JP2007092124A - Method for treating copper converter dust - Google Patents
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- JP2007092124A JP2007092124A JP2005283318A JP2005283318A JP2007092124A JP 2007092124 A JP2007092124 A JP 2007092124A JP 2005283318 A JP2005283318 A JP 2005283318A JP 2005283318 A JP2005283318 A JP 2005283318A JP 2007092124 A JP2007092124 A JP 2007092124A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/02—Working-up flue dust
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/045—Leaching using electrochemical processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
Description
本発明は、銅転炉ダストの処理方法に関するものであり、より詳しく述べるならば、効率的に銅、砒素とカドミウムを分離する方法に関するものである。 The present invention relates to a method for treating copper converter dust, and more particularly to a method for efficiently separating copper, arsenic and cadmium.
銅製錬工程の鉱石を溶解する溶錬工程の後工程である転炉工程(PS-転炉やMI-C炉、フラッシュコンバーターなど)で排ガスに同伴するダストは、一般的にボイラーやバルーン煙道、電気集塵機(ホットコットレル)などで捕集されて、溶錬工程に繰返されるかあるいは別途湿式処理される。転炉工程で排出される全てのダストを転炉ダストとする。 The dust accompanying the exhaust gas in the converter process (PS-converter, MI-C furnace, flash converter, etc.), which is the subsequent process of the smelting process for melting ores in the copper smelting process, is generally boilers and balloon flues. It is collected by an electric dust collector (hot cot rel) or the like and repeated in the smelting process or separately wet-processed. All dust discharged in the converter process is used as converter dust.
銅製錬で排出される転炉ダストは、銅が5〜20mass%程度、砒素が2〜4mass%程度、カドミウムが2〜10mass%程度含まれており、希硫酸で浸出後、溶け残る鉛やビスマスなどと分離される。溶け出した銅、砒素、カドミウム、亜鉛、鉄などは、湿式処理を行い、系外除去されるか製錬工程へ繰り返される。表1に銅転炉ダストの代表的な組成を示す。
銅転炉ダストを水または硫酸により浸出し、銅、砒素、カドミウムを中和処理と硫化処理で分離回収する方法が開示されている。(特許第3052535号:特許文献1)
この方法では、銅と砒素を回収する際に中和処理を行うため、大量の中和残渣が生じる。このため、銅と砒素を製錬工程に繰り返す場合、大量の中和残渣を投入する分、鉱石の投入がカットされる。
A method is disclosed in which copper converter dust is leached with water or sulfuric acid, and copper, arsenic, and cadmium are separated and recovered by neutralization treatment and sulfidation treatment. (Patent No. 3052535: Patent Document 1)
In this method, since a neutralization process is performed when copper and arsenic are recovered, a large amount of neutralization residue is generated. For this reason, when copper and arsenic are repeated in the smelting process, the input of ore is cut as much as a large amount of neutralization residue is input.
本発明は、銅転炉ダストから銅と砒素、カドミウムを分離回収し、かつ回収残渣を低減する方法を提案するものである。 The present invention proposes a method for separating and recovering copper, arsenic and cadmium from copper converter dust and reducing the recovery residue.
本発明は、
(1)銅転炉ダスト中に含まれる銅、砒素、カドミウムを2段硫化処理することで分離し、1段目の硫化処理で得た銅と砒素を回収工程において回収し、2段目の硫化処理で得たカドミウムを系外除去する銅転炉ダストの処理方法。
(2)上記(1)記載の銅転炉ダストを希硫酸浸出し、希硫酸浸出後液を硫化処理する銅転炉ダストの処理方法。
(3)上記(1)〜(2)の何れか記載の希硫酸浸出後液をあらかじめ銀/塩化銀電極で酸化還元電位が290mV以下になるまで還元処理した後、1段目の硫化処理をする銅転炉ダストの処理方法。
(4)上記(1)〜(3)の何れか記載の1段目硫化処理後の後液を銀/塩化銀電極で酸化還元電位が30〜70mVに制御し、亜鉛の少ない硫化カドミウムを得る銅転炉ダストの処理方法。
(5)上記(1)〜(4)の何れか記載の処理工程の後、中和処理によって亜鉛と鉄を系外除去する銅転炉ダストの処理方法。
(6)上記(1)〜(5)の何れか記載の処理工程の残渣で、砒素とカドミウムの硫化混合物を銅溶液に入れて、カドミウムと銅の置換反応処理をする銅転炉ダストの処理方法。
を提供する。
The present invention
(1) Copper, arsenic, and cadmium contained in copper converter dust are separated by two-stage sulfidation treatment, and copper and arsenic obtained by the first-stage sulfidation treatment are collected in the recovery step, and the second stage A copper converter dust treatment method that removes cadmium obtained by sulfidation out of the system.
