KR950007786B1 - Method of slime treatment with copper & arsenic - Google Patents
Method of slime treatment with copper & arsenic Download PDFInfo
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- KR950007786B1 KR950007786B1 KR1019930009978A KR930009978A KR950007786B1 KR 950007786 B1 KR950007786 B1 KR 950007786B1 KR 1019930009978 A KR1019930009978 A KR 1019930009978A KR 930009978 A KR930009978 A KR 930009978A KR 950007786 B1 KR950007786 B1 KR 950007786B1
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Abstract
Description
첨부도면은 비소전물의 처리 공정도.Attached drawing is process chart of non-sintered material.
본 발명은 비소전물(As澱物)에서 Cu(동) 및 As(비소)를 분리·회수하는 방법에 관한 것으로, 보다 상세하게는 전해채취시 생성되는 Cu와 As를 함유한 전착물을 분리 처리하여 동을 함유한 용액은 재사용하고, 비소용액은 아비산의 형태로 회수하는 동 및 비소를 함유한 원료의 처리방법에 관한 것이다.The present invention relates to a method for separating and recovering Cu (copper) and As (arsenic) from an arsenic material, and more particularly, to separate and process an electrodeposited material containing Cu and As generated during electrowinning. The present invention relates to a method for treating raw materials containing copper and arsenic, wherein copper-containing solutions are reused and arsenic solutions are recovered in the form of arsenic acid.
일반적으로 동광석은 용광로, 반사로등의 용련로에서 중간 생성물인 매트(matt)를 만들고 이를 전로, 전기로등에서 조동(粗銅)을 만든 후 이 조동을 다시 정제로에서 유황(S)과 산소를 제거하는데, 이 정제된 조동은 아직 불순물과 회수할 부산물인 유가금속을 함유하고 있으므로 불순물 제거와 부산물 회수가 용이한 정해정련을 하여 전기동이라 부르는 순동을 얻는다.In general, copper ore makes an intermediate product in molten furnaces such as smelters, reflectors, etc., and makes crude copper in converters, electric furnaces, etc. and removes sulfur (S) and oxygen from refineries. However, this refined crude copper still contains impurities and valuable metals, which are by-products to be recovered, and thus, refined refining is easy to remove impurities and recover by-products, thereby obtaining pure copper called electrophoresis.
전해정련에서는 다량의 유리황산을 포함한 황산동 용액을 전해액으로 하고 양극은 불순물이 함유된 조동을 주조하여 양극판으로하며, 음극으로서는 순동의 종판(種板)을 써서 전류를 통하면 Cu는 양극에서 용해되고 음극에서 순동(99.99%이상)이 석출된다.In electrolytic refining, a copper sulfate solution containing a large amount of free sulfuric acid is used as an electrolyte, and the anode is cast as a positive electrode by casting a copper containing impurity.The cathode is a pure copper end plate, and when a current is passed, Cu is dissolved in the anode. Pure copper (more than 99.99%) precipitates at the cathode.
이때 양극에 함유된 불순물 중 어느 것은 용해되지 않고 전해조 밑에 남아서 양극슬라임(anode slime)으로 침전되고, 동보다 전기 화학적으로 卑한 원소들은 용해되어 전해액중에 들어간다.At this time, any of impurities contained in the positive electrode do not dissolve but remain under the electrolytic cell to precipitate as an anode slime, and electrochemically more chemical elements are dissolved and enter the electrolyte.
용해되는 원소의 하나가 비소인데 시간이 경과됨에 따라 양극에서 용출한 비소가 점차 증가되고 양극에서의 용출된 동은 음극에서의 석출동보다 일발적으로 많으므로 전해액중 동량이 증가하는 한편 황산은 감소하므로 순환계통에서 전해액의 일부를 취출하고 새로운 전해액을 보충한다. 취출된 전해액은 전해채취에서 탈동 및 탈비한다.One element that dissolves is arsenic, and as time passes, arsenic eluted from the anode gradually increases, and copper eluted from the anode is larger than precipitated copper from the cathode, so copper content in the electrolyte increases while sulfuric acid decreases. Therefore, part of the electrolyte is removed from the circulation system and the new electrolyte is replenished. The withdrawn electrolyte is desorbed and degreased by electrowinning.
