KR100686985B1 - The nickel collecting method from waste nickel fluid and oxidic acid nickel sludge - Google Patents
The nickel collecting method from waste nickel fluid and oxidic acid nickel sludge Download PDFInfo
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- KR100686985B1 KR100686985B1 KR1020040032603A KR20040032603A KR100686985B1 KR 100686985 B1 KR100686985 B1 KR 100686985B1 KR 1020040032603 A KR1020040032603 A KR 1020040032603A KR 20040032603 A KR20040032603 A KR 20040032603A KR 100686985 B1 KR100686985 B1 KR 100686985B1
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Abstract
본 발명은 니켈폐액 및 수산니켈슬러지에서 니켈회수방법에 관한 것이며 니켈이 함유되는 산업폐기물에서 니켈을 석출하여 자원소재로 활용하고, 산업폐기물을 효과적으로 정화처리 할 수 있도록 함에 목적이 있다.The present invention relates to a nickel recovery method in nickel waste liquor and nickel hydroxide sludge, and has an object to precipitate nickel from industrial waste containing nickel and use it as a resource material and to effectively purify industrial waste.
본 발명은 니켈이 함유하는 니켈폐액 및 수산니켈슬러지에 염산을 투여하여 혼합교반하고, 여기에 아민계 용매를 투여시켜 불순물을 제거시킨 다음 전기분해시켜 니켈을 회수하는 방법이다.The present invention is a method for recovering nickel by administering and stirring hydrochloric acid to the nickel waste liquid and nickel hydroxide sludge containing nickel, and then removing the impurities by administering an amine solvent thereto.
이와 같은 본 발명은 니켈가공공정과 니켈도금공정에서 발생되는 니켈폐액 및 수산니켈슬러지의 산업 폐기물에서 니켈을 효율적으로 석출하여 자원소재로 재활용하고, 폐용수의 정화 처리를 효율적으로 수행할 수 있게 되므로 산업상 유용한 발명이다.As described above, the present invention efficiently precipitates nickel from industrial waste of nickel waste liquid and nickel hydroxide sludge generated in the nickel processing process and the nickel plating process, recycles it as a resource material, and efficiently cleans waste water. Industrially useful invention.
니켈폐액, 수산니켈슬러지, 용매, 전기분해, 석출Nickel waste solution, nickel hydroxide sludge, solvent, electrolysis, precipitation
Description
도1은 본 발명의 작업공정을 보인 블럭도1 is a block diagram showing a working process of the present invention
본 발명은 니켈폐액 및 수산니켈슬러지에서 니켈 회수 방법에 관한 것이며 니켈이 함유하는 산업폐기물에서 니켈은 회수하여 자원소재로 재활용하고, 폐용수는 효율적으로 정화처리하기 위한 것이다.The present invention relates to a method for recovering nickel from nickel waste liquid and nickel sludge, and recovers nickel from industrial wastes contained in nickel and recycles it as a resource material, and efficiently purifies waste water.
종래에는 니켈가공공정 및 니켈도금공정에서 산업폐기물로 발생되는 니켈폐액 및 수산니켈슬러지가 발생 된다. 이와 같은 니켈도금폐액 및 수산니켈슬러지에 함유하는 철을 제거하는 중화제로 염산, 수산화나트륨, 수산화칼륨, 탄산칼슘등이 사용되고, PH를 조정하여 수산철을 제거하게 되나 중화제의 사용시 15∼50%의 니켈의 공침이 생기게 되므로 중화제의 사용은 제한적일수밖에 없게 되고, 암모니아를 이용하게 되면 90%이상의 니켈회수가 가능하게 되나 회수된 니켈에 잔존하는 암모니아의 처리에 따른 2차 오염이 발생되고, 또 암모니아 처리 설비에는 많은 비용이 소요되고, 처리비용이 많아 경제성이 없어 실용화되지 못하고 있다.Conventionally, nickel waste liquid and nickel hydroxide sludge generated as industrial wastes are generated in the nickel processing process and the nickel plating process. Hydrochloric acid, sodium hydroxide, potassium hydroxide, calcium carbonate and the like are used as neutralizing agents for removing iron contained in the nickel plating waste solution and nickel hydroxide sludge, and the pH is adjusted to remove iron hydroxide. Since the coprecipitation of nickel is generated, the use of neutralizing agent is limited, and when ammonia is used, more than 90% of nickel recovery is possible, but secondary pollution occurs due to the treatment of ammonia remaining in the recovered nickel. The facility requires a lot of cost, and the processing cost is high, it is not economical, it is not practical.
