JP2009242850A - Method for leaching lead slag by sulfuric acid - Google Patents

Method for leaching lead slag by sulfuric acid Download PDF

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JP2009242850A
JP2009242850A JP2008089559A JP2008089559A JP2009242850A JP 2009242850 A JP2009242850 A JP 2009242850A JP 2008089559 A JP2008089559 A JP 2008089559A JP 2008089559 A JP2008089559 A JP 2008089559A JP 2009242850 A JP2009242850 A JP 2009242850A
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lead
copper
sulfuric acid
zinc
leaching
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Hidenori Okamoto
秀則 岡本
Yasukatsu Sasaki
康勝 佐々木
Hidetoshi Sasaoka
英俊 笹岡
Keisuke Yamada
敬祐 山田
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Nippon Mining Holdings Inc
Eneos Corp
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Nippon Mining and Metals Co Ltd
Nippon Mining Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method capable of treating lead in which all are performed using a wet process. <P>SOLUTION: The method for leaching lead slag is a method for removing at least copper and zinc in a lead slag which is a smelting intermediate product of non-iron smelting. The method comprises blowing oxygen-containing gas into a liquid of slurried lead slag to oxidize a copper metal to form CuO, oxidizing Cu<SB>2</SB>O by the oxidative effect of ferric sulfate, and adding sulfuric acid to leach at least zinc and copper in the lead slag. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

本発明は、非鉄製錬、基板や電子部品などリサイクル原料の溶融炉・及び産業廃棄物を溶融処理する乾式炉から発生する乾式煙灰中に含まれているPbを回収する方法に関する。 The present invention relates to a method for recovering Pb contained in dry smoke generated from non-ferrous smelting, melting furnaces for recycled materials such as substrates and electronic components, and dry furnaces for melting industrial waste.

例えば銅の乾式製錬においては、自溶炉などで銅鉱石から製造した硫化銅を主とするカワを、転炉で吹錬することで粗銅を製造する。転炉での空気吹き込みによる吹錬時には、カワ、または冷材に含まれる揮発性金属成分（亜鉛、カト゛ミウム、鉛、錫、ヒ゛スマス、砒素等）が、煙灰すなわちタ゛ストとなって回収される。
これらの煙灰成分の処理方法としては、通常、多量に含まれる亜鉛、カト゛ミウム、砒素等を硫酸で浸出して分離し、鉛と錫を主成分とした浸出残渣を得る。この浸出残渣は「鉛滓（粗鉛滓）」と呼ばれる。なお、その鉛滓には飛散した銅分が多く含まれ、その粗鉛滓の組成(重量％)は、鉛23.5〜12.5％、亜鉛9.11〜3.9％、スズ14.6〜6.42％、銅17.3〜5.92％程度となっている。今回用いた鉛滓においては、鉛17.4%、亜鉛6.43%、錫11.7%、銅10.2%となっている。
こういった鉛滓からPbを回収するため、現在一般的には、鉛滓(主成分:硫酸鉛)を、電気炉で溶融還元を行っている。溶融還元により分離されたメタルをソータ゛処理し、その後、メタルをアノート゛鋳造した後、珪フッ素酸浴中にて電解精製することで、Pbを回収している。
また、特2000-109939（特許文献1）では、こうした鉛滓中の鉛を炭酸鉛にする手法が開示されているが、後工程において、硝酸を用いている。 For example, in the dry smelting of copper, crude copper is produced by blowing in a converter a chiefly made of copper sulfide produced from copper ore in a flash smelting furnace or the like. At the time of blowing by air blowing in the converter, volatile metal components (zinc, cadmium, lead, tin, bismuth, arsenic, etc.) contained in the river or cold material are collected as smoke ash, ie, dust.
As a method for treating these smoke ash components, zinc, cadmium, arsenic and the like contained in large amounts are usually leached with sulfuric acid and separated to obtain a leaching residue mainly composed of lead and tin. This leach residue is called “lead lead (crude lead)”. In addition, the lead iron contains a lot of scattered copper, and the composition (weight%) of the crude lead iron is 23.5 to 12.5% lead, 9.11 to 3.9% zinc, 14.6 to 6.42% tin, 17.3 to 5.92 copper %. The lead iron used this time is 17.4% lead, 6.43% zinc, 11.7% tin, and 10.2% copper.
In order to recover Pb from such lead soot, generally lead soot (main component: lead sulfate) is smelted and reduced in an electric furnace. Pb is recovered by subjecting the metal separated by smelting to a sorter, and then subjecting the metal to an anodic casting, followed by electrolytic purification in a silicofluoric acid bath.
Japanese Patent Application Laid-Open No. 2000-109939 (Patent Document 1) discloses a technique for converting lead in such a lead cage into lead carbonate, but nitric acid is used in a subsequent process.

