• Title/Summary/Keyword: Raffinate

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High-purity Lithium Carbonate Manufacturing Technology from the Secondary Battery Recycling Waste using D2EHPA + TBP Solvent (이차전지 폐액으로부터 D2EHPA + TBP solvent를 활용한 탄산리튬 제조기술)

  • Dipak Sen;Hee-Yul Yang;Se-Chul Hong
    • Resources Recycling
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    • v.32 no.1
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    • pp.21-32
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    • 2023
  • Because the application of lithium has gradually increased for the production of lithium ion batteries (LIBs), more research studies about recycling using solvent extraction (SX) should focus on Li+ recovery from the waste solution obtained after the removal of the valuable metals nickel, cobalt and manganese (NCM). The raffinate obtained after the removal of NCM metal contains lithium ions and other impurities such as Na ions. In this study, we optimized a selective SX system using di-(2-ethylhexyl) phosphoric acid (D2EHPA) as the extractant and tri-n-butyl phosphate (TBP) as a modifier in kerosene for the recovery of lithium from a waste solution containing lithium and a high concentration of sodium (Li+ = 0.5 ~ 1 wt%, Na+ = 3 ~6.5 wt%). The extraction of lithium was tested in different solvent compositions and the most effective extraction occurred in the solution composed of 20% D2EHPA + 20% TBP + and 60% kerosene. In this SX system with added NaOH for saponification, more than 95% lithium was selectively extracted in four extraction steps using an organic to aqueous ratio of 5:1 and an equilibrium pH of 4 ~ 4.5. Additionally, most of the Na+ (92% by weight) remained in the raffinate. The extracted lithium is stripped using 8 wt% HCl to yield pure lithium chloride with negligible Na content. The lithium chloride is subsequently treated with high purity ammonium bicarbonate to afford lithium carbonate powder. Finally the lithium carbonate is washed with an adequate amount of water to remove trace amounts of sodium resulting in highly pure lithium carbonate powder (purity > 99.2%).

Ionic Liquids as Benign Solvents for the Extraction of Aromatics

  • Hossain, Md. Anwar;Lee, Jee-Sun;Kim, Dai-Hyun;Nguyen, Dinh Quan;Cheong, Min-Serk;Kim, Hoon-Sik
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3241-3247
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    • 2012
  • Ionic liquids (ILs) have been extensively investigated as promising alternatives to conventional organic solvents such as sulfolane and N,N-dimethylformamide for the selective extraction of aromatic hydrocarbons from the $C_6-C_{10}$ hydrocarbon mixtures produced from the cracking processes of naphtha and light oils. The most important advantage of ILs over conventional organic solvents is that they are immiscible with aliphatic hydrocarbons, and thus the back extraction of ILs from the raffinate phases and top hydrocarbon-rich layers is not necessary. In this paper, a brief review on the state of the art in the utilization of ILs for aromatics separation is presented.

Industrial scale extraction and stripping devices for continuous recovery of gallic acid from Chinese nutgall processing wastewater

  • Wu, Yundong;Xia, Xihe;Dong, Shuyu;Zhou, Kanggen
    • Environmental Engineering Research
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    • v.22 no.3
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    • pp.288-293
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    • 2017
  • In this study, we report the industrial application of an efficient technology for the recovery of gallic acid from Chinese nutgall processing wastewater. The recovery of gallic acid by industrial scale extraction and stripping devices was performed, with tributyl phosphate as the extractant and kerosene as the diluent. The results showed that the theoretical extraction stage was four, while the theoretical stripping stage was two. A closed-cycle system was studied for the continuous countercurrent extraction and stripping, with a five-stage extraction device and a three-stage reflux stripping device. The results showed that the multistage extraction-stripping system could steadily run for a long period, the average gallic acid level in the raffinate was $0.85g{\cdot}L^{-1}$, and the gallic acid content recovered in the strip liquor was higher than $120g{\cdot}L^{-1}$. The average extraction yield of gallic acid was 94.14%. When the strip liquor was used as raw material for production, the average production yield increased by 8.64%. In addition, after extraction, the $COD_{Cr}$ in the wastewater decreased by 38.19%, and the biodegradability of wastewater improved by 1.6 times. This study provided a new impetus for the sustainable development of the Chinese nutgall processing industry.