(2) A method for treating copper converter dust, wherein the copper converter dust described in (1) is leached with dilute sulfuric acid, and the solution after leaching with dilute sulfuric acid is sulfidized.
(3) After the dilute sulfuric acid leaching solution according to any one of (1) to (2) above is reduced with a silver / silver chloride electrode in advance until the oxidation-reduction potential is 290 mV or less, the first-stage sulfidation treatment is performed. To process copper converter dust.
(4) The post-solution after the first-stage sulfidation treatment as described in any one of (1) to (3) above is controlled at a redox potential of 30 to 70 mV with a silver / silver chloride electrode to obtain cadmium sulfide with less zinc. Processing method for copper converter dust.
(5) A copper converter dust treatment method in which zinc and iron are removed from the system by neutralization after the treatment step according to any one of (1) to (4) above.
(6) Treatment of copper converter dust in which the sulfide mixture of arsenic and cadmium is placed in a copper solution with the residue of the treatment process described in any one of (1) to (5) above, and a substitution reaction treatment of cadmium and copper is performed. Method.
I will provide a.
本発明によれば、
(1)銅転炉ダストから選択的に銅と砒素、カドミウムを回収できる。
(2)銅と砒素は混合物として回収できる。
(3)カドミウムを高品位で回収できる。
(4)銅と砒素、カドミウムを二段硫化で回収することにより、回収残渣を低減させることができる。
According to the present invention,
(1) Copper, arsenic and cadmium can be selectively recovered from copper converter dust.
(2) Copper and arsenic can be recovered as a mixture.
(3) Cadmium can be recovered with high quality.
(4) Recovery residue can be reduced by recovering copper, arsenic, and cadmium by two-stage sulfidation.
本発明の処理対象である銅転炉ダストは、銅、鉄、砒素、カドミウム、亜鉛、鉛、ビスマス等を含有している。
通常銅の転炉ダストは、希硫酸(硫酸濃度:10〜50g/L)に溶解後、主に硫酸鉛を沈殿させた希硫酸浸出残渣を得る。
上記の処理は、予め未溶解な硫酸鉛を銅転炉ダストから回収するためである。希硫酸浸出残渣を取り除いた後液には、銅、鉄、砒素、カドミウム、亜鉛等が含まれている。
The copper converter dust which is the object of treatment of the present invention contains copper, iron, arsenic, cadmium, zinc, lead, bismuth and the like.
Usually, copper converter dust is dissolved in dilute sulfuric acid (sulfuric acid concentration: 10 to 50 g / L), and then a dilute sulfuric acid leaching residue in which lead sulfate is mainly precipitated is obtained.
The above treatment is for recovering undissolved lead sulfate from copper converter dust in advance. The liquid after removing the dilute sulfuric acid leaching residue contains copper, iron, arsenic, cadmium, zinc and the like.
(二段硫化処理を用いた銅、砒素とカドミウムの分離回収方法)
図1は、本発明が提案する転炉ダストの処理フローである。転炉ダストを水または希硫酸で浸出し、沈殿した浸出残渣を取り除く。残渣を取り除いた浸出後液にあらかじめ銀/塩化銀電極で酸化還元電位が290mV以下になるまで還元処理を行い、5価の砒素を70%以上3価にしておき、二段硫化を行い、銅、砒素とカドミウムを分離回収する。銀/塩化銀電極の酸化還元電位と砒素の価数の関係を図2に示す。
また、一段目の硫化で生じた一次硫化残渣中にカドミウムの混入が多い場合は、この残渣を希硫酸浸出後液に導入し、カドミウムと銅の置換反応処理を行い、カドミウムを濃縮させることによって回収率を上げることができる。
(Method for separating and recovering copper, arsenic and cadmium using two-stage sulfidation)
FIG. 1 is a processing flow of converter dust proposed by the present invention. The converter dust is leached with water or dilute sulfuric acid to remove the precipitated leaching residue. The leached solution after removal of the residue is subjected to reduction treatment with a silver / silver chloride electrode in advance until the redox potential is 290 mV or less, pentavalent arsenic is made 70% or more trivalent, two-stage sulfidation is performed, and copper is added. Separate and recover arsenic and cadmium. Fig. 2 shows the relationship between the redox potential of the silver / silver chloride electrode and the valence of arsenic.
Also, if there is a lot of cadmium in the primary sulfide residue produced by the first stage sulfidation, this residue is introduced into the solution after leaching with dilute sulfuric acid, and the cadmium and copper are subjected to a substitution reaction treatment to concentrate cadmium. The recovery rate can be increased.