이때 전해채취는 양극을 불용성 물질로하고, 음극은 순동판을 종판으로 하여 조업하면 전해액중의 동은 음극에서 석출채취되나, 동을 포함한 많은 비소는 조바닥에 전착된다.(이들 ˝비소전물˝이하 칭함)At this time, when electrolytic extraction is performed with anode as insoluble material and cathode as pure plate as end plate, copper in electrolyte is extracted from cathode, but many arsenic including copper is electrodeposited on the bottom of the tank. Referred to below)
이 비소전물은 Cu3As를 주성분으로 하는 슬라임상으로 그 외에 Cu2As, Bi, Sb, Pb등을 함유하고 있다. 이런 비소전물을 제련공정으로 되돌려 순환시키면 제련계 내에 다량의 비소가 축척 순환된다.This non-sintered body is a slime phase containing Cu 3 As as a main component, and also contains Cu 2 As, Bi, Sb, Pb, and the like. When the arsenic material is returned to the smelting process, a large amount of arsenic is accumulated in the smelting system.
현재와 같이 비소분이 많은 동광석을 사용해야 하는 상황에서는 더욱 비소 순환량이 많게됨으로 고순도를 유하는 전기, 전자 제품등의 품질에 악영향을 미친다.In the situation where copper ore with a large amount of arsenic needs to be used as described above, the amount of arsenic circulating increases, which adversely affects the quality of electrical and electronic products that maintain high purity.
따라서 이런 비소를 함유한 전물을 제련 공정으로 순환 사용하기 위해서는 비소의 계외 처리가 중요한 문제가 된다.Therefore, the off-system treatment of arsenic becomes an important problem in order to circulate and use the whole thing containing such arsenic in a smelting process.
비소전물의 계외처리에는 건식벅과 습식법을 들 수 있으나, 건식법에서는 필연적으로 As2O3를 함유한 배가스 더스트(dust) 처리가 피룡하게 되고 공해방지 설비등의 설비비가 높게되며 특히 환경규제에 대처하기 곤란하므로 습식법에 의한 처리를 고려하여야 한다.The out-of-system treatment of non-sintered materials includes dry buck and wet methods, but in the dry method, inevitably, flue gas dust treatment containing As 2 O 3 is inevitable, and equipment costs such as pollution prevention facilities are high, especially in response to environmental regulations. The treatment by wet method should be considered.
습식법의 처리방법으로는 일본국 공개 특허공보 (소)54-6959가 알려지고 있는데, 여기에서는 비소전물을 원료로하여 산화하고 슬러리화한 후 수산화 나트륨을 첨가하여 침출처리하고, 침출후액에 소석회를 첨가하여 생성한 비산칼슘을 황산으로 용해하여 석고와 비산으로 분리한다. 그리고 비산을 아황산가스로 환원하는 방법으로 하고 있다.Japanese Patent Application Laid-Open No. 54-6959 is known as a wet treatment method. In this process, non-sintered materials are oxidized and slurried, and sodium hydroxide is added to leach, and lime is added to the leach liquor. Calcium arsenate produced by addition is dissolved with sulfuric acid and separated into gypsum and arsenic acid. In addition, fugitive is reduced to sulfurous acid gas.
그러나 이와 같은 방법에서는 비소를 함유한 석고가 생성되기 때문에 석고 처리에 문제가 있고 수산화 나트륨의 손실을 비롯한 비소에 대하여 이중 침출조작이 필요하는 등의 문제점이 있다.However, in such a method, since arsenic-containing gypsum is produced, there is a problem in the gypsum treatment and a double leaching operation is required for arsenic including loss of sodium hydroxide.
이에 본 발명은 종래와 같이 비소전물을 제련공정으로 순환하지 않고 비소전물에 함유된 동 및 비소를 유가물의 형태로 회수 가능한 습식처리법을 제공코자 하는 것으로, 비소전물을 황산산성 용액에서 침출하고 용매추출에 의해 동과 비소를 분리, 동을 함유한 용액은 전해공정으로 되돌려 사용하고 비소용액은 아비산의 형태로 회수하는 것에 관한 것이다.Accordingly, the present invention is to provide a wet treatment method for recovering copper and arsenic contained in non-sintered materials in the form of valuables without circulating the non-sintered materials in a smelting process as in the prior art. By separating copper and arsenic, the solution containing copper is returned to the electrolytic process and the arsenic solution is recovered in the form of arsenic acid.
이하 본 발명을 설명하면 다음과 같다.Hereinafter, the present invention will be described.
