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Removal of Technetium Impurities from Uranium Hexafluoride

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Removal of Technetium Impurities from Uranium Hexafluoride (19) & (11) EP 0 984 903 B1 (12) EUROPEAN PATENT SPECIFICATION (45) Date of publication and mention (51) Int Cl.: of the grant of the patent: C01G 43/06 (2006.01) G21F 9/00 (2006.01) 01.02.2012 Bulletin 2012/05 G21F 9/02 (2006.01) G21F 9/12 (2006.01) (21) Application number: 98915443.0 (86) International application number: PCT/US1998/007163 (22) Date of filing: 09.04.1998 (87) International publication number: WO 1998/052872 (26.11.1998 Gazette 1998/47) (54) REMOVAL OF TECHNETIUM IMPURITIES FROM URANIUM HEXAFLUORIDE ENTFERNUNG VON TECHNETIUMKONTAMINANTEN AUS URANHEXAFLUORID EXTRACTION D’IMPURETES DE TECHNETIUM D’HEXAFLUORURE D’URANIUM (84) Designated Contracting States: (56) References cited: DE FR GB US-A- 3 165 376 US-A- 3 806 579 US-A- 3 848 048 US-A- 5 613 186 (30) Priority: 21.05.1997 US 860000 • SMILEY S H ET AL: "REMOVAL OF IMPURITIES (43) Date of publication of application: FROM URANIUM HEXAFLUORIDE BY 15.03.2000 Bulletin 2000/11 SELECTIVE SORPTION TECHNIQUES" TRANSACTIONS OF THE AMERICAN NUCLEAR (73) Proprietor: United States Enrichment Corporation SOCIETY, AMERICAN NUCLEAR SOCIETY, LA Bethesda, MD 20817 (US) GRANGE PARK, IL, US, 5 November 1967 (1967-11-05), page 507, XP002910084 ISSN: (72) Inventors: 0003-018X • SARACENO, Anthony, J. • SMILEY S.H. et al., "Removal of Impurities from Waverly, OH 45690 (US) Uranium Hexafluoride by Selective Sorption • BANKS, Keith, D. Techniques", TRANSACTION OF THE Lucasville, OH 45648 (US) AMERICAN NUCLEAR SOCIETY, November 1967, page 507, XP002910084 (74) Representative: Beacham, Annabel Rose et al • MILFORDR.P., "Engineering Design of Oak Ridge Dehns Fluoride Volatility Pilot Plant", INDUSTRIAL AND St Bride’s House ENGINEERING CHEMISTRY, 1958, Vol. 50, No. 2, 10 Salisbury Square pages 187-191, XP002910085 London EC4Y 8JD (GB) Note: Within nine months of the publication of the mention of the grant of the European patent in the European Patent Bulletin, any person may give notice to the European Patent Office of opposition to that patent, in accordance with the Implementing Regulations. Notice of opposition shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention). EP 0 984 903 B1 Printed by Jouve, 75001 PARIS (FR) EP 0 984 903 B1 Description [0001] This invention was made with Government support under Contract No. USEC-96-C-0001, awarded to the United States Enrichment Corporation. The Government has certain rights in this invention. 5 FIELD OF THE INVENTION [0002] The present invention relates to methods of purifying uranium hexafluoride by removing technetium-99 impu- rities. 10 BACKGROUND OF THE INVENTION 99 [0003] Technetium-99 ( Tc) is a contaminant that is typically present in an enriched UF 6 product in low concentrations. This contaminant originates from the fission of 235uranium and is contained in reactor return uranium. Process equipment 15 99 surfaces in gaseous diffusion plants which process UF6 hold the Tc as one or more volatile compounds which are slowly released over time. As a result, the enriched UF6 product which is withdrawn from diffusion plants invariably contains low concentrations of 99Tc, due to a slow leaching from equipment surfaces. The concentrations of the99Tc impurity, although low, may easily exceed product specification limits, making the uranium hexafluoride product unac- 99 23S ceptable to fuel fabricators. Presently, the specification limit for Tc in UF6 product is only 0.2 Pg/g U or, assuming 20 5% 235U enrichment, 0.010 Pg 99Tc/g U (0.010 ppm, U basis). 99 [0004] Methods for the removal of Tc from UF6 have typically involved gas phase operation (contacting gaseous 99 UF6 with a metal fluoride, typically magnesium fluoride adsorbent). These methods are not effective at the lowTc concentrations which impact customer acceptance. For example, the lowest concentrations amenable to gas phase removal are above 0.1 Pg 99Tc/g U. Additionally, sufficient throughput must be maintained to provide adequate quantities 25 of the purified UF6. The throughput for UF6 processing which can be obtained with gas phase operations is only about 2 99 100-500 lbs/ft /hour- If the gas velocity is increased to increase UF 6 processing rates, Tc removal efficiency decreases sharply. Conversely, if gas velocity is decreased to maintain high 99Tc removal, processing rates suffer. In short, existing 99 methods (gaseous UF6 with MgF2 adsorbent) are insufficient to combine both high removal efficiency of Tc for direct control at concentrations applicable to market acceptance, and high UP6 processing rates to produce an economic 30 process without burdensome equipment size. [0005] US 3,165,376 discloses a process for the separation and recovery of technetium and nepturium fluorides from reprocessed UF6. [0006] What is needed in the art are new methods of removing 99Tc from uranium hexafluoride which overcome the problems associated with existing methods. The present invention provides such processes. 