JPH05247552A - Decopperizing method of lead electrolysis anode slime by wet process treatment - Google Patents
Decopperizing method of lead electrolysis anode slime by wet process treatmentInfo
- Publication number
- JPH05247552A JPH05247552A JP8441392A JP8441392A JPH05247552A JP H05247552 A JPH05247552 A JP H05247552A JP 8441392 A JP8441392 A JP 8441392A JP 8441392 A JP8441392 A JP 8441392A JP H05247552 A JPH05247552 A JP H05247552A
- Authority
- JP
- Japan
- Prior art keywords
- anode slime
- copper
- sulfuric acid
- leaching
- slime
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、鉛電解アノードスライ
ム(以下単に「アノ−ドスライム」という)の湿式処理
による脱銅方法に関するものであり、さらに詳しく述べ
るならば鉛電解工程で産出するアノードスライムから銅
を金、銀、アンチモン、ビスマス及び鉛から分離して回
収する脱銅方法に関するものである。上記した脱銅は従
来乾式法により行われていたが、本発明は湿式法により
これら有価物を回収する方法に関するものである。本発
明が有価物回収の対象とするアノードスライムは、典型
的には、Cu:2〜5%、Au:0.3%〜1.5%、
Ag:10〜17%、Sb:19〜27%、Bi:19
〜29%、Pb:8〜15%(%は固形分に対する重量
%)を含有するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a decopperization method by wet treatment of lead electrolytic anode slime (hereinafter simply referred to as "anod slime"). More specifically, the anode slime produced in the lead electrolytic process is described. From copper, gold, silver, antimony, bismuth, and lead. The above-mentioned decoppering has been conventionally performed by a dry method, but the present invention relates to a method for recovering these valuable substances by a wet method. The anode slime targeted for recovery of valuable materials in the present invention is typically Cu: 2 to 5%, Au: 0.3% to 1.5%,
Ag: 10 to 17%, Sb: 19 to 27%, Bi: 19
.About.29%, Pb: 8 to 15% (% is% by weight based on solid content).
【0002】[0002]
【従来の技術】従来の乾式法では、アノードスライムを
電気炉及び溶殿炉で還元溶解して得られた還元メタルを
灰吹法により酸化してまずSbを揮発除去し、さらに酸
化させてBi及びCuをPbO滓中に濃縮しAu−Ag
合金を得、Bi及びCuをPbO滓から電気炉中で還元
して粗Biを得るなどの一連の乾式処理により有価物を
分離精製している。2. Description of the Related Art In a conventional dry method, a reduced metal obtained by reducing and melting an anode slime in an electric furnace and a melting furnace is oxidized by an ash blowing method to first volatilize and remove Sb, and further oxidize it to obtain Bi and Cu was concentrated in PbO slag and Au-Ag
Valuables are separated and purified by a series of dry treatments such as obtaining an alloy and reducing Bi and Cu from PbO slag in an electric furnace to obtain crude Bi.
【0003】[0003]
【発明が解決しようとする課題】したがって従来の乾式
法では各工程で有価物の精練中の揮発や取扱い中の破壊
による粉塵の発生が避けられない。さらに、各工程にお
ける有価物の分離度が低いために、有価物非分離スライ
ムを前工程へ戻す繰り返し量が多くなり、またこのため
に金銀の停滞日数が長くなるなどの問題もある。したが
って、本発明の目的は上記欠点を改良し、銅を効率的分
離する方法を提供することにある。Therefore, in the conventional dry method, generation of dust due to volatilization during refining of valuables and destruction during handling is inevitable in each step. Further, since the degree of separation of valuables in each process is low, the amount of non-separated valuables slime to be returned to the previous process is increased, which also causes a problem that the number of days of gold and silver stagnation increases. Therefore, it is an object of the present invention to remedy the above drawbacks and to provide a method for the efficient separation of copper.