본 발명은 동과 비소를 함유한 비소전물을 황산으로 침출하여 침출여재와 침출액을 얻는 공정과, 이 침출액을 혼합용매로 추출하여 동을 함유한 유기상과 비소를 함유한 추출잔액으로 분리하는 유기용매 추출공정과, 상기한 동을 함유한 유기상은 황산 동액으로 탈거하여 고순도 황산동 용액을 얻는 공정과, 상기한 비소를 함유한 추출잔액은 아황산가스로 환원한 다음 산성화 처리하고 증발농축하여 아비산을 정출하는 공정으로 하여 동과 비소를 분리·회수하는 것이다.The present invention is a process of leaching arsenic containing copper and arsenic with sulfuric acid to obtain a leaching media and leaching solution, and extracting the leaching solution with a mixed solvent to separate the organic phase containing copper and the extraction residue containing arsenic and an organic solvent. The extraction step, the organic phase containing the copper is removed with a copper sulfate solution to obtain a high-purity copper sulfate solution, and the extraction residue containing arsenic is reduced with sulfurous acid gas, acidified and concentrated to evaporate arsenic acid In this process, copper and arsenic are separated and recovered.
본 발명에서 사용하는 혼합용매라 함은 LIX계(미국 헨켈사 상품명) 용매와 희석제의 혼합물을 말한다.The mixed solvent used in the present invention refers to a mixture of a LIX solvent (trade name of Henkel, USA) and a diluent.
여기서 LI계 용매란 LIX84를 의미하는 것으로 2-하드록시-5-노니레이스토페논 옥심(2-hydroxy-5-nonylacetophenone Oxime)이고, 희석제는 케러신(Kerosene)이다.LI-based solvent here means LIX84, 2-hydroxy-5-nonylacetophenone Oxime, and the diluent is Kerosine.
첨부된 도면은 본 발명의 제조공정도로서 이에 따라 구체적으로 설명한다.The accompanying drawings will be described in detail according to the manufacturing process diagram of the present invention.
침출된 2단계에 걸쳐서 행할 수 있는데, 1단계 침출에서는 용매 추출 공정에 알맞는 PH=1.7용액으로 하기위해 약산으로 침출하여 침출여재와 침출액으로 여과 분리한다. 이때 얻어진 침출액은 용매추출 공정으로 보내고, 침출여재는 강산으로 2단계 침출하여 침출여재와 침출액으로 여과 분리한 후 이때 얻어진 침출액은 상기한 1단계 침출 공정으로 순환시킨다.It can be carried out in two stages of leaching. In the first stage leaching, the solution is leached with a weak acid in order to obtain a pH = 1.7 solution suitable for the solvent extraction process, and the filtrate is separated into a leaching medium and a leaching solution. The leaching solution thus obtained is sent to a solvent extraction process, the leaching medium is leached with a strong acid in two stages, and the leachate is filtered and separated into a leaching medium and a leaching solution.
이와 같은 2단계 침출은 1단계에서 나온 침출여재 중에 잔존한 동과 비소를 재활용하기 위한 것이다.This second stage leaching is to recycle the remaining copper and arsenic in the leaching media from the first stage.
1단계 침출 공정에서 얻어진 침출액을 용매 추출 공정에서 LIX계 용매와 희석재가 혼합된 혼합용매를 사용하여 동 이온을 함유한 유기상과 비소를 함유하는 추출잔액으로 추출 분리한다. 이때 용매 혼합물과 침출액의 접촉비(O/A=Organic Phase/Ague ous Phase)는 3-7에서 행할 수 있다. ˝O˝는 LIX와 Kerosene을 부피비로 2 : 8로 혼합 용매이고, ˝A˝는 1단계 침출액을 의미한다.The leaching solution obtained in the step 1 leaching process is extracted and separated into an extraction residue containing an organic phase containing ions and arsenic using a mixed solvent of a LIX solvent and a diluent in a solvent extraction step. At this time, the contact ratio (O / A = Organic Phase / Agueous Phase) of the solvent mixture and the leachate may be performed in 3-7. “O” is a mixed solvent of LIX and Kerosene in a volume ratio of 2: 8, and “A” is a one-step leach solution.