35 SUMMARY OF THE INVENTION [0007] The present invention provides processes according to claim 1 for the removal of technetium from contaminated uranium hexafluoride containing technetium, typically technetium-99 which is present in several chemical forms or 40 compounds. Some common volatile forms are pertechnetyl fluoride (TcO3F), technetium hexafluoride (TcF6) and tech- netium oxytetrafluoride (TcOF4). Less volatile forms of technetium include TCO 2 and TcF4 or TcF5. Volatility is a relative 99 property and depends upon the temperature of the process. It is generally the Tc compounds which are volatile at UF 6 handling temperatures that are present in the UF6 product. [0008] The processes of the present invention involve: 45 a) contacting contaminated uranium hexafluoride in liquid form with a solid metal fluoride, typically magnesium fluoride (MgF2), for a period of time sufficient for the technetium to become adsorbed onto the metal fluoride solid 2 thereby producing a purified uranium hexafluoride liquid wherein the rate of UF 6 processing is at least 2440 kg/m / hour (500 lbs/ft2/hour) ; and 50 b) removing the purified uranium hexafluoride liquid from the solid metal fluoride, typically magnesium fluoride solid, having adsorbed technetium. BRIEF DESCRIPTION OF THE DRAWINGS 55 [0009] Figure 1 illustrates a UF6 cylinder "1S" which is used in the Examples. Figure 2 shows a liquid UF6 filtering apparatus containing 8-12 mesh MgF2 as an adsorbent and a 10 micron filter. 2 EP 0 984 903 B1 Figure 3 illustrates a vacuum manifold system for filtering liquid UF6 and trapping the purified UF6 in a cooled collection vessel. DETAILED DESCRIPTION OF THE INVENTION 5 [0010] This invention disclosure describes a process modification which leads to unexpectedly large improvement in 99 99 the removal of Tc from UF 6. The process reduces Tc in UF6 to below product specification levels for UF 6 and further 99 provides high UF6 throughputs. The methods described herein can be applied to control the removal of Tc at UF6 product withdrawal stations and/or UF6 liquid transfer facilities on a scale that is attractive for installation at uranium 10 enrichment plants. [0011] As noted in the Background, existing technology employs magnesium fluoride (MgF2) in the form of pellets which are placed in a reactor. Uranium hexafluoride is passed through the reactor in the gas phase at atmospheric pressures or less. Gas chase operation in itself is inherently limiting in UF 6 throughputs or processing rates. Furthermore, this mode of operation fails to perform efficiently as99Tc concentrations decrease. The lower concentration limit for 15 useful removal and/or control of99Tc varies with gas velocity and is estimated to be above 0.1P g/g U and probably much higher. (A typical result in gas phase operation at 13.8 kPa (2 psia) is 2.2 Pg/g being reduced by 59% to 0.9 Pg/g). 2 2 It is not possible to obtain UF 6 processing rates above about 2440 kg/m /hour (500 lbs/ft /hour) at atmospheric pressure or below and still achieve acceptable reduction at concentration below 0.1 Pg/g U. [0012] The present invention is based on the surprising discovery that when liquid UF6 (rather than gaseous UF6) is 20 99 99 passed through a trap containing solid MgF2, a remarkable boost in Tc removal efficiency is realized at low Tc concentrations. As one example, at an initial concentration 0.018P g/g U, 99Tc is reduced to 0.0008 Pg/g U. In other demonstration tests, reductions to below the detection limit (0.0004 Pg/g U) are readily obtained. These high efficiencies were not expected considering the state of the art for MgF 2 trapping technology. Furthermore, UF 6 processing rates are 2 2 2 well over 14650 kg/m/hour (3000 lbs/ft2 /hour). Rates as high as 22460 kg/m/hour(4600 lbs/fts /hour) have been 25 successfully demonstrated with no apparent decrease in efficiency. These rates have considerable economic impact as 99 it is now feasible to install a reasonably sized Tc removal apparatus at any existing product withdrawal station or UF 6 99 liquid transfer facility without significantly interfering with present operations. Accordingly, direct control of Tc in UF6 product is possible and results in further cost savings due to greater flexibility of diffusion operations. The highly purified UF6 product which is obtained using the methods herein, further assures customer acceptance of the UF6 product. 30 Embodiments of the Invention [0013] In view of the above surprising discovery, the present invention provides a process for removal of technetium (99Tc), from contaminated enriched uranium hexafluoride which is withdrawn from a diffusion plant containing the tech- 35 netium. This process comprises: (a) contacting the contaminated uranium hexafluoride in liquid form with a metal fluoride in solid form for a period of time sufficient for the technetium to become adsorbed onto the metal fluoride thereby producing a purified uranium 2 2 hexafluoride liquid, wherein the rate of UF6 processing is at least 2440 kg/m /hour (500 lbs/ft /hour); and 40 b) removing the purified uranium hexafluoride liquid from the aolid metal fluoride having adsorbed technetium.
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