• 제목/요약/키워드: Zirconium recovery

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Recovery of Zirconium and Removal of Uranium from Alloy Waste by Chloride Volatilization Method

  • Sato, Nobuaki;Minami, Ryosuke;Fujino, Takeo;Matsuda, Kenji
    • 대한전자공학회:학술대회논문집
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    • 대한전자공학회 2001년도 The 6th International Symposium of East Asian Resources Recycling Technology
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    • pp.179-182
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    • 2001
  • The chloride volatilization method for the recovery of zirconium and removal of uranium from zirconium containing metallic wastes formed in spent fuel reprocessing was studied using the simulated alloy waste, i.e. the mixture of Zr foil and UO$_2$/U$_3$O$_{8}$ powder. When the simulated waste was heated to react with chlorine gas at 350- l00$0^{\circ}C$, the zirconium metal changed to volatile ZrCl$_4$showing high volatility ratio (Vzr) of 99%. The amount of volatilized uranium increases at higher temperatures causing lowering of decontamination factor (DF) of uranium. This is thought to be caused by the chlorination of UO$_2$ with ZrCl$_4$vapor. The highest DF value of 12.5 was obtained when the reaction temperature was 35$0^{\circ}C$. Addition of 10 vol.% oxygen gas into chlorine gas was effective for suppressing the volatilization of uranium, while the volatilization ratio of zirconium was decreased to 68% with the addition of 20 vol.% oxygen. In the case of the mixture of Zr foil and U$_3$O$_{8}$, the V value of uranium showed minimum (44%) at 40$0^{\circ}C$ with chlorine gas giving the highest DF value 24.3. When the 10 vol.% oxygen was added to chlorine gas, the V value of zirconium decreased to 82% at $600^{\circ}C$, but almost all the uranium volatilized (Vu=99%), which may be caused by the formation of volatile uranium chlorides under oxidative atmosphere.ere.

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폐전자부품에서 유가금속 회수기술 (Recovery of Valuable Metal from e-Wasted Electronic Devices)

  • 김유상
    • 한국표면공학회지
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    • 제49권6호
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    • pp.477-485
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    • 2016
  • As expensive and valuable metals being used in electronic and semiconducting industries are abandoned as industrial wastes after use of them, it is required to recover them from e-wasted electronics parts. Gold which is used for printed circuit boards or electronic equipments, accessories, etc., is one of e-Wasted materials and recently indium, gallium, zirconium, cobalt, molybdenum and lithium are bacome valuable metals to be recovered from the e-wastes. Since the amount of precious metals is now being faced with scarcity, lean too much on area and instability of supply, and industrial demands are rapidly increasing every year, it becomes more important to recover the valuable metals from the industrial wastes. In this review, we introduced technologies and research trend of the recovery processes of valuable metals from the e-wastes in high-tech devices over the world.

The Recovery Phenomena of the Cold Worked Pure Zirconium

  • Jung, Dae-Young;Yoon, Jong-Kyu
    • Nuclear Engineering and Technology
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    • 제7권1호
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    • pp.15-23
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    • 1975
  • 냉간 압축가공한 순수 지르코늄의 회복현상을 X-ray line broadening과 미소경도 (microhardness)를 측정하여 연구하였다. Isochronal 소둔한 결과에서 경도나 X-ray line breadth가 30$0^{\circ}C$이하에서는 감소하지 않는다는 것을 알 수 있었다. 같은 크기의 냉간가공도에서 X-ray line breadth의 회복속도는 경도의 회복속도와 다르게 나타났으며 가공도에 상관없이 X-ray line breadth의 회복에 필요한 활성화 에너지는 경도의 회복에 필요한 활성화 에너지보다 작은 것을 알 수 있었다. 8%, 19%, 28% 냉간가공한 지르코늄에서의 X-ray line breadth의 회복에 필요한 활성화 에너지는 각각 64,800cal/gram atom, 56,400 cal/gram atom, 48,500 cal/gram atom이였으며 경도의 회복에 필요한 활성화 에너지는 72,800 cal/gram atom, 64,300 cal/gram atom, 58,600 cal/gram atom인 것으로 나타났다.

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지르코늄 메조기공 구조체를 이용한 수중의 인 제거 (The Phosphorus Removal from Water by Zirconium Mesoporous Structure)

  • 이병천;이관용;이상협;최용수;박기영
    • 상하수도학회지
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    • 제19권4호
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    • pp.455-461
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    • 2005
  • This study was designed to investigate the fundamental aspects of a possible recovery of phosphorus strategy from wastewater by using the zirconium mesoporous structured materials as a new type of ion exchangers. Zirconium mesoporous structure material was synthesized by hydro-thermal synthesis. The synthesized zirconium mesoporous structure was examined by X-ray diffraction (XRD) and Transmission electron micrograph (TEM). From the results of XRD and TEM, it was found out that hexagonal mesoporous structure, pore size was about $47{\AA}$, was synthesized. Experimental results showed that the complex of zirconium sulfate tetrahydrate and surfactant micelles had very high ability for capture of phosphorus. The amount of phosphate ions exchanged into the solid was as great as 3.4mmol/g-ZS. And the ion exchange reaction was occurred between $PO_4{^{3-}}$ and $SO_4{^{2-}}$ and also between $PO_4{^{3-}}$ and $OH^-$. Therefore, it is possible to get the higher removal efficiency than other ion exchange media and adsorbent.

