to a solution containing gold ions extracted using an organic solvent to reduce and deposit gold, a mixed solution of sodium hydroxide and oxalic acid is used as a reducing agent, and the mixed solution is A method for recovering gold, wherein the molar ratio of sodium hydroxide to oxalic acid (NaOH/oxalic acid molar ratio) is 2.1 to 2.5, and the pH during reduction is 10 to 13.
[2] The method for recovering gold according to [1] above, wherein the reduction rate of gold is 96% or more, and the reduced gold contains less than 6 ppm of palladium and less than 20 ppm of tin.
〔具体的な説明〕
以下、本発明の金回収方法を具体的に説明する。
本発明の方法は、有機溶媒を用いて抽出した金イオンを含む溶液に還元剤を加えて金を還元析出させる金の回収方法において、水酸化ナトリウムとシュウ酸の混合溶液を還元剤として用い、該混合溶液の水酸化ナトリウムとシュウ酸のモル比（ＮａＯＨ／シュウ酸モル比）が２.１～２.５であって、還元時のｐＨが１０～１３であることを特徴とする金の回収方法である。
[Specific explanation]
The gold recovery method of the present invention will be specifically described below.
The method of the present invention is a gold recovery method in which a reducing agent is added to a solution containing gold ions extracted using an organic solvent to reduce and deposit gold, wherein a mixed solution of sodium hydroxide and oxalic acid is used as a reducing agent, A gold powder characterized in that the mixed solution has a molar ratio of sodium hydroxide to oxalic acid (NaOH/oxalic acid molar ratio) of 2.1 to 2.5 and a pH of 10 to 13 during reduction. collection method.
本発明の方法において、有機溶媒を用いて抽出した金イオンを含む溶液とは、ジブチルカルビトールなどの有機溶媒を用いて抽出した金イオンを含む有機溶媒液である。例えば、銅電解スライムなどの金、銀及び白金族元素含有物を塩酸などで溶解して、金や白金族などを浸出させ、この金や白金等を含む溶液にＤＢＣなど有機溶媒を接触させて金を抽出した有機溶媒液である。このような有機溶媒液には、銅電解スライム等に由来する金、パラジウム、スズなどが塩化物錯体を形成して含まれている。 In the method of the present invention, the solution containing gold ions extracted using an organic solvent is an organic solvent liquid containing gold ions extracted using an organic solvent such as dibutyl carbitol. For example, gold, silver, and platinum group element-containing materials such as copper electrolytic slime are dissolved in hydrochloric acid, etc., gold and platinum group elements are leached out, and the solution containing gold, platinum, etc. is brought into contact with an organic solvent such as DBC. It is an organic solvent liquid in which gold is extracted. Such an organic solvent liquid contains gold, palladium, tin and the like derived from copper electrolytic slime and the like in the form of chloride complexes.
本発明の金回収方法は、金イオンを含む溶液に加える還元剤として、水酸化ナトリウムとシュウ酸のモル比（ＮａＯＨ／シュウ酸モル比）を２.１～２.５に調整したシュウ酸と水酸化ナトリウムの混合溶液を用い、上記金イオンを含む溶液に該混合溶液を混合した金還元時のｐＨを１０～１３にして金の還元を行う。 In the gold recovery method of the present invention, oxalic acid adjusted to a molar ratio of sodium hydroxide and oxalic acid (NaOH/oxalic acid molar ratio) of 2.1 to 2.5 is used as a reducing agent to be added to a solution containing gold ions. Using a mixed solution of sodium hydroxide, gold is reduced at a pH of 10 to 13 at the time of gold reduction by mixing the mixed solution with the solution containing the gold ions.
従来はシュウ酸ナトリウムを用いる方法が知られているが、シュウ酸ナトリウムに代えて、シュウ酸水溶液に水酸化ナトリウムを混合した溶液を用いることによって、金還元時のｐＨを還元率の高い範囲に調整することができ、また薬剤コストを低減することができる。具体的には、シュウ酸水溶液に水酸化ナトリウムを混合した溶液を用いると、溶液のｐＨは主に水酸化ナトリウムによって定まるので、水酸化ナトリウムの濃度を調整することによって、金還元時のｐＨを還元率の高いｐＨ１０～１３の範囲に容易に調整することができる。 Conventionally, a method using sodium oxalate is known, but by using a solution obtained by mixing sodium hydroxide with an aqueous oxalic acid solution instead of sodium oxalate, the pH during gold reduction can be adjusted to a range with a high reduction rate. can be adjusted and drug costs can be reduced. Specifically, when a solution obtained by mixing sodium hydroxide with an aqueous oxalic acid solution is used, the pH of the solution is determined mainly by sodium hydroxide. It can be easily adjusted to a pH range of 10 to 13 with a high reduction rate.