또 아연(Zn), 구리(Cu), 망간(Mn), 크롬(Cr) 및 기타 불순물의 경우에는 현존하는 중화제로서는 효과적으로 제거할 수 없고, 니켈폐액은 80℃ 이상에서 1시간이상의 수열반응이 동반되어야 하므로 에너지 절감 측면에서도 바람직하지 못한 실정이다.In the case of zinc (Zn), copper (Cu), manganese (Mn), chromium (Cr) and other impurities, existing neutralizing agents cannot be effectively removed, and the nickel waste liquid is accompanied by hydrothermal reaction for over 1 hour at 80 ° C or higher. Since it should be, it is not desirable in terms of energy saving.
또 폐액에서 회수된 니켈(Ni)은 염산, 황산, 질산을 투여하여 증발농축 및 결정화단계를 거쳐 탄산니켈, 황산니켈, 질산니켈등 니켈화합물을 생산하고 이를 제련의 공정으로 니켈메탈이 생산되고 있는 실정이다.In addition, nickel (Ni) recovered from the waste liquid is treated with hydrochloric acid, sulfuric acid, and nitric acid to evaporate and crystallize to produce nickel compounds such as nickel carbonate, nickel sulfate, and nickel nitrate, and nickel metal is produced as a smelting process. It is true.
이에 본 발명은 니켈폐액 (수산니켈슬러지 포함)을 산으로 침출한 침출액과 침출액에서 철분과 불순물을 제거하고, 불순물이 제거된 고순도 니켈수용액을 전기분해로 니켈을 석출할수 있는 니켈폐액 및 수산니켈슬러지에서 니켈회수 방법을 제공함에 목적을 두고 있다.Therefore, the present invention removes iron and impurities from the leaching solution and leaching solution leaching nickel waste liquid (including nickel hydroxide sludge), and the nickel waste liquid and nickel hydroxide sludge which can deposit nickel by electrolysis of the high purity nickel aqueous solution from which impurities are removed. Aims to provide a nickel recovery method.
본 발명은 도1과 같이 니켈이 함유하는 니켈폐액(수산니켈슬러지 포함)을 35%염산에 용해시켜 염화니켈 수용액을 만들고 케로센(kerosene)으로 희석시킨 아민계 용매를 투여하여 불순물 금속이온을 추출하고, 유수분리기에서 유분을 제거하고, 정제된 니켈수용액을 전기분해시켜서 니켈판을 석출하는 니켈 회수 방법이다.In the present invention, as shown in FIG. 1, nickel waste solution (including nickel hydroxide sludge) containing nickel is dissolved in 35% hydrochloric acid to make an aqueous nickel chloride solution, and an impurity metal ion is extracted by administering an amine solvent diluted with kerosene. And, it is a nickel recovery method to precipitate the nickel plate by removing the oil in the oil / water separator, and electrolyzing the purified aqueous nickel solution.
본 발명은 니켈폐액을 염산과 교반시킨다음 용매를 이용하여 니켈을 제외한 기타 중금속을 용매층에서 추출하고, 니켈은 수용액층에 잔류시켜 고순도의 니켈수용액을 조성하게 된다.In the present invention, the nickel waste solution is stirred with hydrochloric acid, and then, using a solvent, other heavy metals except nickel are extracted from the solvent layer, and nickel remains in the aqueous solution layer to form a high-purity nickel aqueous solution.
이때 사용되는 용매는 아민계(amine) 용매로 툴루앤(toluene) 또는 케로센(kerosene)에 희석하여 상비(유기상/수용액상)가 2∼3의 조건하에서 불순물을 추출한다.At this time, the solvent used is an amine solvent (dilution) in toluene (keluene) or kerosene (kerosene) to extract impurities under conditions of 2-3 (organic phase / aqueous phase) is 2-3.
또 용매를 침출액에 투여하여 교반시간은 30초내지 2분간으로 하고, 교반회전수는 300∼500rpm이 적당하고, 분리시간은 1분내지 10분으로 한다.The solvent is added to the leaching solution, and the stirring time is 30 seconds to 2 minutes, the stirring rotation speed is suitably 300 to 500 rpm, and the separation time is 1 minute to 10 minutes.
또 추출제의 농도는 20∼30%가 바람직하고, 20%이하인 경우에는 추출효율이 떨어지고, 30%이상이 되면 분리시간이 길어지거나 분리되지 않을수도 있다.In addition, the concentration of the extractant is preferably 20 to 30%, and the extraction efficiency is lower when the concentration is 20% or less, the separation time may be long or may not be separated when 30% or more.