BaF2 침전 및 불화물 용융염 전해 제련을 통한 폐 산세액 내 지르코늄 회수 (Recovery of Zirconium from Spent Pickling Acid through Precipitation Using BaF2 and Electrowinning in Fluoride Molten Salt)

  • 한슬기;;이영준;최정훈;이종현
    • 한국재료학회지
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    • 제26권12호
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    • pp.681-687
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    • 2016
  • Zirconium(Zr) nuclear fuel cladding tubes are made using a three-time pilgering and annealing process. In order to remove the oxidized layer and impurities on the surface of the tube, a pickling process is required. Zr is dissolved in HF and $HNO_3$ mixed acid during the process and pickling waste acid, including dissolved Zr, is totally discarded after being neutralized. In this study, the waste acid was recycled by adding $BaF_2$, which reacted with the Zr ion involved in the waste acid; $Ba_2ZrF_8$ was subsequently precipitated due to its low solubility in water. It is very difficult to extract zirconium from the as-recovered $Ba_2ZrF_8$ because its melting temperature is $1031^{\circ}C$. Hence, we tried to recover Zr using an electrowinning process with a low temperature molten salt compound that was fabricated by adding $ZrF_4$ to $Ba_2ZrF_8$ to decrease the melting point. Change of the Zr redox potential was observed using cyclic voltammetry; the voltage change of the cell was observed by polarization and chronopotentiometry. The structure of the electrodeposited Zr was analyzed and the electrodeposition characteristics were also evaluated.

Epoxy 및 Siloxane Emulsion 처리가 견직물의 방추성에 미치는 영향 (The Effect of Epoxy and Epoxy-Siloxane Emulsion Treatment on the Anticrease Property of Silk Fabrics)

  • 장병호;신광호;이병학
    • 한국염색가공학회지
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    • 제5권1호
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    • pp.10-18
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    • 1993
  • Epoxy compound was synthesized from bisphellol-A with epichlorophydrine. Epoxy compound and siloxane were emulsified conjugative one or another. The water repellency of silk fabrics was also highly improved by the treatment of epoxy-siloxane mixed emulsions containing stannic chloride and zirconium oxychloride. The maximum wrinkle recovery was obtained from the fabrics treated under the condition 2.5%-epoxy-siloxane emulsion at 16$0^{\circ}C$. The breaking elongation, the reflectance, the tensile strength and the bending properties of silk fabrics were not degraded severely by the treatment of epoxy-siloxane emulsion.

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불화물계 용융염을 이용한 지르코늄 스크랩의 다중전극 전해정련 거동 (Electrorefining Behavior of Zirconium Scrap with Multiple Cathode in Fluoride-Based Molten Salt)

  • 박동재;김승현;박경태;문종한;이혁희;이종현
    • 방사성폐기물학회지
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    • 제13권1호
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    • pp.11-19
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    • 2015
  • 원자력발전소 증설에 따라 핵연료 피복관의 생산량이 증가 할 것으로 예상되며, 튜브 제조 시 발생되는 지르코늄(Zr) 스크랩 역시 증가 할 것으로 판단된다. 지르코늄(Zr) 정련기 대용량화와 회수율 향상을 위한 사전 연구로서 LiF-KF-ZrF4 불화물의 염에서 다전극을 이용하여 전해정련실험을 실시하였다. LiF-KF-ZrF4염에서는 -0.8 V(vs.Ni)에서 환원전위가 관찰되었으며, 분극 거동 관찰 결과 전극의 개수가 증가할수록 셀의 저항이 낮아져 인가전류량이 증가하였다. 6개의 다 전극을 이용하여 정련 실험을 한 결과 가장 낮은 전류밀도인 25.64 mA/cm2조건에서 98%의 회수율로 가장 높은 회수율은 보였다. XRD 및 TG 분석 결과 순수한 Zr이 회수되었으며, ICP 분석결과 양극재의 기본 불순물 함량을 포함한 순도 97.8% 보다 낮은 불순물의 함량을 포함한 순도 99.92%의 Zr을 나타내었다. 폭 20 mm 높이 65 mm의 전극 6개를 사용시 전력소모율은 7.15 kWh/Kg으로 크롤 공정대비 39.7% 전력을 소모하게 된다. 다 전극 사용 시 단일 전극 사용에 비해 인가전류와 셀 효율 및 회수율 증대로 대용량화를 위한 효율적인 기술로 판단된다.