表2に代表的な希硫酸浸出後液中の各元素の液中濃度を示す。
H3AsO4
+ H2S → HAsO2 + S + 2H2O (1)
あるいは、
2H3AsO4
+ 2NaHS + H2SO4 → 2HAsO2 +2S + Na2SO4
+ 4H2O (2)
Table 2 shows typical concentrations of each element in the solution after leaching with dilute sulfuric acid.
H 3 AsO 4
+ H 2 S → HAsO 2 + S + 2H 2 O (1)
Or
2H 3 AsO 4
+ 2NaHS + H 2 SO 4 → 2HAsO 2 + 2S + Na 2 SO 4
+ 4H 2 O (2)
これを解決するため、あらかじめ砒素を3価にしておくと砒素の硫化反応速度が早まり、カドミウムより早く硫化し、分離することができることが本発明の重要な点である。 In order to solve this problem, it is an important point of the present invention that if arsenic is trivalent in advance, the arsenic sulfidation reaction rate is increased, and the arsenic can be sulfided and separated faster than cadmium.
ここで、銅の硫化反応式は以下の通りである。
CuSO4 + H2S → CuS + H2SO4 (3)
あるいは、
2CuSO4 + 2NaHS → 2CuS + Na2SO4 + H2SO4 (4)
銅は硫化水素あるいは硫化水素ナトリウムと1:1で反応する。
また、砒素の硫化反応式は以下の通りである。
2HAsO2 + 3H2S → As2S3 + 4H2O (5)
あるいは、
4HAsO2 + 6NaHS + 3H2SO4
→ As2S3 + 3Na2SO4
+8H2O (6)
5価の砒素が残っている場合、(1)あるいは(2)式の反応が先に起こり、その後(5)または(6)式の反応が起こる。砒素が3価の場合、硫化水素あるいは硫化水素ナトリウムと1:1.5で反応し、5価の場合1:2.5で反応する。
銅と砒素の濃度を元に計算した硫化水素あるいは硫化水素ナトリウムの当量を1.0〜1.25倍用いると希硫酸浸出後液中から全ての銅と砒素が硫化され、沈殿する。これを一次硫化工程とする。銅と砒素の硫化物は、銅製錬工程の原料となる。
Here, the sulfurization reaction formula of copper is as follows.
CuSO 4 + H 2 S → CuS + H 2 SO 4 (3)
Or
2CuSO 4 + 2NaHS → 2CuS + Na 2 SO 4 + H 2 SO 4 (4)
Copper reacts 1: 1 with hydrogen sulfide or sodium hydrogen sulfide.
The arsenic sulfurization reaction formula is as follows.
2HAsO 2 + 3H 2 S → As 2 S 3 + 4H 2 O (5)
Or
4HAsO 2 + 6NaHS + 3H 2 SO 4
→ As 2 S 3 + 3Na 2 SO 4
+ 8H 2 O (6)
When pentavalent arsenic remains, the reaction of formula (1) or (2) occurs first, and then the reaction of formula (5) or (6) occurs. When arsenic is trivalent, it reacts with hydrogen sulfide or sodium hydrogen sulfide at 1: 1.5, and when pentavalent, it reacts at 1: 2.5.
When the equivalent of hydrogen sulfide or sodium hydrogen sulfide calculated based on the concentrations of copper and arsenic is used 1.0 to 1.25 times, all copper and arsenic are sulfided and precipitated from the solution after diluting sulfuric acid. This is the primary sulfidation step. Copper and arsenic sulfide is a raw material for the copper smelting process.
一次硫化工程を終えた後液には、主にカドミウム、亜鉛、鉄が残存している。ここで、さらに硫化水素あるいは硫化水素ナトリウムを加えると、カドミウムを硫化することができる。反応式を以下に示す。
CdSO4 + H2S
→ CdS + H2SO4 (7)
あるいは、
2CdSO4 + 2NaHS → 2CdS +
Na2SO4 + H2SO4 (8)
このとき、亜鉛も多少硫化反応を起こすが、反応液をAg/AgCl電極で銀/塩化銀電極において酸化還元電位30〜70mVで制御すると亜鉛の少ない硫化カドミウムを得ることができる。カドミウムを硫化する工程を二次硫化工程とする。
Cadmium, zinc, and iron mainly remain in the liquid after the primary sulfidation step. Here, when hydrogen sulfide or sodium hydrogen sulfide is further added, cadmium can be sulfided. The reaction formula is shown below.