【0004】[0004]
【課題を解決するための手段】上記目的を達成するため
に本発明者は検討を重ねた結果、少なくとも銅、金、
銀、アンチモン、ビスマス及び鉛を含む鉛電解アノード
スライムを希硫酸もしくは水で処理して、該アノードス
ライムに付着している珪弗酸分を洗浄した後、含銅硫酸
酸性溶液中で空気を吹込みながら浸出処理を行って、該
鉛電解アノードスライム中の銅を浸出するとともに該ア
ノードスライム中に含まれる金、銀、アンチモン、ビス
マス及び鉛から銅を分離する方法、およびこの好ましい
実施態様として、浸出により得られた銅溶液を電解処理
して銅を電解採取するともに、電解採取後液を銅浸出液
の少なくとも一部として使用する鉛電解アノードスライ
ムの湿式処理による脱銅方法の発明を完成した。As a result of repeated studies by the present inventors in order to achieve the above object, at least copper, gold,
A lead electrolytic anode slime containing silver, antimony, bismuth and lead is treated with dilute sulfuric acid or water to wash the silicofluoric acid content adhering to the anode slime, and then blown with air in a copper-containing sulfuric acid acidic solution. A leaching treatment is carried out while leaching to leaching copper in the lead electrolytic anode slime and separating copper from gold, silver, antimony, bismuth and lead contained in the anode slime, and as a preferred embodiment thereof, The copper solution obtained by leaching is electrolyzed to electrolytically extract copper, and the invention of a decoppering method by wet treatment of lead electrolytic anode slime in which the solution after electrowinning is used as at least a part of the copper leaching solution has been completed.
【0005】以下本発明の構成を説明する。鉛電解は珪
弗酸浴中で実施されるために、アノードスライムには珪
弗酸が付着している。このアノードスライムをそのまま
硫酸浸出工程に送ると、アンチモンの一部が溶出するた
めに、アノードスライムを予め洗浄することが必要であ
る。洗浄には希硫酸溶液または水を使用する。ただし、
水洗浄を行うと珪弗酸が加水分解してSiO2 が沈殿す
るので、希硫酸の使用が好ましい。希硫酸溶液の濃度は
特に限定されないが、遊離硫酸濃度が3〜10g/Lの
範囲内にあることが好ましい。なお、洗浄後のアノード
スライムは銅の浸出工程に、また水洗液はPb2+及びH
2 SiF6 を含有しているので、これらを有効利用する
ために鉛電解工程に戻す。The structure of the present invention will be described below. Since lead electrolysis is carried out in a silicofluoric acid bath, silicofluoric acid adheres to the anode slime. If this anode slime is sent to the sulfuric acid leaching step as it is, a part of antimony is eluted, so that it is necessary to wash the anode slime in advance. Use dilute sulfuric acid solution or water for washing. However,
It is preferable to use dilute sulfuric acid because silicofluoric acid is hydrolyzed and SiO 2 is precipitated by washing with water. The concentration of the dilute sulfuric acid solution is not particularly limited, but the free sulfuric acid concentration is preferably in the range of 3 to 10 g / L. The anode slime after cleaning is used in the copper leaching process, and the washing liquid is Pb 2+ and H.
Since it contains 2 SiF 6 , it is returned to the lead electrolysis step in order to effectively use these.
【0006】上述のように珪弗酸洗浄を行った後に硫酸
浸出を行う。アノードスライムを構成するAu,Ag,
Sb,Bi,Cuなどの有価物はほとんどがメタリック
状であるので、アノードスライムを銅イオン含有硫酸溶
液によりリパルプして、液温が典型的には40℃以上、
好ましくは60℃以上の条件下で空気を吹き込みながら
浸出処理することにより、Cuを95%以上の回収率で
効率的に浸出することができる。また、Au,Ag,S
b,Bi,Pbなどの有価物はアノードスライム中に残
存する。Sulfuric acid leaching is performed after the silicofluoric acid cleaning is performed as described above. Au, Ag, which constitutes the anode slime,
Most valuable materials such as Sb, Bi and Cu are metallic, so the anode slime is repulped with a copper ion-containing sulfuric acid solution and the liquid temperature is typically 40 ° C. or higher.