또 추출한 불순물의 유기상은 용매재생을 위하여 역추출하여 반복 사용하게 되며 역추출에는 염산 농도가 5%미만인 수용액을 이용하고, 상비와 교반시간, 분리시간은 추출시와 같으며 재생용매와 새로운 용매간에 용매, 색차지, 추출능력에 차이가 발생되지 않도록 유의한다.In addition, the extracted organic phase of the impurity is repeatedly extracted for solvent regeneration, and for back extraction, an aqueous solution having a hydrochloric acid concentration of less than 5% is used. Care should be taken to avoid differences in solvent, color charge, and extraction capacity.
이와 같은 용매를 이용하여 니켈을 제외한 기타 중금속을 추출하고, 잔존하는 니켈수용액에서 니켈을 전해방식으로 석출하게 되며, 그화학 반응은 다음과 같다.Using such a solvent to extract other heavy metals except nickel, and to precipitate nickel in the remaining nickel aqueous solution by electrolytic method, the chemical reaction is as follows.
음극(-)cathode(-)
Ni2+ + 2e- → NiNi 2+ + 2e- → Ni
2H+ + 2e- → H22H + + 2e- → H2
양극(+)Positive (+)
H2O → (1/2)O2 + 2H+ + 2e-H 2 O → (1/2) O 2 + 2H + + 2e-
2Cl- →Cl2 + 2e-2Cl- → Cl 2 + 2e-
또 전해조에 사용되는 음극(-)에는 경제성과 내화학성 및 내구성을 고려하여 티탄(Ti)을 사용하고, 양극(+)에는 불용성 전극인 DSA전극을 사용하는 것이 적합하다.In addition, it is suitable to use titanium (Ti) for the negative electrode (-) used in the electrolytic cell in consideration of economy, chemical resistance and durability, and to use the DSA electrode which is an insoluble electrode for the positive electrode (+).
또 전해조의 양극(+)에는 산소기체와 염소기체가 발생되고, 이들 기체는 전극표면에 부착되어 전극면적을 감소시키며 전해액의 저항을 증가시켜 전류효율을 감소시키고, 특히 염소기체는 인체에 유해하고, 부식성으로 인해 설비를 부식시키게 되므로 포집처리 한다.Oxygen gas and chlorine gas are generated at the anode (+) of the electrolytic cell, and these gases are attached to the surface of the electrode to reduce the electrode area and increase the resistance of the electrolyte, thereby reducing the current efficiency. Especially, the chlorine gas is harmful to the human body. In addition, it is corrosive to corrode the equipment, so it should be collected.
이와 같은 방법으로 석출된 니켈은 88∼92%가 회수되었고, 회수된 니켈의 순도는 99.76%의 순도를 유지하게 된다.The nickel precipitated in this manner was recovered from 88 to 92%, and the recovered nickel retained 99.76% purity.
이와 같은 본 발명의 구체적인 실시예는 다음과 같다.Such specific embodiments of the present invention are as follows.
제1공정(침출액의 혼합과 교반)First step (mixing and stirring of leachate)
용기에 니켈폐액(니켈폐액이나 수산니켈슬러지) 1kg과 35% 공업용 염산 350ml 및 용수 1,850ml를 넣고 열판위에 얹어 스틸러(Stirrer)로 200∼300rpm으로 20분간을 교반한다.1kg of nickel waste liquid (nickel waste liquid or nickel sludge sludge), 350 ml of 35% industrial hydrochloric acid, and 1,850 ml of water are added to the vessel and placed on a hot plate and stirred for 20 minutes at 200-300 rpm with a stirrer.
이와 같이 교반된 수산니켈슬러지의 금속 성분을 측정한 바 성분은 아래와 같다.The metal components of the nickel hydroxide sludge stirred as described above were measured.
제2공정(침출액에서의 불순물 제거공정)2nd step (Impuration process of leaching liquid)
제1공정을 거친 용액에 케로센(kerosene)으로 희석시킨 아민계 용매를 상비(유기상/수용액상)를 2.5로 셋팅하고, 진탕기에서 500rpm으로 30초간 교반하고, 추출제 농도는 25%로 셋팅하여 불순물을 제거하고, 유수분리기로 유분을 제거한 니켈수용액을 조성한다.The amine solvent diluted with kerosene in the solution after the first step was set to 2.5 in normal ratio (organic / aqueous phase), stirred at 500 rpm in a shaker for 30 seconds, and the concentration of the extractant was set to 25%. Impurities are removed to form an aqueous nickel solution from which oil is removed using an oil / water separator.