一方、従来使用されているシュウ酸ナトリウム溶液（２％溶液）のｐＨは８.５～９.５であり、ｐＨがこの範囲では金の還元率が９０％程度に止まり、金の還元率を９６％以上に高めるのは難しい。このような従来のシュウ酸ナトリウム溶液に代えて、シュウ酸水溶液に水酸化ナトリウムを混合した溶液を用いることによって、９６％以上の高い還元率で金を析出させることができる。 On the other hand, the pH of the conventionally used sodium oxalate solution (2% solution) is 8.5 to 9.5. It is difficult to raise it above 96%. Gold can be deposited with a high reduction rate of 96% or more by using a solution in which sodium hydroxide is mixed with an aqueous oxalic acid solution instead of such a conventional sodium oxalate solution.
また、シュウ酸水溶液に水酸化ナトリウムを混合した溶液は、シュウ酸ナトリウムよりもｐＨ制御が容易であるので、金の還元速度を高めることができ、さらにシュウ酸ナトリウムに比べてシュウ酸のほうが水に対する溶解度が高いので反応が進みやすい。
シュウ酸は水中で〔H2C2O4 →2H＋＋C2O4
２－〕のようにシュウ酸イオンに分解し、ここに水酸化ナトリウムが混合されると、水素イオンが消費されてシュウ酸の分解反応が進み、シュウ酸イオン(C2O4
２－)が増加するので、金の還元を促すことができる。
In addition, a solution obtained by mixing an oxalic acid aqueous solution with sodium hydroxide is easier to control the pH than sodium oxalate, so the reduction rate of gold can be increased. Because of its high solubility in , the reaction proceeds easily.
Oxalic acid decomposes into oxalic acid ions like [H 2 C 2 O 4 →2H + +C 2 O 4 2- ] in water. Since the acid decomposition reaction proceeds and oxalate ions (C 2 O 4 2− ) increase, the reduction of gold can be promoted.
また、ＤＢＣなどに抽出された金は塩化金酸(HAuCl４)などの形態で含まれている。この塩化金酸(HAuCl４)は、以下の逆抽出反応に示すように、シュウ酸イオン(C2O4 ２－)と反応して塩化金酸(Ｉ)(HAuCl２)を生じる。この塩化金酸(Ｉ)(HAuCl２)は、以下の還元反応に示すように、さらにシュウ酸イオン(C2O4 ２－)と反応して金メタル(Au)に還元される。 In addition, gold extracted from DBC is contained in the form of chloroauric acid (HAuCl 4 ). This chloroauric acid (HAuCl 4 ) reacts with oxalate ions (C 2 O 4 2− ) to produce chloroauric acid (I) (HAuCl 2 ) as shown in the following back extraction reaction. This chloroauric acid (I) (HAuCl 2 ) further reacts with oxalate ions (C 2 O 4 2− ) to be reduced to gold metal (Au) as shown in the following reduction reaction.
この還元反応において、塩酸が減少すれば、塩化金酸(Ｉ)(HAuCl２)が還元される方向に反応が進み、金メタルの析出が増える。そこで、本発明の方法は、ＮａＯＨ／シュウ酸モル比を２.１～２.５にして金還元時のｐＨを従来よりも高く１０～１３の範囲にし、水酸化ナトリウムを増やして塩酸と水酸化ナトリウムとの反応によって塩酸を減らすようにし、還元反応の平衡を崩して金の還元を進める。 In this reduction reaction, if the amount of hydrochloric acid decreases, the reaction progresses in the direction of reduction of chloroauric acid (I) (HAuCl 2 ), and the deposition of gold metal increases. Therefore, in the method of the present invention, the molar ratio of NaOH/oxalic acid is set to 2.1 to 2.5, the pH during the gold reduction is set to a higher value in the range of 10 to 13 than in the conventional method, and the amount of sodium hydroxide is increased to increase the amount of hydrochloric acid and water. By reacting with sodium oxide, hydrochloric acid is reduced, and the equilibrium of the reduction reaction is disturbed to promote reduction of gold.