PWR 사용후핵연료 중 Zr 및 Zr 동위원소 정량을 위한 분리 및 정제 (Separation and Purification for the Determination of Zirconium and Its Isotopes in PWR Spent Nuclear Fuels)

  • 김정석;전영신;박용준;이창헌;김원호
    • 분석과학
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    • 제11권6호
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    • pp.421-428
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    • 1998
  • 사용후핵연료의 화학특성을 규명하기 위하여 시료 중에 함유되어 있는 핵분열생성물 중 Zr을 분리, 정제하는 연구를 수행하였다. 우라늄과 핵분열생성물 대신 비방사성 금속이온들로 구성된 사용후핵연료 모의 용해용액을 시료로 사용하였다. 12 M HCl 용액으로 전처리한 Dowex $1{\times}8$ 음이온교환수지관에서 Ce, Nd, Cs, Rb, Ba, Sr, Ru, Rh, Pd, Ag 및 Cd을 용리시킨 후 5 M HCl 용액으로 Zr을 95% 이상 분리, 회수할 수 있었다. 용출액에 함유되어 있는 Zr 동위원소의 동중원소인 Mo을 제거하기 위하여 5 M HCl 용액으로 전처리한 Dowex $1{\times}8$ 음이온교환수지관에서 정제하였으며, 실제 PWR 사용후핵연료에 함유되어 있는 Zr 분리, 정제에 적용하여 질량분석한 결과 Mo 및 Sr에 의한 동중원소 영향이 나타나지 않았다.

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Electrorefining of CuZr Alloy Using Ba2ZrF8-LiF Electrolyte

  • Lee, Seong Hun;Choi, Jeong Hun;Yoo, Bung Uk;Lee, Jong Hyeon
    • 한국재료학회지
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    • 제27권12호
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    • pp.672-678
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    • 2017
  • In the production of zirconium cladding tube, a pickling acid solution is used to remove surface contaminants, which generates tons of pickling acid waste. The waste pickling solution is a valuable resource of Hf-free Zr. Many studies have investigated separating the Hf-free Zr source from the waste pickling acid. The results showed that $Ba_2ZrF_8$ precipitates prepared from the waste pickling acid were useful as an electrolyte for the electrorefining of Zr in molten salt. In the present work, electrorefining was performed in a $Ba_2ZrF_8-LiF$ binary electrolyte to recover Zr from a Hf-free CuZr ingot anode prepared by electroreduction. Before electrorefining, two pretreatments are performed. First, electrolyte melting was carried out to determine the eutectic temperature, and second, the electrolyte was treated to eliminate impurities, mainly hydride. After electrorefining, the cathode deposits were analyzed by $O_2$ gas analyzer and SEM-EDX to explore the possibility of recovering nuclear-grade Zr metal. Moreover, the anode was analyzed by SEM-EDX to determine the Zr dissolution depth.

Study on the Separation of MAs from HLLW and Their Extraction Behavior Using New Extractants of Amido Podand

  • An, Ye-Guo;Luo, Fang-Xiang;Zhu, Zhi-Xuan;Zhang, Xiang-Ye;Zhu, Wen-Bin
    • 한국방사성폐기물학회:학술대회논문집
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    • 한국방사성폐기물학회 2004년도 Proceedings of the 4th Korea-China Joint Workshop on Nuclear Waste Management
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    • pp.245-256
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    • 2004
  • The extraction of three kinds of amido podands, N,N,N'N'-tetrabutyl-3-oxa-pentanedi- amide (TBDGA), N,N,N'N'-tetra-isobutyl-3-oxa-pentanediamide(TiBDGA) and N,N,N'N'-tetra- butyl-3,6-dioxa-oct-anediam- ide(TBDOODA) on U(VI),Pu(IV), Am(III), Eu(III) and other metal ions is studied in nitric acid solutions. 40%octanol-kerosene is chosen as diluents to eliminate third phase and emulsion. TBDGA and TiBDGA show extraction selectivity to An(III) and Ln(III) much higher than to U(VI) and Pu(IV). Fe, Ru and Mo is poorly extracted by the three kinds of amid podands in 2~3mol/L $HNO_3$ solutions. Aiming to eliminate interface crude when using simulated HLLW solution in the system of 0.2mol/L TBDGA/Octanol+kerosene, acetohydroxyamic acid was adapted. Distribution ratio of zirconium was decreased when adding acetohydroxyamic acid in aqueous solution, and interface crude disappeared as mixing extractant with HLLW. The counter-current extraction test is carried out in a set of miniature mixer-settler, with 0.2mol/L TBDGA/ 40% octanol-kerosene as extractant to separate U(VI), Pu(IV), Am(III) and Eu(III) from simulated high level liquid waste(HLLW) solution. In battery A, lanthanides and actinides are coextracted into organic phase with the recovery of 99.98% for U(Ⅵ), >99.99% for Pu(IV), and >99.99% for Am(III) and Eu(III) respectively. In battery R1, 99.99% U, 86.2% Pu and a part of Am or Eu are stripped into aqueous phase by 0.2mol/L acetohydroxyamic acid (AHA) in 0.01mol/L $HNO_3$ solution. In battery $R_2$, Am, Eu and remained Pu are completely back-extracted by 0.2mol/L AHA. This separation process contains no salt reagent, and it is not necessary to dilute HLLW feed.

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