Preferably, Cu can be efficiently leached at a recovery rate of 95% or more by performing leaching treatment while blowing air under conditions of 60 ° C. or higher. Also, Au, Ag, S
Valuable materials such as b, Bi and Pb remain in the anode slime.
【0007】銅イオンはアノードスライム中に含有され
るメタリックアンチモン、メタリックビスマス等を酸化
するために必要である。その含有量は10〜30g/L
であることが好ましい。Copper ions are necessary to oxidize metallic antimony, metallic bismuth, etc. contained in the anode slime. Its content is 10-30g / L
Is preferred.
【0008】空気吹き込み量は、気液反応によるCuの
酸化に必要な溶存酸素量を確保するように定める必要が
ある。その量はほぼ10ppm程度である。実操業にお
いてはパルプ1L当たり毎分0.5L/L/min以
上、より好ましくは2L/L/min以上を指標とする
ことができる。銅浸出液中の遊離硫酸(H2 SO4 )濃
度は30〜60g/Lであることが好ましい。The amount of air blown in must be determined so as to secure the amount of dissolved oxygen required for the oxidation of Cu by the gas-liquid reaction. The amount is about 10 ppm. In actual operation, 0.5 L / L / min or more per 1 L of pulp, and more preferably 2 L / L / min or more can be used as an index. The free sulfuric acid (H 2 SO 4 ) concentration in the copper leachate is preferably 30 to 60 g / L.
【0009】上記浸出液に含有されるCu2+は電解採取
により回収する。Cu2+の電解条件は通常のものであ
る。なお電解浴中のCu2+濃度は一般に0.5〜10g
/Lであり、この場合の電流効率は50〜80%であ
る。Cu 2+ contained in the leachate is recovered by electrowinning. The Cu 2+ electrolysis conditions are conventional. The Cu 2+ concentration in the electrolytic bath is generally 0.5 to 10 g.
/ L, and the current efficiency in this case is 50 to 80%.
【0010】本発明の好ましい実施態様によると、電解
採取により脱銅された銅浸出後液の一部を硫酸浸出工程
に戻すことにより、浸出液中のCu2+濃度を高め、銅浸
出速度を高めることができる。この結果、含銅浸出液の
Cu2+濃度を10g/L〜30g/Lに高め、銅電解採
取することにより電流効率が95%以上と大幅に高めら
れる。According to a preferred embodiment of the present invention, by returning a part of the copper leaching solution decopperized by electrowinning to the sulfuric acid leaching step, the Cu 2+ concentration in the leaching solution is increased and the copper leaching rate is increased. be able to. As a result, by increasing the Cu 2+ concentration of the copper-containing leachate to 10 g / L to 30 g / L and conducting electrolytic extraction of copper, the current efficiency is significantly increased to 95% or more.
【0011】[0011]
【作用】本発明が特徴とする銅イオン存在下での硫酸浸
出液中への空気吹き込みによる銅の浸出作用を下記実験
結果により説明する。珪弗酸洗浄を行ったアノードスラ
イムを下記条件で硫酸溶液によりリパルプし、また硫酸
浸出を行った。リパルプ条件 パルプ量:1L スラリー濃度:200g/L 遊離硫酸濃度: 50g/L浸出条件 空気吹き込み量:2L/min 浸出温度:60℃ 攪拌機:浮選機型エアレーター 攪拌速度:1400rpm 銅イオン濃度:20g/L 上記浸出によるCuとSb浸出率の時間変化を図1に示
す。The action of leaching copper by blowing air into the sulfuric acid leaching solution in the presence of copper ions, which is a feature of the present invention, will be explained by the following experimental results. The anodic slime washed with silicofluoric acid was repulped with a sulfuric acid solution under the following conditions and leached with sulfuric acid. Re- pulp condition Pulp amount: 1 L Slurry concentration: 200 g / L Free sulfuric acid concentration: 50 g / L Leaching condition Air blowing amount: 2 L / min Leaching temperature: 60 ° C Stirrer: Flotation machine aerator Stirring speed: 1400 rpm Copper ion concentration: 20 g / L The time change of Cu and Sb leaching rate by the above leaching is shown in FIG.