上記の、現在一般的に行われている方法では、前処理工程が乾式法であり、排カ゛ス処理設備を設置する必要性がある。また、乾式回収工程によると、鉛滓中の揮発しやすい成分（鉛、亜鉛、カト゛ミウム、錫、ヒ゛スマス）が再びタ゛ストによって飛散し、このタ゛ストは、残留銅分を回収する目的で銅製錬の炉へと再び送入されることから、前述の揮発しやすい、鉛・亜鉛・カト゛ミウム・錫・ヒ゛スマスの混入により、粗銅の品質低下や、系内への、銅に対する不純物の蓄積をもたらす、という問題が生じている。
一方、さらに後工程の、鉛の電解精製では、珪フッ素酸を用いていることから、排水にフッ素を処理する設備を必要とする。
特許文献1では、炭酸化した鉛滓から鉛を溶かし出すために硝酸を使用しているため、後工程での取り扱いが好ましく行われない。
特開２０００−１０９９３９ 鉛滓からの鉛、錫、ヒ゛スマスの分離方法 出願人：日鉱金属株式会社 In the method generally used at present, the pretreatment process is a dry method, and it is necessary to install an exhaust gas treatment facility. Also, according to the dry recovery process, components that easily volatilize (lead, zinc, cadmium, tin, and mass) in the lead metal are scattered again by the dust, and this dust is used in the copper smelting furnace to recover the residual copper. The problem is that the above-mentioned volatilization of lead, zinc, cadmium, tin, and mass causes the deterioration of the quality of crude copper and the accumulation of impurities with respect to copper in the system. Has occurred.
On the other hand, the lead electrolytic refining, which is a later process, uses silicofluoric acid, and therefore requires equipment for treating fluorine in the waste water.
In Patent Document 1, since nitric acid is used to dissolve lead from the carbonated lead soot, handling in a subsequent process is not preferably performed.
JP, 2000-109939, A Method for Separating Lead, Tin, and Mass from Lead Iron Applicant: Nikko Metal Co., Ltd.

従来の技術に対して、鉛滓から鉛を効率よく回収するために、鉛に対する不純物として多く含まれる銅および亜鉛を、タ゛ストとして飛散させない湿式法により、効率よく鉛と分離させる処理方法が要望されている。 Compared to conventional technology, in order to efficiently recover lead from lead iron, there is a demand for a processing method that efficiently separates copper and zinc, which are abundant as impurities in lead, from lead as a dust by a wet method. ing.