여기서 비소전물중의 혼합조성은 일정하지 않고 각각의 작업조건(전해채취)에 따라 비소전물중의 동 및 비소의 함량이 변화될 수 있다. 즉, 동의 함량이 25wt%에서 45wt%로 변화될 때 O/A비는 3에서 7로 변화할 수 있다. 또한 O/A비는 용매의 본래 특성에 따라 변화될 수 있다.Here, the mixing composition of the non-sintered material is not constant, and the contents of copper and arsenic in the non-sintered material may change according to respective working conditions (electrolytic extraction). That is, when the copper content is changed from 25wt% to 45wt%, the O / A ratio may be changed from 3 to 7. The O / A ratio may also vary depending on the nature of the solvent.
이와 같이 본 발명에 이용되는 혼합용매는 비소전물의 품위에 따라 변환 될 수 있음으로 상기한 O/A=327비는 실시예를 제시한데 불과하다. 따라서 본 발명은 상기한 수치범위에 국한하지 않는다.As described above, the mixed solvent used in the present invention may be converted according to the quality of the non-sintered material, and thus the O / A ratio of 327 is merely an example. Therefore, the present invention is not limited to the above numerical range.
상기한 추출 공정에서 분리된 동 이온을 함유한 유기상은 황상동 용액으로 탈거하여 고순도 황산동 용액을 얻으며 용매는 물로 세척하여 추출공정에 재사용 한다.The organic phase containing copper ions separated in the extraction process is removed with a sulfur phase copper solution to obtain a high purity copper sulfate solution, and the solvent is washed with water and reused in the extraction process.
한편 상기한 동이 제거된 추출잔액(비소함유용액)은 아황산가스를 이용하여 비소(V)를 비소(III)로 환원한 다음 황산을 가하여 산성화한 후, 증발농축하여 아비산을 정출시켜 고액 분리하다.On the other hand, the extraction residue (arsenic-containing solution) from which the copper is removed is reduced to arsenic (V) using arsenic acid gas, followed by acidification with sulfuric acid, and then concentrated by evaporation to extract arsenic acid to solid-liquid separation.
이때 얻어진 정출여재는 상기의 2단계 침출공정으로 이동된다.The crystallization medium obtained at this time is moved to the two-step leaching process.
다음은 실시예에 따라 설명한다.The following is described according to the embodiment.
동 27.82wt%, 비소 26.47wt%를 함유한 비소전물 75g을 아래와 같은 조건으로 침출을 2단계 실시하였다.A leaching of 75 g of arsenic material containing 27.82 wt% copper and 26.47 wt% arsenic was carried out in two steps under the following conditions.
1단계 침출조건Stage 1 Leaching Conditions
-황산농도 : 30g/lSulfuric acid concentration: 30g / l
-침출시간 : 4HrLeaching time: 4Hr
-Phlp density : 150g/l-Phlp density: 150g / l
-침출온도 : 90℃Leaching temperature: 90 ℃
공기압 : 1Kg/cm2, 10mmΦ 유리대롱으로 공기 공급Air pressure: 1Kg / cm 2 , air supply to 10mmΦ glass cupboard
1단계 침출에서는 500mml의 침출액을 얻었으며 침출액의 조성은 다음과 같다.In the first stage leaching, 500mml of leachate was obtained and the composition of leachate was as follows.
[표 1]TABLE 1
2단계 침출조건Stage 2 Leaching Conditions
-황산농도 : 90g/lSulfuric acid concentration: 90g / l
-침출시간 : 4HrLeaching time: 4Hr
-Phlp density : 150g/l-Phlp density: 150g / l
-침출온도 : 90℃Leaching temperature: 90 ℃
공기압 : 1Kg/cm2, 10mmΦ 유리대롱으로 공기 공급Air pressure: 1Kg / cm 2 , air supply to 10mmΦ glass cupboard
1단계 침출에서는 얻어진 침출여재에 대해 상기 2단계 침출조건으로 침출한 결과 아래와 같은 조성의 2단계 침출여재 2.6gr을 얻었다.In the first stage leaching, the leaching media obtained were leached under the above two stage leaching conditions to obtain 2.6 gr of a two stage leaching media having the following composition.
[표 2]TABLE 2
상기와 같이 1, 2단계의 총 침출율은 As 97%, Cu 99% 이상을 나타내었다. 1단계 침출액은 아래와 같은 조건으로 다단식 용매추출장치에서 행하였다.As described above, the total leaching rates of the first and second stages were As 97% and Cu 99% or more. The first stage leaching solution was carried out in a multi-stage solvent extraction apparatus under the following conditions.