【0012】図1に示すように硫酸溶液中で空気を吹き
込みながら浸出を行うことによりSbを溶出させること
なくCuを浸出分離することができる。As shown in FIG. 1, by leaching while blowing air in a sulfuric acid solution, Cu can be leached and separated without eluting Sb.
【0013】アノードスライム中のPb,Sb,Bi,
Cuなどはメタリック状で存在している。Pb,Sb,
BiなどはCuの溶解を妨げるので、Cuイオンにより
一旦酸化を行う。図1において2時間の処理で表れるS
bのピークは、Cuイオンの作用によりSbが浸出液中
でイオン化していることを示す。その後アノードスライ
ムからのCuの浸出が始まり、浸出液のCu濃度が急速
に上昇する。Pb, Sb, Bi in the anode slime,
Cu and the like are present in a metallic form. Pb, Sb,
Since Bi or the like hinders the dissolution of Cu, it is temporarily oxidized by Cu ions. In Fig. 1, S that appears after 2 hours of processing
The peak of b indicates that Sb is ionized in the leachate by the action of Cu ions. After that, the leaching of Cu from the anode slime starts, and the Cu concentration of the leachate rapidly rises.
【0014】図3は各種アノードスライムを遊離H2 S
O4 濃度が100g/L及び50g/Lの硫酸溶液で浸
出した場合のSb浸出率を示すグラフである。浸出条件
は以下のとおりであった。 パルプ量:1L スラリー濃度:200g/L 浸出温度:60℃ 空気吹き込み量:2L/min 攪拌速度:1400rpm 攪拌機:浮選機型エアレーターFIG. 3 shows that various types of anode slime are separated into free H 2 S.
It is a graph which shows the Sb leaching rate at the time of leaching with a sulfuric acid solution whose O 4 concentration is 100 g / L and 50 g / L. The leaching conditions were as follows. Amount of pulp: 1 L Slurry concentration: 200 g / L Leaching temperature: 60 ° C. Air blowing amount: 2 L / min Stirring speed: 1400 rpm Stirrer: Flotation type aerator
【0015】使用したスライムは以下のものである。 (a)元スライム、すなわち鉛電解で得られたままのア
ノードスライム(洗浄をしないで水分を含有した状態で
のSb浸出率を調査する比較例) (b)乾燥スライム(洗浄をしないで乾燥をした場合の
Sb浸出率を調査する比較例) (c)硫酸洗浄スライム(6g/L−H2 SO4 溶液で
アノードスライムを洗浄した本発明の好ましい実施態
様) (d)水洗スライム(水でアノードスライムを洗浄した
本発明の実施態様)The slimes used are as follows: (A) Original slime, that is, anode slime as it is obtained by lead electrolysis (comparative example for investigating Sb leaching rate in a state of containing water without washing) (b) Dry slime (drying without washing Comparative example for investigating the Sb leaching rate in the case of performing) (c) Sulfuric acid washed slime (a preferred embodiment of the present invention in which the anode slime was washed with a 6 g / L-H 2 SO 4 solution) (d) Washed slime (anode with water Embodiment of the present invention in which slime is washed)
【0016】Sb浸出率を示す図3より、予め行う硫酸
洗浄または水洗浄がSbの浸出液中への移行を防止する
のに有効であることが分かる。以下、図2のフローチャ
ートを参照して実施例により本発明を詳しく説明する。It can be seen from FIG. 3 showing the Sb leaching rate that the sulfuric acid cleaning or the water cleaning performed in advance is effective in preventing the transfer of Sb into the leachate. Hereinafter, the present invention will be described in detail with reference to the flowchart of FIG.
