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WO2021137721A1 - Procédé de séparation de ni-63 à partir d'une cible éclairée, et de sa purification pour éliminer les impuretés - Google Patents

Procédé de séparation de ni-63 à partir d'une cible éclairée, et de sa purification pour éliminer les impuretés Download PDF

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Publication number
WO2021137721A1
WO2021137721A1 PCT/RU2020/000553 RU2020000553W WO2021137721A1 WO 2021137721 A1 WO2021137721 A1 WO 2021137721A1 RU 2020000553 W RU2020000553 W RU 2020000553W WO 2021137721 A1 WO2021137721 A1 WO 2021137721A1
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WO
WIPO (PCT)
Prior art keywords
solution
nickel
impurities
cobalt
precipitated
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/RU2020/000553
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English (en)
Russian (ru)
Inventor
Павел Сергеевич БУТКАЛЮК
Ирина Львовна БУТКАЛЮК
Александр Степанович КОРНИЛОВ
Евгения Валерьевна ЧЕРНООКАЯ
Валерий Алексеевич ДИТЯТКИН
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Research Institute Of Nuclear Reactors State Scientific Centre Joint Stock Co
Original Assignee
Research Institute Of Nuclear Reactors State Scientific Centre Joint Stock Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
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Application filed by Research Institute Of Nuclear Reactors State Scientific Centre Joint Stock Co filed Critical Research Institute Of Nuclear Reactors State Scientific Centre Joint Stock Co
Publication of WO2021137721A1 publication Critical patent/WO2021137721A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • GPHYSICS
    • G21NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21GCONVERSION OF CHEMICAL ELEMENTS; RADIOACTIVE SOURCES
    • G21G4/00Radioactive sources

Definitions

  • the invention relates to the field of radiochemistry and can be used in analytical chemistry, technology for the isolation and purification of the preparation of the radionuclide Ni-63 and the isolation and purification of nickel from industrial waste.
  • the solubility of nickel chloride in 12 mol / L HC1 is 3.7 g / L, and 2.7 liters of HC1 solution are needed to dissolve a reactor target containing 10 g of nickel. Accordingly, in order to process large quantities of nickel, it is necessary to proportionally increase the volume of hydrochloric acid. The use of hydrochloric acid leads to corrosion of expensive equipment for handling radioactive substances.
  • Ni-63 is the coprecipitation of impurities with iron (III) hydroxide and the subsequent precipitation of hexammininickel perchlorate [Andreev OI, Kornilov AS, Filimonov V.T. Method of purification of the preparation of radionuclide nickel-63, RF patent N ° 2219133 dated 20.12.2003.].
  • the solution is separated from the Fe (OH) precipitate.
  • Ni-63 is precipitated from the filtrate in the form of hexammininickel perchlorate.
  • sodium or ammonium perchlorate is introduced at a ratio of molar concentrations of perchlorate ions and nickel in the range of 10-20. Separate the mother liquor from the sediment. The precipitate is washed with a solution containing ammonia (at least 4 mol / l), perchlorate ions (0.5-2 mol / l) and hydrogen peroxide 0.01-0.1 mol / l. The precipitate is dissolved in nitric acid with a concentration of 0.5-2 mol / l at a molar ratio of the amounts of acid and nickel of 8-10. From the resulting solution, the Ni-63 radionuclide is sorbed on a strongly acidic cation exchanger Dowex-50.
  • the sorbent is sequentially washed with water and a solution of hydrochloric acid with a concentration of 0.3-0.5 mol / l.
  • the method allows to purify Ni-63 from radioactive isotopes of cobalt, cesium, barium, europium, cerium, ruthenium, iodine, silver, niobium, chromium, manganese. This method has its drawbacks.
  • the task of the proposed technical solution is to separate and purify large amounts of Ni (tens of grams) from impurities: Fe-59, Co-60, Cr-51, Mn-54, Sb-124, Sc-46, Sn-117, Zn-65 from targets.
  • cobalt (II) is oxidized to cobalt (III) hydroxide.
  • the molar ratio of persulfate ions to cobalt is at least 15.
  • the pH of the solution is maintained in the 5-He range by introducing calcium carbonate.
  • the molar ratio of calcium carbonate to sodium or potassium persulfate must be at least 2.
  • Zinc fluoride is precipitated from an aqueous-alcoholic solution under conditions of partial precipitation of nickel fluoride, which is a non-isotopic carrier for zinc fluoride.
  • the molar ratio of PSA / CaCO 3 should be no more than 0.5.
  • ethyl alcohol as a salting-out agent leads to a decrease in the solubility of most inorganic compounds.
  • Tables 1-2 show the data on the distribution of zinc between the fluoride precipitate and the solution during the deposition of Z11F2 with a support and without a support, depending on the concentration of alcohol and the initial concentration of nickel.
  • the distribution of zinc was estimated by the factor of purification of nickel from zinc - the ratio of the initial content of zinc in nickel to the final one.
  • the precipitate is dissolved in nitric acid, evaporated to salts, and dissolved in water to obtain a solution with a nickel concentration of 10 g / l.
  • Inactive zinc is added to this solution and zinc fluoride is precipitated from a 30-50% alcohol solution.
  • Nickel losses in this case will not exceed 12% (table 1).
  • the purified nickel mother liquor is added to the first mother liquor. The total nickel losses are 2-3%.
  • the precipitate was separated from the mother liquor by filtration, washed twice with 70 ml of 50% alcohol. The washings were added to the mother liquor and mixed with the first precipitation mother liquor. The combined mother liquor was evaporated to 300 ml, the nickel content and the activity of impurity radionuclides were determined.
  • the nickel content in the combined mother liquor was 14.7 g, the weight of the metallic nickel powder was 14.4 g, and the nickel yield was 96%.
  • the factor of purification from the most significant radionuclides Co-60, Fe-59, Zn-65, Sb-124 is at least 1500, which makes it possible to obtain a preparation of the radionuclide Ni-63 with the total activity of gamma impurities to the preparation no more than 1-10% of the activity of Ni-63.
  • Table 1 Deposition of ZnF 2 without support. Dependence of the degree of deposition of NiF 2 and the degree of purification of nickel from zinc on the concentration of alcohol and the initial concentration of nickel.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