［逆抽出反応］ HAuCl４＋C2O4
2－＝ HAuCl２＋2Cl－＋2CO２
［還元反応］ 2HAuCl２＋C2O4
2－＝ 2Au＋2Cl－＋2HCl＋2CO２
[Reverse extraction reaction] HAuCl 4 +C 2 O 4 2− = HAuCl 2 +2Cl − +2CO 2
[Reduction reaction] 2HAuCl 2 +C 2 O 4 2− = 2Au+2Cl − +2HCl+2CO 2
上記ＮａＯＨ／シュウ酸モル比が２.１より低いと、該還元剤のｐＨが１０を下回るようになり、還元速度が遅くなるので好ましくない。一方、該還元剤のＮａＯＨ／シュウ酸モル比が２.５より高いと、該還元剤のｐＨが１３を超えるようになり、有機相と水相の分相性が低下する。また、還元析出した金に含まれる不純物濃度が高くなる。具体的には、例えば、還元金の鉛濃度が１０ppmを超え、またＳｎ濃度が１０００ppmを超える場合があるので好ましくない。 If the NaOH/oxalic acid molar ratio is lower than 2.1, the pH of the reducing agent will be lower than 10, and the reduction rate will be slow, which is not preferable. On the other hand, when the NaOH/oxalic acid molar ratio of the reducing agent is higher than 2.5, the pH of the reducing agent exceeds 13 and the phase separation between the organic phase and the aqueous phase is lowered. In addition, the concentration of impurities contained in gold deposited by reduction is increased. Specifically, for example, the lead concentration of the reduced gold may exceed 10 ppm, and the Sn concentration may exceed 1000 ppm, which is not preferable.
還元時の液温は５０～７５℃が好ましい。液温が５０℃未満では反応速度が遅くなり、７５℃を超えると液が揮発しやすくなる。 The liquid temperature during reduction is preferably 50 to 75°C. If the liquid temperature is less than 50°C, the reaction rate becomes slow, and if it exceeds 75°C, the liquid tends to volatilize.
本発明の金回収方法は、還元剤としてシュウ酸と水酸化ナトリウムの混合溶液を用い、そのＮａＯＨ／シュウ酸モル比を２.１～２.５の範囲にして、該還元剤のｐＨを１０～１３に調整することによって、金の還元が促進されるので、金の還元率を大幅に高めることができる。金の還元率を高めることによって、実操業での生産効率を上げることができる。また、本発明の金回収方法によれば、不純物の少ない高純度の金メタルを回収することができる。 In the gold recovery method of the present invention, a mixed solution of oxalic acid and sodium hydroxide is used as a reducing agent, the NaOH/oxalic acid molar ratio is in the range of 2.1 to 2.5, and the pH of the reducing agent is adjusted to 10. Adjusting to ~13 promotes the reduction of gold, so that the rate of gold reduction can be greatly increased. By increasing the reduction rate of gold, production efficiency in actual operation can be increased. Moreover, according to the gold recovery method of the present invention, high-purity gold metal with few impurities can be recovered.
以下、本発明の実施例を示す。
〔実施例１～５、比較例１～７〕
銅電解スライムを塩酸浸出し、この浸出液にＤＢＣを接触させて金、パラジウム、スズを含む有機溶媒液を得た。この有機溶媒液を洗浄して不純物を除去した後、この洗浄した有機溶媒液を１００ml分取して試料にした。この試料を金の還元工程に供した。一方、シュウ酸水溶液１５０mlに所定量の水酸化ナトリウムを加えた混合溶液を還元剤として用いた。シュウ酸の量は、ＤＢＣ中に含まれる金に対して当量分で調製した。
上記試料を７０℃まで加熱した後に、上記還元剤の混合溶液を添加した。添加は１時間で終わるように速度を調整した。添加終了後、３時間加熱攪拌した。反応終了後、有機相、水相、還元金を分離し、それぞれ分析を行った。金属濃度はＩＣＰ－ＡＥＳによって測定した。還元剤のＮａＯＨ／シュウ酸モル比とｐＨに対する金の還元効果（金還元率、金純度、Ｐｄ濃度、Ｓｎ濃度）を表１に示した。なお、還元率は以下の式によって算出した。
Examples of the present invention are shown below.
[Examples 1 to 5, Comparative Examples 1 to 7]
Copper electrolytic slime was leached with hydrochloric acid, and DBC was brought into contact with this leaching solution to obtain an organic solvent solution containing gold, palladium, and tin. After removing impurities by washing the organic solvent liquid, 100 ml of the washed organic solvent liquid was taken as a sample. This sample was subjected to a gold reduction step. On the other hand, a mixed solution obtained by adding a predetermined amount of sodium hydroxide to 150 ml of an aqueous oxalic acid solution was used as a reducing agent. The amount of oxalic acid was prepared in terms of the amount equivalent to the gold contained in the DBC.