CdSO 4 + H 2 S
→ CdS + H 2 SO 4 (7)
Or
2CdSO 4 + 2NaHS → 2CdS +
Na 2 SO 4 + H 2 SO 4 (8)
At this time, zinc also undergoes some sulfurization reaction, but cadmium sulfide with less zinc can be obtained by controlling the reaction solution with an Ag / AgCl electrode at a silver / silver chloride electrode at a redox potential of 30 to 70 mV. The step of sulfiding cadmium is referred to as a secondary sulfidation step.
二次硫化工程を終えた後液には、主に亜鉛と鉄が残存している。これらは、水酸化ナトリウムなどのアルカリ剤を加えて、液のpHが8.5〜10になるまで上げて水酸化物として回収する。これを中和工程とする。 Zinc and iron mainly remain in the liquid after the secondary sulfiding step. These are added as an hydroxide by adding an alkaline agent such as sodium hydroxide until the pH of the liquid becomes 8.5 to 10. This is the neutralization step.
(実施例)
希硫酸浸出後液の還元処理を亜硫酸ガスの吹き込みによって行った。2Lの転炉ダストの希硫酸浸出後液に100%SO2を500mL/min.の流速で30分間吹き込み、銀/塩化銀電極で酸化還元電位を270mVまで下げた。亜硫酸ガスによる砒素の還元の効果を表3に示す。
After the dilute sulfuric acid leaching, the solution was reduced by blowing in sulfurous acid gas. 100% SO 2 was blown into the 2 L converter dust after dilute sulfuric acid leaching for 30 minutes at a flow rate of 500 mL / min., And the redox potential was lowered to 270 mV with a silver / silver chloride electrode. Table 3 shows the effect of arsenic reduction with sulfurous acid gas.
SO2還元後の希硫酸浸出後液中の主な成分を表4に示す。
一次硫化工程終了後の後液中の主な成分を表5に示す。
次に、二次硫化工程として、銀/塩化銀電極で酸化還元電位が40mVになるまで320g/L硫化水素ナトリウム溶液を加えた。加えた量は70mLである。
Table 5 shows the main components in the post-solution after the completion of the primary sulfidation step.
Next, as a secondary sulfiding step, 320 g / L sodium hydrogen sulfide solution was added until the oxidation-reduction potential reached 40 mV at the silver / silver chloride electrode. The amount added is 70 mL.
二次硫化工程終了後の後液中の主な成分を表6に示す。
次に、中和工程として、pHが9.5に上がるまで48%水酸化ナトリウム溶液を加えた。中和工程後液中の主な成分を表7に示す。
Next, as a neutralization step, 48% sodium hydroxide solution was added until the pH increased to 9.5. Table 7 shows the main components in the solution after the neutralization step.
Claims (6)
A method for treating copper converter dust, characterized in that the residue of the treatment step according to any one of claims 1 to 5, wherein a sulfite mixture of arsenic and cadmium is placed in a copper solution and a substitution reaction treatment of cadmium and copper is performed. .
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Cited By (4)
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JP2011026687A (en) * | 2009-07-29 | 2011-02-10 | Pan Pacific Copper Co Ltd | Method for treating copper converter dust |
JP2011032516A (en) * | 2009-07-31 | 2011-02-17 | Pan Pacific Copper Co Ltd | Treatment method for copper converter dust |
JP2017213507A (en) * | 2016-05-31 | 2017-12-07 | 住友金属鉱山株式会社 | Waste acid treatment method |
CN109499340A (en) * | 2019-01-02 | 2019-03-22 | 湖南省环境保护科学研究院 | The method of arsenic alkaline slag and flue gas desulfurization combined processing |
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JP3052535B2 (en) * | 1992-02-25 | 2000-06-12 | 三菱マテリアル株式会社 | Treatment of smelting intermediates |
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KR100707110B1 (en) * | 2004-09-29 | 2007-04-13 | 닛코 킨조쿠 가부시키가이샤 | Copper converter dust treatment method |
-
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JPS58141346A (en) * | 1982-02-15 | 1983-08-22 | Dowa Mining Co Ltd | Collecting method of metal from industrial by-product |
JPH1112667A (en) * | 1997-06-26 | 1999-01-19 | Nikko Kinzoku Kk | Treating method and recovering method of solution containing cadmium and zinc |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2011026687A (en) * | 2009-07-29 | 2011-02-10 | Pan Pacific Copper Co Ltd | Method for treating copper converter dust |
JP2011032516A (en) * | 2009-07-31 | 2011-02-17 | Pan Pacific Copper Co Ltd | Treatment method for copper converter dust |
JP2017213507A (en) * | 2016-05-31 | 2017-12-07 | 住友金属鉱山株式会社 | Waste acid treatment method |
CN109499340A (en) * | 2019-01-02 | 2019-03-22 | 湖南省环境保护科学研究院 | The method of arsenic alkaline slag and flue gas desulfurization combined processing |
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