여기에서 용매에 의한 불순물이 제거된 니켈수용액의 성분은 아래와 같다.Herein, the components of the nickel aqueous solution from which impurities are removed by the solvent are as follows.
(추출단수는 1단과 3단에서 불순물의 농도가 비슷하고, 니켈농도가 3단이 1단보다 작아지므로 1단으로 Fix한다.)(The number of extraction stages is similar to the impurity concentration in the first stage and the third stage, and the nickel concentration is fixed in the first stage because the third stage becomes smaller than the first stage.)
또 불순물을 추출한 유기상을 상비3에서 염산으로 역추출 한 결과는 아래와 같다In addition, the result of back extraction of the organic phase from which impurities were extracted with hydrochloric acid from the standing solution 3 is as follows.
여기에서 실험조건은 상비를 제외하고, 추출조건은 위와 같이 한다.Here, the experimental conditions are the same as above except for the normal condition.
위의 실험결과에서 용매의 PH가 4이고, 5단과 6단의 파라메터(Parameter)조건이 비슷하므로 5단으로 Fix하면 된다.In the above experimental results, since the pH of the solvent is 4 and the parameter conditions of the 5th and 6th stages are similar, fix them to the 5th stage.
위의 조건에서 상비를 1로 셋팅하면 분리시간이 10분을 경과하므로 단의 크기는 커지고, 투자비와 용매소모가 커지게 되어 원가비용이 높아지게 된다.If the standing ratio is set to 1 under the above conditions, the separation time is 10 minutes, so the size of the stage is increased, the investment cost and solvent consumption are increased, resulting in high cost.
또 슬러지 상태의 성분과 용매에 의한 불순물을 제거하였을때 제거율을 보면 아래와 같다.In addition, the removal rate when the impurities in the sludge and the solvent are removed is as follows.
위 표에서 보면 철(Fe), 크롬(Cr), 아연(Zn)의 경우 99.8%이상, 구리(Cu)의 경우 96.5%, 코발트(Co) 71.7%, 마그네슘(Mg), 망간(Mn), 나트륨(Na), 납(Pb)의 경우 10∼30%가 제거되고, 니켈(Ni)은 7% 미만이 된다.In the table above, more than 99.8% for iron (Fe), chromium (Cr), zinc (Zn), 96.5% for copper (Cu), 71.7% cobalt (Co), magnesium (Mg), manganese (Mn), In the case of sodium (Na) and lead (Pb), 10 to 30% is removed, and nickel (Ni) is less than 7%.
제3공정(전기분해)Third process (electrolysis)
제2공정의 니켈수용액 1ℓ를 니켈농도 40,000ppm, 전류밀도 1.5A/d㎡, 액온도 35℃ 에서 7시간의 전해반응후 수용액에 잔존하는 니켈의 농도는 950ppm이고, 초기반응은 급격하게 전기분해가 진행되고, 농도가 엷어질수록 반응률이 저하되어 1,000ppm에서는 급속히 저하되었고, 여기에서 석출된 니켈판의 순도는 아래표와 같다.After 1 hour of electrolytic reaction of 1 liter of aqueous nickel solution in the second process with a nickel concentration of 40,000 ppm, a current density of 1.5 A / dm 2, and a liquid temperature of 35 ° C., the concentration of nickel remaining in the aqueous solution was 950 ppm, and the initial reaction rapidly electrolyzed. Progressed, the thinner the concentration, the lower the reaction rate and rapidly decreased at 1,000 ppm, and the purity of the nickel plate deposited therein is shown in the following table.
위에서와 같이 니켈의 회수율은 니켈폐액에 잔존하는 니켈은 불순물 제거 공정에서 6∼8%와, 전기분해 완료후에 잔존하는 2∼4%를 합하면 8∼12%가 제외된 92∼88%가 회수되고, 니켈의 순도는 99.76%가 된다.As described above, the recovery rate of nickel is 92 to 88%, excluding 8 to 12%, when 6 to 8% of nickel remaining in the nickel waste liquid is added to the impurities removal process and 2 to 4% remaining after the electrolysis is completed. , The purity of nickel is 99.76%.