After heating the sample to 70° C., the mixed solution of the reducing agent was added. The rate was adjusted so that the addition was completed in 1 hour. After completion of the addition, the mixture was heated and stirred for 3 hours. After completion of the reaction, the organic phase, aqueous phase and reduced gold were separated and analyzed. Metal concentrations were measured by ICP-AES. Table 1 shows the reduction effect of gold (gold reduction rate, gold purity, Pd concentration, Sn concentration) on the NaOH/oxalic acid molar ratio of the reducing agent and pH. In addition, the reduction rate was calculated by the following formula.
還元率(％)＝ Ａ／〔Ａ＋Ｂ＋Ｃ〕×１００
還元率の上記式において、Ａは還元金の物量(ｇ)、Ｂは有機相中の金の物量(ｇ)、Ｃは水相中の金の物量(ｇ)。
Reduction rate (%) = A / [A + B + C] x 100
In the above formula for the reduction rate, A is the quantity (g) of reduced gold, B is the quantity (g) of gold in the organic phase, and C is the quantity (g) of gold in the aqueous phase.
表１に示すように、ＮａＯＨ／シュウ酸モル比が２.１より低いと、金の還元率は９５％以下である（比較例１～５）。なお、比較例５は、還元剤として水酸化ナトリウムを用いずにシュウ酸ナトリウム溶液を用い、その他は実施例１～５と同様にして還元処理を行った。この比較例５の金の還元率は９１％であり、還元率が低い。 As shown in Table 1, when the NaOH/oxalic acid molar ratio is lower than 2.1, the gold reduction rate is 95% or less (Comparative Examples 1-5). In Comparative Example 5, the reducing treatment was carried out in the same manner as in Examples 1 to 5 except that sodium oxalate solution was used as the reducing agent instead of sodium hydroxide. The reduction rate of gold in Comparative Example 5 is 91%, which is low.
還元剤のＮａＯＨ／シュウ酸モル比が２.１～２.５の範囲であって還元時の溶液のｐＨが１０～１３の範囲では、金の還元率が９６％以上、多くは９８％以上であり、不純物濃度も大幅に少ない（実施例１～５）。 When the NaOH/oxalic acid molar ratio of the reducing agent is in the range of 2.1 to 2.5 and the pH of the solution during reduction is in the range of 10 to 13, the reduction rate of gold is 96% or more, often 98% or more. and the impurity concentration is significantly low (Examples 1 to 5).
還元剤のＮａＯＨ／シュウ酸モル比が２.５を超えると、概ね溶液のｐＨが１３を超えるようになり、還元金の含まれる不純物（ＰｄおよびＳｎ）の濃度が高くなる（比較例６、７）。 When the NaOH/oxalic acid molar ratio of the reducing agent exceeds 2.5, the pH of the solution generally exceeds 13, and the concentration of impurities (Pd and Sn) contained in the reduced gold increases (Comparative Example 6, 7).
Claims (2)
2. The method for recovering gold according to claim 1, wherein the reduction rate of gold is 96% or more, and the reduced gold contains less than 6 ppm of palladium and less than 20 ppm of tin.
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| WO1998058089A1 (en) | 1997-06-16 | 1998-12-23 | Mitsubishi Materials Corporation | Method for smelting noble metal |
| JP2001207223A (en) | 2000-01-25 | 2001-07-31 | Sumitomo Metal Mining Co Ltd | Method for recovering valuable metal from copper electrolytic slime |
| JP2005273009A (en) | 2004-02-26 | 2005-10-06 | Mitsubishi Materials Corp | Method for recovering gold and method for producing the same |
| JP2015131989A (en) | 2014-01-10 | 2015-07-23 | アサヒプリテック株式会社 | REDUCTION AND RECOVERY METHOD OF Au FROM ORGANIC PHASE |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998058089A1 (en) | 1997-06-16 | 1998-12-23 | Mitsubishi Materials Corporation | Method for smelting noble metal |
| JP2001207223A (en) | 2000-01-25 | 2001-07-31 | Sumitomo Metal Mining Co Ltd | Method for recovering valuable metal from copper electrolytic slime |
| JP2005273009A (en) | 2004-02-26 | 2005-10-06 | Mitsubishi Materials Corp | Method for recovering gold and method for producing the same |
| JP2015131989A (en) | 2014-01-10 | 2015-07-23 | アサヒプリテック株式会社 | REDUCTION AND RECOVERY METHOD OF Au FROM ORGANIC PHASE |
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