[논문]저급 탄산리튬의 재결정화를 통한 고순도 탄산리튬 제조에 대한 연구

김보람; 김대원; 황성옥; 정수훈; 양대훈

doi:10.6111/jkcgct.2021.31.1.016

[국내논문] 저급 탄산리튬의 재결정화를 통한 고순도 탄산리튬 제조에 대한 연구
A study on the fabrication of high purity lithium carbonate by recrystallization of low grade lithium carbonate 원문보기

한국결정성장학회지 = Journal of the Korean crystal growth and crystal technology, v.31 no.1, 2021년, pp.16 - 23

김보람 (고등기술연구원 신소재공정센터) , 김대원 (고등기술연구원 신소재공정센터) , 황성옥 ((주)지엠텍) , 정수훈 ((주)지엠텍) , 양대훈 ((주)지엠텍)

초록
AI-Helper

리튬이차전지 제조 공정 중 발생한 폐액으로부터 회수된 탄산리튬의 경우, 이차전지 양극재의 원료인 코발트, 니켈 및 망간의 중금속이 함유되어 있다. 본 연구에서는 탄산리튬의 재결정화를 통하여 순도 98.28 %의 저급 탄산리튬 분말에 함유된 중금속을 제거하고 탄산리튬의 순도를 높이고자 하였다. 먼저 염산 수용액을 이용하여 탄산리튬의 침출 효율을 살펴보았으며, pH 5 조건으로 침출 후 탄산나트륨의 당량 및 농도의 탄산리튬 재결정에 대한 영향을 확인하였다. 리튬의 함량 기준 대비 탄산나트륨 1 당량에서 1.5로 증가할수록, 농도 1.4 M에서 2.8 M로 증가할수록 회수율은 향상되었으며, 탄산나트륨의 투입 조건이 달라짐에 따라 결정 형상이 달라지는 것을 SEM 분석을 통해 확인할 수 있었다. 재결정된 탄산리튬 분말은 수세하여 순도 99.9 % 이상의 고순도 탄산리튬을 회수할 수 있었다.

Abstract ▼ AI-Helper

Lithium carbonate recovered from the waste solution generated during the lithium secondary battery manufacturing process contains heavy metals such as cobalt, nickel, and manganese. In this study, the recrystallization of lithium carbonate was performed to remove heavy metals contained in the powder and to increase the purity of lithium carbonate. First, the leaching efficiency of lithium carbonate according to pH in the aqueous hydrochloric acid solution was examined, and the effect on the recrystallization of lithium carbonate according to the equivalent and concentration of sodium carbonate was confirmed. As the equivalent and concentration of sodium carbonate increased, the recovery rate of lithium carbonate improved. And the SEM image showed that the crystal shape was changed depending on the reaction conditions with sodium carbonate. Finally, the high purity lithium carbonate of 99.9% or more was recovered by washing with water.

주제어

표/그림 (14)

그림 Fig. 1. XRD patterns of Li₂CO₃ powder.
표 Table 1 Chemical composition of low grade Li₂CO₃ powder (ppm)
그림 Fig. 2. FE-SEM image of Li₂CO₃ powder and corresponding the digital photographs.
그림 Fig. 3. Experimental flow chart for the process of high purity of lower lithium carbonate.
그림 Fig. 4. Leaching rate of low grade Li₂CO₃ powder according to pH.
그림 Fig. 6. FE-SEM image of recrystallized Li₂CO₃ powder according to pH and corresponding the digital photographs.
그림 Fig. 5. XRD pattern of recrystallized Li₂CO₃ powder accord-ing to pH.
표 Table 2 Chemical composition of low-grade Li₂CO₃ leachate (ppm)
그림 Fig. 7. Grade and recovery of recrystallized lithium carbonate according to pH.
표 Table 3 Chemical composition of recrystallized Li₂CO₃ powder (ppm)
그림 Fig. 8. SEM image of recrystallized lithium carbonate powder according to the equivalent and concentration of sodium carbonate.
표 Table 4 Chemical composition of recrystallized Li₂CO₃ powder according to the equivalent and concentration of sodium carbonate (ppm)
표 Table 5 Grade and recovery of lithium carbonate powder recovered according to the equivalent and concentration of sodium carbonate
표 Table 6 Chemical composition of lithium carbonate powder before and after washing with water (ppm)

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