Separation of Amino Acids by Simulated Moving Bed Using Competitive Langmuir Isotherm

  • Yang, Yun-Jeong;Lee, Chong-Ho;Koo, Yoon-Mo
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.9 no.5
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    • pp.331-338
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    • 2004
  • The Separation of two amino acids, phenylalanine and tryptophan, was carried out using laboratory simulated moving bed (SMB) chromatography. The SMB process consisted of four zones, with each zone having 2 columns. The triangle theory was used to obtain the operating conditions for the SMB. The mass transfer coefficients of the two amino acids were obtained from the best-fit values by comparing simulated and experimental pulse data. The competitive adsorption isotherms of the two amino acids were obtained by single and binary frontal analyses, taking into consideration the competition between the two components. A competitive Langmuir isotherm, obtained from single-component frontal chromatography, was used in the first run, and the isotherm from binary frontal chromatography in the second, with the flow rate of zone 1 modified to improve the purity. Compared to the first and second runs, the competitive Langmuir isotherm from the binary frontal chromatography Showed good agreement with the experimental results. Also, adjusting the flow rate in zone 1 increased the purity of the products. The purities of the phenylalanine in the raffinate and the tryptophan in the extract were 99.84 and $99.99\%$, respectively.

Recovery of Nitric Acid and Valuable Metals from Spent Nitric Etching Solutions of Printed Circuit Board

  • Ahn, Jae-Woo;Ahn, Jong-Gwan;Lee, Man-Seung
    • Proceedings of the IEEK Conference
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    • 2001.10a
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    • pp.140-143
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    • 2001
  • A study has been made on the recovery of nitric acid and valuable metals such as Cu, Sn, Pb from the spent nitric etching solutions. The nitric acid was extracted effectively by TBP but the heavy metals such as Fe, Cu, Sn, Pb were not extracted by TBP from the spent nitric etching solutions. From the experimental results, 95% of nitric acid in spent etching solution was extracted at O:A ratio of 3:1 with five stage by 60% TBP and 98% of nitric acid was stripped from the loaded organic phase at O:A ratio of 1:1 with four stages by distilled water. After extracting nitric acid, Cu was recovered as a metal by electrowinning effectively and Sn was successfully removed by precipitation method by adjusting the pH of raffinate solution. Finally, Pb was recovered by cementation with iron scrap at $65^{\circ}C$. Parameters controlling the cementation process, such as temperature, pH and the effect of the additives were investigated.

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Simulation of (R)- and (S)- Ketoprofen Separation in Simulated Moving Bed (SMB) ((R)-케토프로펜과 (S)- 케토프로펜 분리를 위한 유사 이동층 크로마토그래피의 전산모사)

  • Lee, Il Song;Lee, In Su;Kim, In Ho
    • KSBB Journal
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    • v.29 no.4
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    • pp.250-262
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    • 2014
  • A simulation study for finding purity changes of extract and raffinate as well as the best purity of (S)-ketoprofen in simulated moving bed (SMB) was performed with changing parameters of $m_2$ and $m_3$ from triangle theory. Aspen simulator allowed separation process simulation of (R)- and (S)-ketoprofen in SMB and compared 4-bed SMB and 8-bed SMB based on the same Henry constant and mass transfer coefficient. The 4-bed SMB consisted of 4 columns (200 mm of length, 10 mm of diameter) and the 8-bed SMB constructed by 8 columns (100 mm of length, 10 mm of diameter), and therefore total column length was made the same as 800 mm. Considering purities of both (R)-and (S)-ketoprofen, both 4-bed SMB and 8-bed SMB had the best purity when $m_2$ and $m_3$ were on 12.0 and 13.0 in the center of triangle. Taking only (S)-ketoprofen into account, 4-bed SMB as well as 8-bed SMB had the best purity when $m_2$ and $m_3$ were on 10.9 and 12.6 in the left outside triangle, and their purities were 93.3 % for 4-bed SMB and 96.9 % for 8-bed SMB.

