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FCC 폐촉매로부터 Ce , Nd 및 V 의 분리 회수 프로세스
전성균,양종규,김종화,이성식 ( Sung Kyun Jeon,Jong Gyu Yang,Jong Hwa Kim,Sung Sik Lee ) 한국공업화학회 1997 공업화학 Vol.8 No.4
석유화학공업에서 사용된 유동접촉분해(FCC) 폐촉매의 주성분은 Si와 Al이며, 그외에 Fe, Zn, Ti 등의 기본금속과 알칼리금속 및 Ce, Nd, Ni, V 등의 회유금속이 함유되어 있다. 0.25 mol/dm³-H₂SO₄를 침출제로 폐촉매를 침출하였을 때 Ce가 640, Nd가 310, 그리고 V가 450mg/dm³ 함유된 pH 1.0의 침출액을 얻었고, 아미노인산형 킬레이트수지에 의하여 Ce와 Nd를 선택흡착시킨 후, 4.0 mol/dm³-HCl로 용리시켜 1.2g/dm³의 Ce와 0.75 g/dm³의 Nd 농축액을 얻었다. 농축액을 다시 옥살산 침전 및 공기산화법으로 처리하여 Ce와 Nd의 분리가 가능하였으며, 염소이온 공존하에 추출제 TOPO를 이용한 용매추출법으로 V와 AJ을 각각 분리시켜, FCC 폐촉매로부터 순도가 99%인 Ce, Nd 및 V의 분리정제가 가능하였다. The major constituents in spent FCC catalysts are Si, Al, Fe, Ti, alkali metals and some others. The spent catalyst is also composed small amounts of rare metals such as Ce, Nd, Ni and V. The selective adsorption and concentration of Ce and Nd from the leaching solution of spent FCC catalysts with sulfuric acid(0.25mo1/dm³) were carried out by the column method with a chelate resin having a functional group of aminophosphoric acid type. Ce and Nd were separated from eluate liquor containing Al, Nd and V by the precipitation process with oxalic acid. Vanadium is purified from chloride ion coexistance by solvent extraction, employing tri-n-octyl phosphine oxide as extractant with Al in the raffinate solution. Rare metals with the purity of 99 percent were obtained from the spent FCC catalyst.
산 침출액에서 EHPNA 에 의한 코발트와 니켈 금속 이온의 추출평형
양종규,전성균,이성식,강봉근 한국화학공학회 1997 Korean Chemical Engineering Research(HWAHAK KONGHA Vol.35 No.3
산 전해질 용액에 침출된 코발트와 니켈 이온의 추출평형을 구하기 위하여 산 추출제인 EHPNA로써 Co(NO₃)₂-Acids(HCl, H₂SO₄)-H₂O, Ni(NO₃)₂-Acids(HCl, H₂SO₄)H₂O계의 추출평형을 실험하여 총괄추출평형식과 추출평형 상수를 구하였으며 각 금속 이온과 추출제의 복합체는 (CoR₂·2HR) ̄, (NiR₄·4HR) ̄이었다. 금속 추출공정에서 산용액의 열역학적 특성인 활동도를 고려하기 위하여 3성분 전해질 용액으로부터 실험적으로 얻은 equi-a(-H₂O) data로써 용질의 평균활동도 계수값인 γ_±[Co(NO₃)₂], γ_±[Ni(NO₃)₂], γ_±(HCl), γ_±(H₂SO₄)를 Mckay-Perring method로써 구하였다. 평균활동도 계수값은 LogD_M/γ_(±HCl) 와 LogD_M/γ_(±H₂SO₄)의 추출 분배계수 곡선에 영향을 미쳤으며, 산용액의 낮은 농도를 제외하고는 Modified Mckay-perring method에 의한 이론값과 실험값이 가장 잘 일치하였다. Extraction equilibrium formulations were studied for the distribution coefficient of cobalt and nickel ions from acidic leach solutions by using 2-Ethylhexylphosphonic Acid Mono-2-Ethylhexyl Ester(EHPNA) dissolved in n-heptane at 298。K. The extration equilibrium constants, K_(ex) of cobalt and nickel by EHPNA were investigated and they were different from each other that by DEHPA. Complex form of cobalt and nickel in the organic phase was CoR₂·2HR, NiR₂·4HR. With metal extraction processes, considering that the activity is one of the basic parameters in characterizing the solution itself, the mean activity coefficients of solutes, γ_±[Co(NO₃)₂], γ_±[Ni(NO₃)₂], γ_±(HCl), γ_±(H₂SO₄) in aqueous mixed electrolyte solutions were calculated by Mckay-Perring method and its modified form using the equi-water activity data of those solutions experimentally determined. The mean activity coefficients had an effect on extraction curve and experimental results agreed with well those calculated by Modified Mckay-Perring method on extraction profiles except at low acid concentrations.
이성식,양종규 동아대학교 환경문제연구소 1994 硏究報告 Vol.17 No.1
A process for recovery of boron from steelmaking dust in which it exists at very low concentration with a mixture of high concentration of less desirable species was studied. Of the boron contained in, 72% can be leached with 3.0 ㏖/l sodium hydroxide solution. The leached liquor contains aluminum, cupper and zinc in addition to boron. The selective concentration of boron was carried out using a glucamine type chelating resin column, and the eluate containing 1.8g/1 of B was obtained employing EHD (2-ethyl-1, 3-hexanediol) as an extractant. Concentrated boron liquor having 98% purity for borax production was obtained in this process.