용매추출조건Solvent Extraction Conditions
1) 추출(Extraction)1) Extraction
-급액(Feel sol'n) : 1단계 침출액-Feel sol'n: Stage 1 leachate
-용매(Solvent) : LIX84(20Vol% in Kerosene)Solvent: LIX84 (20Vol% in Kerosene)
-pH : (암모니아수로서 1.7로 조절)-pH: (adjusted to 1.7 as ammonia water)
-접촉비(O/A ratio) : 5.5Contact ratio (O / A ratio): 5.5
-단수 : 4단-Single stage: 4 stage
2) 탈거(Stripping)2) Stripping
-탈취액(Strip sol'n) : Cu 25g/l, H2SO4: 200g/lStrip sol'n: Cu 25g / l, H 2 SO 4 : 200g / l
-접촉비(O/A ratio) : 2O / A ratio: 2
-단수 : 2단-Single stage: 2 stage
* O/A에서 ˝O˝는 추출단계를 거친 혼합용매와 동이온 loading된 것이며, A는 탈취액(Cu 25g/l, H2SO4200g/l의 조성)을 의미함* O / A in ˝O˝ will rough the extraction step with a mixed solvent of copper ion loading, A is also a deodorizing liquid (25g Cu / l, H 2 Composition of SO 4 200g / l)
용매추출시 물량(Cu, As)Quantity of solvent extraction (Cu, As)
[표 3]TABLE 3
이상과 같은 용매추출에 의하여 동을 함유한 탈거액(Pregnatn Strip sol'n) 1325ml와 비소를 함유한 추출잔액(Raffinate) 500ml을 얻었으며 각각의 조성은 위와 같으며 동의 용매추출율 및 비소의 분리율은 Cu 99%, As 96% 이상이었다.By the above solvent extraction, 1325 ml of copper stripping solution (Pregnatn Strip sol'n) and 500 ml of arsenic-containing extract (Raffinate) were obtained, and the composition of each was as described above. Cu was 99% and As 96% or more.
위와 같은 용매추출에서 얻어진 추출잔액(Raffinate sol'n) 500ml로부터 비소를 아비산의 형태로 회수하기 위해 아래와 같은 조건으로 아비산 정출을 행하였다.In order to recover arsenic in the form of arsenic from 500 ml of the extract (Raffinate sol'n) obtained by the solvent extraction as described above, arsenic acid was purified under the following conditions.
아비산정출조건Absorption conditions
1) 아황산가스 환원 : 상온에서 600ml/min으로 3Hr1) Sulfur Dioxide Reduction: 3Hr at 600ml / min at room temperature
2) 황산농도에 따른 As(III)의 용해도차를 이용하여 아비산을 정출시키기 위하여, 산성화처리(Acidificaion) 및 증발농축(Evaporation)을 행하였다.2) Acidification and evaporation were performed to determine the arsenic acid using the solubility difference of As (III) according to sulfuric acid concentration.
-산성화처리 : 상기 아황산가스환원 여액에 H3SO4735g/l 용액 500ml을 첨가.Acidification treatment: 500 ml of a solution of 735 g / l H 3 SO 4 was added to the sulfurous acid gas reduction filtrate.
-증발농축 : 증발농축 처리전 부피의 1/2까지 실시.Evaporative concentration: up to 1/2 of the volume before evaporative concentration.
상기 아비산 정출공정에 의해 아비산결정 5.96gr 및 정출후액 500ml를 얻었으며 각각의 조성은 다음과 같다.By the above arsenic acid crystallization process, 5.96 gr of arsenic acid crystals and 500 ml of crystallized liquid were obtained, and the composition of each was as follows.
[표 4]TABLE 4
정출과정의 비소의 회수율 83% 이상의 결과를 나타내었다.Arsenic recovery was more than 83%.
결과적으로 1단계 침출액으로부터 용매추출, 정출과정을 종합하여 고려하면 동회수율은 99% 이상이며, 비소회수율은 80% 이상을 나타내어 동과 비소를 함유하는 원료로부터 동과 비소를 분리·회수하는 방법을 제공하게 된다.As a result, considering the solvent extraction and extraction process from the first stage leachate, the copper recovery rate is over 99% and the arsenic recovery rate is over 80%, thus separating and recovering copper and arsenic from raw materials containing copper and arsenic. Will be provided.
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