Regeneration of $FeCl_3$ from a Spent Etching Solution Containing Nickel by Solvent Extraction (니켈 함유 에칭폐액으로부터 용매추출에 의한 $FeCl_3$의 재생)

  • Lee, Kyoung-Joo;Lee, man-Seung;Oh, Young-Joo
    • Proceedings of the Korean Institute of Resources Recycling Conference
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    • 2004.05a
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    • pp.218-226
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    • 2004
  • Solvent extraction and stripping experiments were conducted to separate iron from a spent $FeCl_3$ etching solution containing nickel. In the extraction, PC88A, MIBK and Alamine336 were tested as an extractant in various diluents. Alamine336 salt in toluene led to the highest extraction percentage of iron. Stripping percentage of iron from the loaded organic by Alamine336 increased with decreasing HCl conentration of stripping solution and with increasing volume ratio of aqueous to organic. In the operation of bench scale mixer-settler, 7 extraction stage with 1.0M Alamine336 salt in toluene and 10 stripping stage with 0.01M HCl solution resulted in a stripped solution with 133g/L of iron and in a raffinate with most of nickel together with a small amount of iron when the flow rate ratio of organic to aqueous was 7.

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Recovery of Copper from Spent Copper Solution of Printed Circuit Board Process by Solvent Extraction Method (인쇄회로기판 제조과정에서 발생되는 동폐액의 용매추출에 의한 재활용)

  • Moon, Young-Hwan
    • Clean Technology
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    • v.2 no.1
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    • pp.47-52
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    • 1996
  • The solvent extraction method was applied on a spent solution containing copper, which was produced in a printed circuit board process, to recover copper and to reuse the etching solution. Lix 64 N ($\alpha$-Hydroxyoxime + $\beta$-Hydroxybenzophenone Oxime) was used as a solvent. The acidic spent copper solution was mixed with and alkaline copper solution to pH=2. The solvent including 30 volume% of Lix 64 N extracted 17.1gr/l of copper from the mixed spent copper solution. In the continuous bench scale experiment, 4 stages for extraction, 2 stages for stripping and 4 stages for washing were used. Recovered copper was recycled as copper sulfate and the raffinate was reused as copper etchant. The percentage of copper recovery and the purity of copper sulfate were higher than 99.9%, respectively.

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Recovery of Pt from the Chloride Leaching Solution of Spent Catalysts by using Column Extractor (폐촉매(廢觸媒) 염산침출액(鹽酸浸出液)에서 컬럼형 추출기(抽出器)에 의한 백금(白金) 회수(回收))

  • Sun, Pan-Pan;Lee, Man-Seung
    • Resources Recycling
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    • v.22 no.6
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    • pp.26-32
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    • 2013
  • In order to recover Pt from the hydrochloric acid leaching solution of spent catalysts, bench scale Karr reciprocating column was employed. At an optimum flow rate and vibration frequency, iron and Pt was completely extracted by using TBP and Aliquat 336. At the same vibration frequency, iron and Pt was completely stripped by HCl and $HClO_4$ after adjusting the flow rate. In the case of extraction of HCl from the raffinate with TEHA, it was difficult to maintain the stability of the column extractor. A comparison of the operation results between column extractor and mixer-settler is reported.

Recovery of Nickel Metal from the Spent FeCl$_3$ Etching Solution by Solvent Extraction and Chemical Reduction (FeCl$_3$ 에칭廢液으로부터 溶媒抽出과 化學沈澱에 의한 니켈金屬 回收)

  • Lee, Man-Seung;Kim, Myoung-Sik
    • Resources Recycling
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    • v.14 no.3
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    • pp.48-54
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    • 2005
  • Solvent extraction and chemical reduction experiments have been performed to separate iron and nickel from a spent FeCl$_3$ etching solution and to recover nickel metal. It was possible to separate iron and nickel by extracting the spent solution with Alamine336. At the O/A ratio of 7:1, iron extraction percentage of 99% was obtained. In the stripping of the loaded organic with 0.01 M HCl solution, iron stripping percentage of 99% was obtained when the A/O ratio was 7:1. When the pH of the raffinate was controlled to be 10.5, nickel metal powder with 99% purity was obtained by using hydrazine as a reducing agent at 100$^{\circ}C$. A process was suggested to recover nickel metal from the spent FeCl$_3$ solution and to regenerate etching solution.