本発明者等は、上記の課題を解決するため以下の発明を成した。
（１）非鉄製錬、基板や電子部品などリサイクル原料の溶融炉、及び産業廃棄物を溶融処理する乾式炉より発生する煙灰から産出する鉛滓中の、銅・亜鉛を除去する方法において、
鉛滓をスラリー化した液中に酸素含有カ゛スを吹き込み、銅メタルを酸化し、CuOとし、
硫酸第2鉄の酸化作用によりCu2Oを酸化し、
硫酸を添加することにより前記鉛滓中の亜鉛と銅を少なくとも浸出処理することを特徴とする、鉛滓の浸出方法。
（２）上記（1）記載の方法に於いて、鉛滓スラリーに、遊離硫酸濃度100〜200g/L、硫酸第2鉄濃度35〜60g/Lとなるように、硫酸及び硫酸第2鉄を入れて、酸素含有カ゛スを吹き込み、銅および亜鉛の浸出率を、それぞれ80%以上にすることを特徴とする、鉛滓の浸出方法 The present inventors made the following invention in order to solve the above-mentioned problems.
(1) In a method for removing copper and zinc in lead iron produced from smoke ash generated from non-ferrous smelting, melting furnaces for recycled materials such as substrates and electronic components, and dry furnaces for melting industrial waste,
Oxygen-containing gas is blown into the slurry containing lead soot to oxidize copper metal to CuO,
Oxidation of ferric sulfate oxidizes Cu 2 O,
A method for leaching lead soot, wherein at least zinc and copper in the lead soot are leached by adding sulfuric acid.
(2) In the method described in (1) above, sulfuric acid and ferric sulfate are added to the lead bran slurry so that the free sulfuric acid concentration is 100 to 200 g / L and the ferric sulfate concentration is 35 to 60 g / L. And leaching oxygen-containing gas so that the leaching rate of copper and zinc is 80% or more respectively.

本発明により、従来の技術に対して、
（１）硫酸第2鉄と空気の酸化力を利用し、硫酸浸出で銅分・亜鉛分を浸出液中に容易に溶かすことができる。
（２）CuおよびZnの浸出率は、それぞれ、90%、88.6%以上とすることができる。
（３）硫酸及び、硫酸第2鉄を添加することで、酸性にし、酸化度を上げ、鉛回収において障壁となる銅と亜鉛の除去条件を売ることができた。
（４）鉛滓から鉛を効率よく回収するために、多く含まれる銅および亜鉛を、湿式法により効率よく取り出せる処理方法の一部分を実現する条件を、見出すことができた。 According to the present invention, over the prior art,
(1) Utilizing the oxidizing power of ferric sulfate and air, sulfuric acid leaching can easily dissolve copper and zinc in the leachate.
(2) The leaching rates of Cu and Zn can be 90% and 88.6% or more, respectively.
(3) By adding sulfuric acid and ferric sulfate, it was made acidic, the degree of oxidation was increased, and the removal conditions of copper and zinc that became a barrier in lead recovery could be sold.
(4) In order to efficiently recover lead from lead soot, it was possible to find conditions for realizing a part of the processing method in which a large amount of copper and zinc can be efficiently taken out by a wet method.

以下に本発明をさらに詳細に説明する。
本発明における処理対象物は、鉛滓である。
鉛滓の原料となる転炉タ゛スト中では、銅はCuSO4，Cu2S，Cuメタル，CuO，Cu2Oなど，亜鉛はZnSO4，ZnSなどの形で存在する。これは、カワの主成分である琉化鉱が、転炉において空気酸化されるが、酸化物を経ず直接金属相になり遊離するものもあるということを意味している。さらにこれは、鉛滓を作る弱酸浸出工程でも、完全には液中に溶け出していない。 The present invention is described in further detail below.
The object to be treated in the present invention is lead iron.
In the converter dust which is the raw material of lead iron, copper exists in the form of CuSO 4 , Cu 2 S, Cu metal, CuO, Cu 2 O, etc., and zinc exists in the form of ZnSO 4 , ZnS, etc. This means that the hatching ore, which is the main component of the river, is oxidized in the converter in the air, but there are some that are directly converted into the metal phase and free from the oxide without passing through the oxide. Furthermore, it is not completely dissolved in the liquid even in the weak acid leaching process for producing lead iron.

