279 1 - , 2 "Ta Emil 1 re L ORNL UNCLASSIFIED . . 1 M 14 Lumi T :1..."M! WWW 174 IV. . LL SS - - - - - SEP2 II DRNL-P.279 CONF-571-11 MASTER VOLATILIZATION OF URANIUM AS THE HEXAFLUORIDE FROM DROPS OF MOLTEN FLUORIDE SALT* . . . . . . . . . . . - : -.- Nearly complete volatilization of uranium from molten fluoride salt droplets 100 u in diameter is possible with a 3-sec exposure to fluorine at 600°C. J. C. Mailen Oak Ridge National Laboratory Oak Ridge, Tennessee -LEGAL NOTICE -- The report *mapan muno a Owen n withWhat the word wete, worawan , mr my own with a b ath Owen was A. Kiwy warray armpito son, der lethed, march to any mney, w p , or waters of the information cout.ned in to repert, or that the wo nog weathen, wenn man w mom dechondo waport my w mong 1. As my Westies no repet tema de for m aty treat wowote, warum, med et mon denied womporta M wand was the women person acties on Mall of the Common" methane meny ma. moyens e motrat a C , * plyn wool contrast, the water that mel para o contractor of the Commi , w wplyw a w ountractor para dennamen, wenn man w, med drugim po Member of our wa he or unin, « We plant ott neutractor. *Research sponsored by the U. S. Atomic Energy Commission under contract with the Union Carbide Corporation. To be presented at the American Chemical Society meeting in Chicago, Illinois, September 2, 1964. - - - - - - MV 1 . . " H*XA tonin- PRESENT FLUORIDE-VOLATILITY PROCESS SATISFACTORY FOR RECOVERING URANIUM The current fluoride-volatility process for recovering uranium from certain spent reactor fuels shows considerable promise as a competitor to aqueous process methods, but it is deficient with respect to recovering plutonium. In the current process, uranium-bearir.g alloy or oxide is dissolved in a suitable molten fluoride salt (the "carrier") by sparging with HF (hydrofluorination), thus converting the uranium to UF. The uranium is then volatilized as the hexafluoride by contacting the melt with elemental fluorine. ",2,3 The carrier salt may consist of NaF, ZrF 4, LiF or others in suitable proportions. Batch sparging of the melt is the normal method for fluorinating the UF4 to produce the volatile compound, UFg. The UF, is then recovered in a sodium fluoride trap or cold trap. As presently operated the fluoride volatility process achieves excellent uranium removal, but has too low a ratio of fluorine flow rate to salt volume to allow rapid plutonium volatilization.“ Under laboratory experimental conditions approximately 20 hr were required to remove 99% of the plutonium where the initial concentration was 2 ppm. AN IMPROVED PROCESS, BASED ON CONTACTING DROPLETS OF FUSED FLUORIDES WITH FLUORINE MAY BE SUITABLE FOR RECOVERING BOTH URANIUM AND PLUTONIUM More rapid removal rates for both uranium and plutonium should be possible with a gas-phase-continuous system, in which falling droplets of the fused salt are contacted by an upflowing stream of fluorine at a temperatung above the salt liquidus temperature. Suitable fluorination rates should be attainable because the diffusion distances are short, and the thermodynamic instability of Pufo is decreased by the large excess of fluorine. Additional advantages are: 1. Lower corrosion rate of the containment vessel because its alternating contact with fluorine and molten salt is avoided.' 2. A spray tower, in which the droplets are generated and then contacted with fluorine, is easily adapted to continuous processing. 