【0017】[0017]
【実施例】下記組成のアノードスライムを図2に示すフ
ローチャートにより有価物の回収を行った。また回収に
使用した薬剤は、アノードスライムの重量(水分を含
む)を1kgとして、示す。 アノードスライム組成:Pb:10.0%;Ag:1
2.8%;Au:1.01%;Bi:27.2%;S
b:25.2%;As:0.5%;Cu:3.52%;
T.SiF6 :2.1%[Examples] Valuable materials were recovered from the anode slime having the following composition according to the flowchart shown in FIG. The weight of the anode slime (including water) for the chemicals used for recovery is 1 kg. Anode slime composition: Pb: 10.0%; Ag: 1
2.8%; Au: 1.01%; Bi: 27.2%; S
b: 25.2%; As: 0.5%; Cu: 3.52%;
T. SiF 6 : 2.1%
【0018】アノードスライムを3Lの水で洗浄して
脱珪弗酸処理した。また別の処理ではアノードスライム
を3Lの希硫酸溶液(遊離H2 SO4 濃度:6g/L)
で洗浄した。脱珪弗酸処理後のアノードスライムは
800gとなった。またその組成は下記のとおりであっ
た。The anode slime was washed with 3 L of water and treated with desilicofluoric acid. In another process, the anode slime was diluted with 3 L of a dilute sulfuric acid solution (concentration of free H 2 SO 4 : 6 g / L).
Washed with. The amount of anode slime after the desilicofluoric acid treatment was 800 g. The composition was as follows.
【0019】脱珪弗酸処理後のアノードスライム組
成:Pb:10.5%;Ag:16.0%;Au:1.
26%;Bi:34.0%;Sb:31.5%;As:
0.63%;Cu:4.4%;T.SiF6 :0.05
% 脱珪弗酸処理後の水洗水は容量が3Lであり、組成
は、Pb:5.33g/L;T.SiF6 は6.87g
/Lであった。この水洗水を鉛電解工程に戻した。Anode slime composition after desilicofluoric acid treatment: Pb: 10.5%; Ag: 16.0%; Au: 1.
26%; Bi: 34.0%; Sb: 31.5%; As:
0.63%; Cu: 4.4%; SiF 6 : 0.05
% The washing water after desilicofluoric acid treatment had a volume of 3 L and had a composition of Pb: 5.33 g / L; SiF 6 is 6.87g
Was / L. This washing water was returned to the lead electrolysis step.
【0020】脱珪弗酸処理後のアノードスライムを
電解採取後液4Lにリパルプした。このアノードスライ
ムパルプに空気を6.5L/minの割合で6.5時
間、総量で2.5m3 吹き込んで銅の浸出を行った。得
られた含銅浸出液は、容量が4Lであり、組成が次の
とおりであり、浸出率は98%であった。 含銅浸出液組成:Cu:16.9g/L;As:0.
1g/L;Bi:0.3g/L;Sb:0.1g/L;
遊離H2 SO4 :21.0g/LThe anode slime after the desilicofluoric acid treatment was electrolytically collected and then repulped into 4 L of liquid. Air was blown into this anode slime pulp at a rate of 6.5 L / min for 6.5 hours for a total amount of 2.5 m 3 to leach copper. The obtained copper-containing leachate had a volume of 4 L, a composition as described below, and a leach rate of 98%. Copper-containing leachate composition: Cu: 16.9 g / L; As: 0.
1 g / L; Bi: 0.3 g / L; Sb: 0.1 g / L;
Free H 2 SO 4 : 21.0 g / L
【0021】含銅浸出液を電解採取し、電着銅(1
0)(組成−Cu:99%;その他1%)を34g得
た。この電着銅(10)は銅製錬工程に回して、純銅と
して回収した。一方電解採取工程では副産物として電解
採取後液が4L得られ、この組成は次のとおりであっ
た。また電流効率は99%であった。The copper-containing leachate is electrolyzed and electroplated copper (1
0) (composition-Cu: 99%; other 1%) was obtained. This electrodeposited copper (10) was sent to a copper smelting step and recovered as pure copper. On the other hand, in the electrowinning process, 4 L of liquid after electrowinning was obtained as a by-product, and the composition was as follows. The current efficiency was 99%.