原料として、本発明で用いている鉛含有物（鉛滓）を、スラリー濃度で100〜250g/Lとなるよう入れ、水、硫酸、硫酸第2鉄を加え、空気を吹き込みながら硫酸浸出処理を行う。当該浸出方法の模式図として、その一例を図2に示す。
なお、以後、硫酸第2鉄（Fe2(SO4)3=399.7）濃度は、それに含有する鉄濃度で示している。例えば、鉄濃度11.17g/Lとは、硫酸第2鉄自体の濃度としては11.17×（Fe2(SO4)3/2Fe=11.17×39.97g/Lに相当する。
ここで、浸出状況は、サンフ゜リンク゛したスラリーを自然ろ過もしくは強制ろ過させ、得られたろ液中の各成分濃度をICP吸光分析法で測定した結果と、全量ろ過後の液量から、液中に浸出した量とした。 As a raw material, the lead-containing material (lead lead) used in the present invention is added so that the slurry concentration is 100 to 250 g / L, water, sulfuric acid, ferric sulfate is added, and sulfuric acid leaching treatment is performed while blowing air. Do. An example of the leaching method is shown in FIG.
Hereinafter, the ferric sulfate (Fe 2 (SO 4 ) 3 = 399.7) concentration is indicated by the concentration of iron contained therein. For example, the iron concentration of 11.17 g / L corresponds to 11.17 × (Fe 2 (SO 4 ) 3 /2Fe=11.17×39.97 g / L as the concentration of ferric sulfate itself.
Here, the leaching state is that the sample slurry is subjected to natural filtration or forced filtration, and the concentration of each component in the obtained filtrate is measured by ICP absorption spectrometry, and the total amount after filtration is leached into the liquid. Was the amount.

鉄濃度35-60g/L，硫酸濃度100-200g/L，空気吹き込み流量を0.25L/min・L以上とし、液温を60-80℃で浸出することが好ましい。上記条件であると、銅、亜鉛の浸出率が、80％以上となるためである。 It is preferable to leach at an iron concentration of 35-60 g / L, sulfuric acid concentration of 100-200 g / L, an air blowing flow rate of 0.25 L / min · L or more, and a liquid temperature of 60-80 ° C. This is because the leaching rate of copper and zinc is 80% or more under the above conditions.

鉛滓からの浸出には硫酸を用いる。CuおよびZnを浸出させる反応式は、以下の通りである。
CuO＋H2SO4→CuSO4＋H2O (式1)
（酸化銅(2価)、酸化亜鉛の硫酸浸出）
ZnO＋ H2SO4→ZnSO4＋H2O (式2)

（鉄(3価)添加による銅の溶解）
Cu2O＋ H2SO4＋Fe2(SO4)3→2CuSO4＋2FeSO4+H2O (式3)

（熱濃硫酸による銅の酸化作用）
Cu＋2H2SO4→CuSO4＋SO2＋2H2O (式4)
また、空気の吹き込みは、Cuメタルを酸化させてCuOにすることを促進し、その後硫酸によって溶解させるためである。 Sulfuric acid is used for leaching from the lead tank. The reaction formula for leaching Cu and Zn is as follows.
CuO + H 2 SO 4 → CuSO 4 + H 2 O (Formula 1)
(Copper oxide (divalent), zinc oxide sulfuric acid leaching)
ZnO + H 2 SO 4 → ZnSO 4 + H 2 O (Formula 2)

(Dissolution of copper by adding iron (trivalent))
Cu 2 O + H 2 SO 4 + Fe 2 (SO 4 ) 3 → 2 CuSO 4 + 2FeSO 4 + H 2 O (Formula 3)

(Oxidation of copper by hot concentrated sulfuric acid)
Cu + 2H 2 SO 4 → CuSO 4 + SO 2 + 2H 2 O (Formula 4)
Also, the blowing of air is to promote the oxidation of Cu metal to CuO and then dissolve with sulfuric acid.

条件設定として、硫酸濃度、硫酸第2鉄濃度、液温によって浸出量を制御することを想定し、ヒ゛ーカー試験では、これらを変化させて、ろ液中の各成分の濃度を測定した。 As the condition setting, it was assumed that the leaching amount was controlled by sulfuric acid concentration, ferric sulfate concentration, and liquid temperature. In the beaker test, these were changed, and the concentration of each component in the filtrate was measured.