3. The waste salt is in the form of free-flowing spheres, possibly facilitating disposal (see Fig. 1). OTHERS HAVE STUDIED THIS APPROACH, INDICATING THAT TEMPERATURE AND DROPLET SIZE ARE IMPORTANT J. D. Gabor et al., º of Argonne National Laboratory, performed 'several experiments with a droplet-fluorination apparatus in which molten fluoride salt was sprayed into fluorine held at a temperature below that of the liquidus point of the salt. Relatively poor uranium removals were found, probably due to a combination of effects: the shortness of the time before solidification of the surface of the droplets and the reaction of the uranium hexafluoride with the sodium fluoride of the frozen salt to form complexes, for example, NaF-UF. Some of their temperatures were 20, 100, and 200°C. J. R. Knox, Jr. performed some limited experiments in which he dropped large drops, 2800 u in diameter, through a fluorine-filled column in which the temperature was maintained above the liquidus point of the salt. After collection, the drops were protected from contact with UF, and F, by a blanket of inert gas. Due to the large diameter of the drops the results (4% uranium removal) were inconclusive. SMALL DROPLETS CAN BE FORMED BY MELTING SIZED POWDERS Since large, expensive equipment would be required to study spray systems at the high temperatures required (500-700°C), small drops were obtained by feeding sized powders through a helium-blanketed preheater furnace where they were melted before falling into the fluorination section of the column. Large drops, 3000 u in diameter, were produced directly by means of a high-temperature pipette. - - - - - - VERY RAPID URANIUM REMOVAL IS POSSIBLE IF THE DROPLETS ARE ABOUT 200 J IN DIAMETER Molten salt droplets ranging from 53 to 3200 u in diameter have been fluorinated by dropping them through fluorination columns 28, 44, and 56 in. long. The carrier salt used in this study was 50-50 mole % NaF-ZrF4 containing 2.5, 4, and 9 mole % UFA Fluorination temperatures ranged from 550 to 670°C. Uranium removals better than 99.9% are attainable for droplets smaller than 150 u at the top range of the temperature with a 56-in.-long fluorinator, and such recovery should be possible for 200- droplets at 700°C. APPARATUS AND OPERATION The main parts of the equipment in the apparatus falling-drop fluorinations are shown in Fig. 2 and are as follows: 1. powder feeder (glass), 2. preheater section (nickel), 3. fluorination column (nickel), and 4. salt receiver (stainless steel). et response Auxiliary ports are: 5. gas supplies and regulators, 6. electrical resistance heaters, and 7. trop for F2 and UF 6 The apparatus will be improved, as needed, in future work. The Lengths of the Preheater and Fluorination Sections are Adjustable, Allowing Different Contact Times By changing the position of the gas take-off point, the portions of the column devoted to preheating and fluorinating could be varied, thus allowing the study of different contact times for droplets of various sizes. Experiments were run with fluorination sections that were 28, 44, and 56 in. long. Separate Furnaces Allow Closer Control of the Temperature Since gas streams enter both ends of the column, and since the cool ends act as heat sinks, several separate furnaces are required to partially offset these end effects. In the present equipment, five furnaces with separate Variac controls are used. During ear iy runs, a moveable internal thermocouple was used to measure the temperature at each furnace. This iki - .. temperature was correlated with the wall temperatures at the furnace junctions. Thereafter, . * - . satisfactory internal temperatures were calculated from the wall temperatures. Startup Procedure Before beginning an experiment, the entire column is first flushed with helium for an hour, and then the fluorination section is flushed with fluorine, with an equal volume of helium flowing through the preheater. During the fluorine flush, the column is brought to the operating temperature, 550 to 670°C. During a run, the fluorine and helium flows are kept equal, at 100 or 200 cc/min (STP). Simple Powder Feeder is Made of Glass The powder feeder is shown in Fig. 3. Sized salt powder is fed through the glass salt feeder by turning a nickel helix. This salt powder drops into a centering funnel that admits the powder to the preheater section. A flow of helium through the powder feeder protects it from fluorine and serves as the blanket gas for the preheater section of the column. Frozen Droplets, Collected Under Liquid Fluorocarbon, are Prevented from Sorbing Uranium Hexafluoride