L'invention se rapporte au domaine de la radiochimie et peut être utilisée en chimie analytique, dans les techniques de séparation et de purification d'une préparation de radionucléides de Ni-63 et dans la séparation et la purification de nickel à partir de déchets industriels. Le but de la présente invention est de séparer et de purifier de grandes quantités de Ni-63 (dizaines de grammes) et d'éliminer les impuretés: Fe-59, Со-60, Cr-51, Mn-54, Sb-124, Sc-46, Sn-117, Zn-65 depuis des cibles. La purification du radionucléide cible pour éliminer les Fe-59, Со-60, Cr-51, Mn-54, Sb-124, Sc-46, Sn-117 se fait par précipitation desdites impuretés à un pH =5-6 après dilution isotopique avec du cobalt inactif et une oxydation de ce dernier par du persulfate de potassium ou de sodium. La valeur donnée du pH est maintenue en ajoutant à la solution des carbonates insolubles de calcium et de baryum.
PCT/RU2020/000553 2019-12-30 2020-10-19 Procédé de séparation de ni-63 à partir d'une cible éclairée, et de sa purification pour éliminer les impuretés Ceased WO2021137721A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2019145013 2019-12-30
RU2019145013A RU2720703C1 (ru) 2019-12-30 2019-12-30 Способ выделения Ni-63 из облученной мишени и очистки его от примесей

Publications (1)

Publication Number Publication Date
WO2021137721A1 true WO2021137721A1 (fr) 2021-07-08

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PCT/RU2020/000553 Ceased WO2021137721A1 (fr) 2019-12-30 2020-10-19 Procédé de séparation de ni-63 à partir d'une cible éclairée, et de sa purification pour éliminer les impuretés

Country Status (2)

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RU (1) RU2720703C1 (fr)
WO (1) WO2021137721A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5571308A (en) * 1995-07-17 1996-11-05 Bhp Minerals International Inc. Method for recovering nickel from high magnesium-containing Ni-Fe-Mg lateritic ore
RU2219133C1 (ru) * 2002-04-22 2003-12-20 Федеральное государственное унитарное предприятие Государственный научный центр РФ Научно-исследовательский институт атомных реакторов Способ очистки препарата радионуклида никеля-63
RU2328537C2 (ru) * 2006-05-02 2008-07-10 Общество с ограниченной ответственностью "Институт Гипроникель" Способ осаждения никеля, кобальта и меди селективно от цинка из сульфатных растворов в виде сульфидов
RU2654535C1 (ru) * 2017-08-14 2018-05-21 Федеральное государственное унитарное предприятие "Горно-химический комбинат" (ФГУП "ГХК") Способ получения радионуклида никель-63

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2312908C2 (ru) * 2003-04-02 2007-12-20 Константин Сергеевич Фокин Способ извлечения цветных, редких и благородных металлов из упорного минерального сырья
RU2313149C1 (ru) * 2006-06-20 2007-12-20 Федеральное государственное учреждение Российский научный центр "Курчатовский институт" Способ получения радионуклида никель-63
CN103069500B (zh) * 2010-03-10 2016-10-12 南非核能有限公司 生产放射性核素的方法
RU2569543C1 (ru) * 2014-07-08 2015-11-27 Федеральное государственное унитарное предприятие "Горно-химический комбинат" Способ получения радионуклида никель-63 для бета-вольтаических источников тока
RU2629014C2 (ru) * 2015-12-31 2017-08-24 Федеральное государственное унитарное предприятие "Производственное объединение "Маяк" Способ получения радионуклида никель-63

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5571308A (en) * 1995-07-17 1996-11-05 Bhp Minerals International Inc. Method for recovering nickel from high magnesium-containing Ni-Fe-Mg lateritic ore
RU2219133C1 (ru) * 2002-04-22 2003-12-20 Федеральное государственное унитарное предприятие Государственный научный центр РФ Научно-исследовательский институт атомных реакторов Способ очистки препарата радионуклида никеля-63
RU2328537C2 (ru) * 2006-05-02 2008-07-10 Общество с ограниченной ответственностью "Институт Гипроникель" Способ осаждения никеля, кобальта и меди селективно от цинка из сульфатных растворов в виде сульфидов
RU2654535C1 (ru) * 2017-08-14 2018-05-21 Федеральное государственное унитарное предприятие "Горно-химический комбинат" (ФГУП "ГХК") Способ получения радионуклида никель-63

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