空気吹き込み量を0.25L/min・Lに固定して実施した。同じ鉄濃度、同じ温度にて、硫酸濃度を100，150，200g/Lとふって実験を実施し、Cu・Znそれぞれの浸出率を算出した（図3）。硫酸濃度が150g/L程度で、浸出率が最大となる。 The air blowing rate was fixed at 0.25 L / min · L. Experiments were conducted at the same iron concentration and the same temperature with sulfuric acid concentrations of 100, 150, and 200 g / L, and the leaching rates of Cu and Zn were calculated (Fig. 3). The sulfuric acid concentration is about 150g / L, and the leaching rate is maximized.

また、この範囲で、浸出率がすべて80%を超えることが確認された。硫酸濃度を200g/L以上まで大きくしてしまうと、酸化剤としての作用よりも、酸・塩基の作用が強くなってしまい、鉛滓中の各種金属成分が溶解しにくくなる。そのため、硫酸濃度は、200g/Lまでとした。 In this range, it was confirmed that the leaching rate exceeded 80%. If the sulfuric acid concentration is increased to 200 g / L or more, the action of acid and base becomes stronger than the action as an oxidizing agent, and various metal components in the lead bran are difficult to dissolve. Therefore, the sulfuric acid concentration was set to 200 g / L.

硫酸濃度・温度一定で、鉄濃度を変化させ、実施し、Cu・Znそれぞれの浸出率を算出した（図4）。Cu・Znいずれも浸出率80%を超えるには、鉄濃度を35g/L以上にする必要がある。 The experiment was carried out by changing the iron concentration at a constant sulfuric acid concentration and temperature, and the leaching rates of Cu and Zn were calculated (Fig. 4). In order to exceed the leach rate of 80% for both Cu and Zn, the iron concentration needs to be 35 g / L or more.

次のことがわかった。
鉛滓をスラリー濃度で100〜250g/Lとなるよう入れる。硫酸を100〜200g/L（フリー硫酸）、硫酸第2鉄を、鉄濃度換算で35〜60g/L、となるように、硫酸と硫酸第2鉄を入れる。
さらに、浸出液中に空気を0.25L/min・L以上吹き込む。この条件下で、銅と亜鉛の浸出率を、それぞれ80%以上にできる。 I found the following.
Add lead soot to a slurry concentration of 100 to 250 g / L. Sulfuric acid and ferric sulfate are added so that sulfuric acid is 100 to 200 g / L (free sulfuric acid) and ferric sulfate is 35 to 60 g / L in terms of iron concentration.
Furthermore, air is blown into the leachate at a rate of 0.25 L / min · L or more. Under these conditions, the leaching rates of copper and zinc can each be 80% or more.

CuおよびZnの浸出率はそれぞれ、90%、88.6%以上となる。
硫酸および、硫酸第2鉄を添加することで、酸性にし、酸化度を上げ、鉛回収において障壁となる銅と亜鉛の除去条件を得ることができた。
こうして、本発明は、従来の技術に対して、鉛滓から鉛を効率よく回収するために、多く含まれる銅および亜鉛を、湿式法により効率よく取り出せる処理方法の一部分を実現する条件を、見出すことができた。 The leaching rates of Cu and Zn are 90% and 88.6%, respectively.
By adding sulfuric acid and ferric sulfate, it was made acidic, the degree of oxidation was increased, and conditions for removing copper and zinc, which became a barrier in lead recovery, could be obtained.
Thus, the present invention finds a condition for realizing a part of a processing method capable of efficiently removing a large amount of copper and zinc by a wet method in order to efficiently recover lead from the lead slag with respect to the prior art. I was able to.

本発明における、硫酸浸出工程のフロー図である。It is a flowchart of the sulfuric acid leaching process in this invention. 本発明における、硫酸浸出方法の簡略模式図である。It is a simplified schematic diagram of the sulfuric acid leaching method in the present invention. 本発明における、硫酸濃度と浸出率の関係の一例である。It is an example of the relationship between sulfuric acid concentration and leaching rate in the present invention. 本発明における、鉄濃度と浸出率との関係の一例である。It is an example of the relationship between iron concentration and leaching rate in the present invention.