After being fluorinated the salt droplets are frozen and must be prevented from sorbing the UF: Gaseous UF, forms double salts with some solid fluorides. An inert-gas blanket or a sufficient countercurrent flow of fluorine are possible sorption preventers, but each has its drawbacks. For example, an inert-gas blanket dilutes the fluorine and creates difficulties in interpreting the data. The use of a large counter- current flow of fluorine would be ideal, but the difficulties in handling large flows of fluorine (excessively large fluorine traps, possibilities of large-scale leaks, etc.) make yet another approach desirable. In this study, the frozen droplets were caught in a chilled (0°C or less) pool of CF. An additional advantage of capturing the droplets in a chilled liquid is that they retain a more nearly spherical shape thus making their separation from any accompanying nickel fluoride scale easier. The fluorination column, made of nickel, corroded slowly, and analysis of the salt required separation of the nickel fluoride scale. The stainless steel collection cup, containing the liquid fluorocarbon, was supported in the base of the column on a stainless steel plate held against the bottom of the column by springs. A seal between the plate and the column was made with Kel-F grease, a waxy chlorofluorocarbon, also characterized by its good resistance to fluorine and UF. The entire plate and the bottom of the column were covered with powdered dry ice to keep the liquid fluorocarbon cool. MECHANISM AND CORRELATION EQUATION It is probable that the complete fluorination of uranium in a molten salt is not simply the result of the reaction between dissolved fluorine and UF4, and the subsequent evolution of UF: Evidence indicates that there are several intermediate oxidation states (between (IV) and (VI)) and interactions among those states. For this reason, diffusion involves the interaction among the several species represented by those oxidation states and the carrying of the fluorine by uranium. This last facet of the mechanism effectively increases the solubility of fluorine in the melt. Since the reactions are so complex and little understood, only semiempirical equations can be written at the present time. Although Gabor et al.° assumed a surface reaction between UF4 and F2 to yield UFG our experimental evidence indicates that F2 enters the drop before reaction occurs. Specifically, we observed decreased pressures in the column immediately after dropping a small amount of powder, indicating that fluorine had been taken up without a balancing release of UF A good correlation of the experimental data can be made using the following equation: c c = 3.81x1027 - 2.88x204 102 TTC 2 . where, Cu = weight fraction of U at time t, w = weight fraction of U at time = 0, t = fluorination time, sec, = droplet diameter, M. T a where = cdjusted absolute fluorination temperature as defined below. = + 273 + 515 the = fluorination temperature, °C, = salt liquidus temperature, °C. to RESULTS OF EXPERIMENTS Experiments have been made with drop diameters ranging between 53 and 3200 M, with fluorination columns 28, 44, and 56 in. long. All runs so far have used, as the carrier salt, a 50-50 mole ratio NaF-ZrF4 salt with UF4 added to produce melts that were 2.5, 4, and 9 mole % in UF4. Results are well Described by the Correlation Equation The results obtained with the 44-in.-long fluorination column are given in Table 1. Table 2 lists liquidus temperatures for the salts. Fluorination times are calculated using drag coefficients by the standard method, and for the sizes reported here are very nearly given by: Table 1. Results of Falling-Drop Fluorinations with 44-in.