위의 공정에서 니켈전착을 최대화 하기 위해서는 전류밀도(A/d㎡) 니켈농도(ppm)의 최적범위를 찾아야 되므로, 전해조에서 니켈수용액을 4,000ppm, 10,000ppm, 20,000ppm으로 희석하고, 60,000ppm으로 농축액 1.5A/d㎡의 전류밀도로 하여 전해조에서 단위 시간당 니켈 석출량을 산출하고 40,000ppm에서 전류밀도를 변경하여 아래와 같은 결과를 산출하였다.In order to maximize the electrodeposition of nickel in the above process, it is necessary to find the optimum range of the current density (A / dm 2) nickel concentration (ppm). In the electrolyzer, dilute the aqueous nickel solution to 4,000ppm, 10,000ppm, 20,000ppm, and to 60,000ppm. The amount of nickel precipitated per unit time in the electrolytic cell was calculated with a current density of 1.5 A / dm 2, and the current density was changed at 40,000 ppm to obtain the following results.
_
위표에서 보는 바와 같이 니켈 전착을 최대화 하기 위해서는 전류밀도(A/d㎡)는 클수록 유리하고, 니켈농도(ppm)는 40,000ppm에서 최대값이 나타나고 석출효율이 최대치를 나타내고 있다.As shown in the above table, in order to maximize nickel electrodeposition, the larger the current density (A / dm 2), the better, and the nickel concentration (ppm) shows the maximum value at 40,000 ppm and the precipitation efficiency is the maximum value.
이와 같은 본 발명은 니켈폐액 또는 수산니켈슬러지를 염산과 혼합 교반하고, 케로센(kerosene)으로 희석시킨 아민계 용매로 불순물을 제거시킨 다음 유수분리시킨 후 니켈수용액을 일반적으로 활용하고 있는 전기분해 방식을 통하여 니켈판을 석출하게 되므로서 2차 오염과 공침이 없는 순도가 높은 니켈을 회수할 수 있게 된다.The present invention is an electrolysis method in which a nickel waste solution or a nickel hydroxide sludge is mixed and stirred with hydrochloric acid, and an impurity is removed with an amine solvent diluted with kerosene, followed by oil and water separation. Since the nickel plate is precipitated through, it is possible to recover high purity nickel without secondary contamination and coprecipitation.
따라서 이상과 같은 본 발명은 니켈가공공정과 니켈도금공정에서 발생되는 니켈폐액과 수산니켈슬러지의 산업폐기물에서 니켈을 효율적으로 석출하여 자원소재로 재활용하고, 니켈이 제거된 폐용수는 정화처리를 효율적으로 수행할 수 있게 된다. Therefore, the present invention as described above efficiently precipitates nickel in industrial wastes of nickel waste liquid and nickel hydroxide sludge generated in the nickel processing process and nickel plating process, and recycles it as a resource material. It can be done with
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| KR20200013524A (en) | 2018-07-30 | 2020-02-07 | (주)에코프로지이엠 | Apparatus and method for manufacturing high pure metal sulfate for production of cathode active material precursor for lithium secondary battery |
| KR20220000622A (en) * | 2020-06-26 | 2022-01-04 | 주식회사 가온기술 | Highly purified metal nickel powder manufactured by electrochemical cleaning and method of manufacturing the same |
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| KR100912522B1 (en) * | 2007-11-08 | 2009-08-18 | 재단법인 포항산업과학연구원 | Ferronickel Mass and Method for Manufacturing the Ferronickel Mass |
| JP5133403B2 (en) | 2007-05-15 | 2013-01-30 | リサーチ インスティチュート オブ インダストリアル サイエンス アンド テクノロジー | Method for producing Fe, Ni-containing raw material, ferronickel mass using the Fe, Ni-containing raw material, and method for producing the same |
| WO2018043773A1 (en) * | 2016-08-29 | 2018-03-08 | 동국대학교 경주캠퍼스 산학협력단 | Technique for removing and controlling heavy metal by means of electrolysis |
| CN111875124B (en) * | 2020-06-05 | 2022-11-25 | 中船(邯郸)派瑞特种气体股份有限公司 | Treatment method of nickel-containing waste residue wastewater generated in nitrogen trifluoride preparation process |
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| KR19990045359A (en) * | 1997-11-18 | 1999-06-25 | 나가시마 카쭈시게 | High purity nickel production method and high purity nickel material for thin film type |
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| KR20220000622A (en) * | 2020-06-26 | 2022-01-04 | 주식회사 가온기술 | Highly purified metal nickel powder manufactured by electrochemical cleaning and method of manufacturing the same |
| KR102645124B1 (en) * | 2020-06-26 | 2024-03-08 | (주)에프엠 | Highly purified metal nickel powder manufactured by electrochemical cleaning and method of manufacturing the same |
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