Claims (2)

非鉄製錬、基板や電子部品などリサイクル原料の溶融炉、及び産業廃棄物を溶融処理する乾式炉より発生する煙灰から産出する鉛滓中の、銅・亜鉛を除去する方法において、
鉛滓をスラリー化した液中に酸素含有カ゛スを吹き込み、銅メタルを酸化し、CuOとし、
硫酸第2鉄の酸化作用によりCu2Oを酸化し、
硫酸を添加することにより前記鉛滓中の亜鉛と銅を少なくとも浸出処理することを特徴とする、鉛滓の浸出方法。 In the method of removing copper and zinc in lead smelt produced from smoke ash generated from non-ferrous smelting, melting furnaces of recycled materials such as substrates and electronic parts, and dry furnaces that melt industrial waste,
Oxygen-containing gas is blown into the slurry containing lead soot to oxidize copper metal to CuO,
Oxidation of ferric sulfate oxidizes Cu 2 O,
A method for leaching lead soot, wherein at least zinc and copper in the lead soot are leached by adding sulfuric acid. 請求項1記載の方法に於いて、鉛滓スラリーに、遊離硫酸濃度100〜200g/L、硫酸第2鉄濃度35〜60g/Lとなるように、硫酸及び硫酸第2鉄を入れて、酸素含有カ゛スを吹き込み、銅および亜鉛の浸出率を、それぞれ80%以上にすることを特徴とする、鉛滓の浸出方法。

In the method according to claim 1, sulfuric acid and ferric sulfate are added to the lead soot slurry so that the free sulfuric acid concentration is 100 to 200 g / L and the ferric sulfate concentration is 35 to 60 g / L, and oxygen A lead leaching method is characterized in that the containing gas is blown and the leaching rate of copper and zinc is 80% or more respectively.

JP2008089559A 2008-03-31 2008-03-31 Method for leaching lead slag by sulfuric acid Withdrawn JP2009242850A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012077341A (en) * 2010-09-30 2012-04-19 Jx Nippon Mining & Metals Corp Method for treating lead slag
JP2013237920A (en) * 2012-05-17 2013-11-28 Sumitomo Metal Mining Co Ltd Treatment method of copper smelting flue cinder
CN106086465A (en) * 2016-06-14 2016-11-09 内蒙古兴安铜锌冶炼有限公司 Utilize the method that top blast stove processes zinc leaching residue
WO2022137585A1 (en) 2020-12-23 2022-06-30 三菱マテリアル株式会社 Method for recovering lead from copper smelting dust
CN116144918A (en) * 2022-04-26 2023-05-23 河南永续再生资源有限公司 Process and device for treating regenerated lead refining alkaline residue
WO2024185838A1 (en) * 2023-03-09 2024-09-12 三菱マテリアル株式会社 Lead recovery method

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012077341A (en) * 2010-09-30 2012-04-19 Jx Nippon Mining & Metals Corp Method for treating lead slag
JP2013237920A (en) * 2012-05-17 2013-11-28 Sumitomo Metal Mining Co Ltd Treatment method of copper smelting flue cinder
CN106086465A (en) * 2016-06-14 2016-11-09 内蒙古兴安铜锌冶炼有限公司 Utilize the method that top blast stove processes zinc leaching residue
WO2022137585A1 (en) 2020-12-23 2022-06-30 三菱マテリアル株式会社 Method for recovering lead from copper smelting dust
KR20230057443A (en) 2020-12-23 2023-04-28 미쓰비시 마테리알 가부시키가이샤 Method for recovering lead from copper smelting dust
CN116144918A (en) * 2022-04-26 2023-05-23 河南永续再生资源有限公司 Process and device for treating regenerated lead refining alkaline residue
WO2024185838A1 (en) * 2023-03-09 2024-09-12 三菱マテリアル株式会社 Lead recovery method

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