-long Fluorinator, Showing the Excellent Uranium Removals Which are Possible with Proper Conditions n Time Fluorination Temp. (°C) 556 Initial U Conc (ppm) 83,900 Run 23B *(+ Final u Conc (ppm) 190 ) Droplet- Size Range (u) 63-88 88-105 105-125 125-149 (sec) 6.3 4.7 x 106 290 590 2190 8.64 x 106 8.34 x 106 4.44 x 106 24B 560 84,000 1.9 125-149 149-177 177-210 1650 6980 4500 1.3 0.94 5.93 x 106 2.62 x 106 8.42 x 106 25B 636 84,800 8.95 x 108 63-88 88-105 105-125 125-149 x 108 bWw 2.7 1.65 x 10 1.9 2.04 x 108 26B 636 87,100 105-125 125-149 149-177 177-210 10.3 9.7 179 474 4.82 x 10 1.03 x 108 1.11 x 10° 8.4 x 107 1.3 C.94 27B 559 54,400 202 6.3 63-88 88-105 105-125 125-149 212 3.8 419 4.42 x 109 1.18 x 107 7.42 x 100 5.61 x 100 1724 2.7 1.9 28B 638 51,600 125-149 149-177 177-210 75 126 260 1.9 1.3 0.94 1.33 x 108 1.58 x 108 1.53 x 108 29B 556 170,000 3.8 88-105 105-125 125-149 149-177 1700 2700 9700 1.46 x 106 1.81 x 100 9.72 ^ 105 7.95 x 105 1.9 1.3 21,900 30B 640 186,000 2.7 105-125 125-149 149-177 70 65 162 7.1 x 10'. 1.54 x 108 1.23 x 108 ......... W ...... WW . .... ............. ....... .. " . Table 2. Liquidus Temperatures of Salt Compositions Used" Salt Composition, Molo Percentage of NaF-ZrF4-UF4 Liquidus Temperature, I'm (°C) 48.75 - 48.75 - 2.5 48 - 48 - 4 45.5 - 45.5 - 9 . (1.246 x 10-902 where L is the length of the fluorination section. A plor of the long ofko ( A plot of the log of k = on vs 1/T for this data and for two large drops is given in Fig. 5. Data obtained for other lengths of the fluorinator section appears quite similar to this and is also adequately fitted by the correlation equation. Of particular significance is the fact that, although considerable scatter is present, the data is adequately fitted by the equation over the full ranges of temperature, droplet diameter, and uranium concentration. 99.9% Removal of Uranium is Possible from Droplets Having Diameters up to 235 u Assuming that Eq. (10) is valid, an interesting question is: "What is the maximum diameter from which 99.9% of the uranium can be removed with reasonable operating conditions?" A reasonable maximum fluorination temperature is probably about 700°C. If a 48-48-4 mole % NaF-ZrFc-UF, salt is considered, and if the fluorinator is 60 in. long, the maxir.um diameter of a droplet from which 99.9% of the uranium can be removed in a single pass is 235 H. Data Illustrates the Unwanted Sorption of UFG on Unprotected, Frozen Droplets As mentioned before, the frozen droplets, from which the UF has been removed, must be kept from contacting UFG because it can be sorbed on them and thus lower the removal efficiency. Figure 6 is a plot of the percentage of uranium removal vs droplet diameter for fluorination at about 570°C, using a fluorinator section 56 in. long. The closed points are .. . il 1 for runs in which UF, sorption on the frozen droplets was prevented by a fluorocarbon layer. The open points are for samples caught in a dry cup. One observes significant differences in the two series, which illustrate the importance of preventing contact between frozen salt and gas containing UFg Rosults indicate Process Works well for Uranium Removal All experimental results and the correlation equation indicate a gas-phase-continuous spray column of moderate height would work well for uranium volatilization on a large scale. The Process Also Promising for Removing Plutonium Although no falling-drop runs for volatilizing plutonium have been made, the results obtained when volatilizing plutonium from a molten pool indicate that rapid removal should be possible. The results of molten-pool experiments indicate that, in plutonium removal, an equilibrium condition exists whereby a high concentration of fluorine is necessary to drive the equilibrium toward the formation of Puf.''