【0022】電解採取後液組成:Cu:8.3g/
L;As:0.1g/L;Bi:0.3g/L;Sb:
0.1g/L;遊離H2 SO4 :50g/LLiquid composition after electrolysis: Cu: 8.3 g /
L; As: 0.1 g / L; Bi: 0.3 g / L; Sb:
0.1 g / L; free H 2 SO 4 : 50 g / L
【0023】[0023]
【発明の効果】本発明は上述したように鉛電解アノード
スライムの銅を事前に湿式で除去することにより、有価
物を高収率で回収処理をすることができる。加えて、含
銅浸出液の電解後液を銅浸出工程に戻すことにより銅の
浸出速度を大幅に高めることができた。As described above, according to the present invention, by removing the copper of the lead electrolytic anode slime in advance by wet method, the valuable material can be recovered in a high yield. In addition, by returning the solution after electrolysis of the copper-containing leaching solution to the copper leaching step, the leaching rate of copper could be significantly increased.
【図1】CuとSbの浸出率を示すグラフである。FIG. 1 is a graph showing the leaching rates of Cu and Sb.
【図2】本発明による鉛電解アノードスライムの処理フ
ローチャートである。FIG. 2 is a processing flowchart of a lead electrolytic anode slime according to the present invention.
【図3】アノードスライム脱銅処理時のSb浸出率を示
すグラフである。FIG. 3 is a graph showing the Sb leaching rate during the anode slime decoppering treatment.
Claims (2)
スマス及び鉛を含む鉛電解アノードスライムを希硫酸も
しくは水で処理して、該アノードスライムに付着してい
る珪弗酸分を洗浄した後、含銅硫酸酸性溶液中で空気を
吹込みながら浸出処理を行って、該鉛電解アノードスラ
イム中の銅を浸出するとともに該アノードスライム中に
含まれる金、銀、アンチモン、ビスマス及び鉛から銅を
分離することを特徴とする鉛電解アノードスライムの湿
式処理による脱銅方法。1. A lead electrolytic anode slime containing at least copper, gold, silver, antimony, bismuth and lead is treated with dilute sulfuric acid or water to wash the silicofluoric acid content adhering to the anode slime, Leaching is performed in a copper-containing sulfuric acid acidic solution while blowing air to leach copper in the lead electrolytic anode slime and separate copper from gold, silver, antimony, bismuth and lead contained in the anode slime. A method for removing copper by wet treatment of lead electrolytic anode slime, which comprises:
理して銅を電解採取するともに、電解採取後液を銅浸出
液の少なくとも一部として使用することを特徴とする請
求項1記載の鉛電解アノードスライムの湿式処理による
脱銅方法。2. The lead according to claim 1, wherein the copper solution obtained by the leaching is electrolyzed to electrolytically extract copper, and the solution after electrowinning is used as at least a part of the copper leaching solution. Copper removal method by wet treatment of electrolytic anode slime.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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JP8441392A JPH05247552A (en) | 1992-03-06 | 1992-03-06 | Decopperizing method of lead electrolysis anode slime by wet process treatment |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP8441392A JPH05247552A (en) | 1992-03-06 | 1992-03-06 | Decopperizing method of lead electrolysis anode slime by wet process treatment |
Publications (1)
Publication Number | Publication Date |
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JPH05247552A true JPH05247552A (en) | 1993-09-24 |
Family
ID=13829904
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JP8441392A Pending JPH05247552A (en) | 1992-03-06 | 1992-03-06 | Decopperizing method of lead electrolysis anode slime by wet process treatment |
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