. Due to the magnitude of the equilibrium constant, contacting the salt with a very large volume of fluorine is required to ensure good recovery of plutonium. If this is true, a gas-phase-continuous column, where the ratio of fluorine to salt is very high, should work well. Possibly the size of the droplets and other conditions may be the same as those needed for removing uranium. Uranium Volatilizes First from Mixtures of Uranium and Plutonium According to experiments in which UFG and PuF are volatilized from a molten pool when a salt containing both UF4 and PuF4 is fluorinated, the uranium is completely volatilized, 2 X __ 2 or nearly so, before the Puf, starts to be removed. This suggests a method for separating uranium from plutonium. The uranium could be volatilized by sparging fluorine through a molten salt pool followed by spray fluorination for plutonium removal. This would circum- vent any problems in the separation of UF, from Pufg Future Work with Molton Fluorides Containing Plutonium and Plutonium-Uranium Tetrafluoridos During fall, 1964, work with plutonium-containing salt and salt that contains both plutonium and uranium will begin. ACKNOWLEDGEMENTS Acknowledgement is due to J. R. Knox, H. F. Soard, and T. E. Crabtree for construction and original operation of the equipment, and to the Analytical Chemistry Division for the many uranium analyses. - .. . - REFERENCES 1. G. I. Cathers, R. L. Jolley, and E. C. Moncrief, "Laboratory Scale Demonstration of the Fused Salt Volatility Process," Nucl. Sci. and Eng. 13, 391-7 (1962). 2. R. P. Milford, "Engineering Design of Oak Ridge Fluoride Volatility Pilot Plant," Ind. Eng. Chem., 50, (2), 187-91 (February 1958). 3. G. I. Cathers, M. R. Bennett, and R. L. Jolley, "The Application of Fused Salt-Fluoride Volatility Processing to Various Reactor Fuels," Nucl. Eng. Symposium Series, Vol. 10, March 1964 (presented at the Alche 54th Annual Meeting, New York, Dec. 3-7, 1961). 4. M. R. Bennett, Oak Ridge National Laboratory, personal communication. 5. A. P. Litman and A. E. Goldman, Corrosion Associated with Fluorination in the Oak Rid;e National Laboratory Fluoride Volatility Process, ORNL-2832 (June 5, 1961). 6. J. D. Gabor, et al., Spray Fluorination of Fused Salt as a Uranium Recovery Process, Chem. Eng. Division, ANL Report 6131, March 1961. 7. G. I. Cathers, M. R. Bennett, and R. L. Jolley, "UFG3NaF Complex Formation and Decomposition," Ind. Eng. Chem. 50, 1709-10 (1958). 8. J. R. Knox, Jr., personal communication. 9. G. I. Cathers, personal communication. 10. R. E. Thoma, Phase Diagrams of Nuclear Reactor Materials, ORNL-2548 (Nov. 20, 1959). Figure 1. Solidified Droplets. The spherical, free-flowing waste salt allows easy handling and disposal.. 事​, 為 ​* ... - | | _ ( * * * A - 23:33 A { WWWWWW | 事 ​TAAA. ?」 ANN 3 全书 ​* ) 小 ​4 ( “ . .. 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S CYCLES X 70 DIVISION INDE IN V.S A KLUFTEL CSSER CO. 358.91 SEMI-LOGARITHMIC O O KES O Dore NO. 4. AIM SEMCO.GRAM PAPER 250 X 110 DIVISIONS : SLAVLDING.MOSS COMIANY KOSION 10. MASS. MADE IN V. S. A. DITATII 11 . . . • • . JALAYA S 2. 2 . la PO E D r et 1: COLLECTED UNDER 21 WACARBON Elemento para o VIJO LLECTED W Dey; Cup win Bikes BESADO pomi vele .... . . . . . . . sport O . . . . U - . O . :.'1 0 O . . . . . :. - : su HEMWED : . . . . . . , . U ' C 1 • 0 . . CO 1 . 931 7.1.1 M I LA! 1 . D U . . to 10 20 30 40 so 60 29 210 211 SA 70 80 90 100 110 120 130 140 150 iboi DreorLET DIAMETER, Michons (4) We DATE FILMED 11/23/164 · LEGAL NOTICE This roport was proparod as an account of Govorament sponsorod work. Noither the United Statos, nor the Commission, nor any person aoting on behall of the Commission: A. Makos any warranty or roprosentation, expressod or impliod, with respect to the accu- racy, completonoss, or usofulnous of the information contained in this report, or that the uso of any information, apparatus, method, or procoss disclosed in this roport may not infringe privately ownod rights; or B. Assumos any liabilitos with rospect to the use of, or for damagos rosulting from the uso of any information, apparatus, motbod, or procesu disclosed in this roport. Ao vsod in tho above, "person aoting on behalf of the Commission" includes any on- ployoo or contractor of the Commission, or omployee of such contractor, to the oxtont that such omployee or contractor of the Commission, or omployeo of such contractor praparos, disseminatos, or provides accOUS to, any information pursuant to als employment or contract with the Commission, or his omployment with such contractor. . . . END .. . .. .