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Á4-2-4-2-2-121Attorney Oct. 23, 1951 F. A. JENKNS 2,572,156 PROCESS OF PRODUCING URANIUM HEXACHLORIDE Filed July 13, 1943 12 2/ To Vacuum Line // Original Charge | Residue UCls INVENTOR. Francis A. Jenkins -á4-2-4-2-2-121ATTORNEY. Patented Oct. 23, 1951 2,572,156 UNITED STATES PATENT of FICE PROCESSES OF PRODUCING URANUM HEXACHORDE Francis A. Jenkins, Berkeley, Calif., assignor to the United States of America as represented by the United States Atomic Energy Commission Application July 13, 1943, Serial No. 494,447 Claims. (CI.23-14.5) 1 The present invention relates to UCls and suitable charge of uranium pentachloride is processes of producing the Same. placed in a substantially conventional molecular Heretofore the compound UCls has not been Still which comprises a hot Surface heated in any known. Moreover, it has been predicted that the Suitable manner, such, for example, as by a hot possibility of its production is virtually negligible Sandbath, and a cold Surface. cooled in any Suit in view of its expected great instability. This able manner, Such, for example, as by liquid air. view is entirely plausible since the tetrahalides In the still the hot surface and the cold surface of uranium form a series decreasing in stability are disposed in Spaced apart relation, and the in a regular-manner-from the fluoride through space therebetween is evacuated to -an-extremely the chloride-and-the-bromide to the iodide, and O low pressure by Suitable vacuum pumping ap since UF6 is... extremely unstable. Thus it has paratus. More particularly, the charge is placed always been assumed that the hexahalide Series on the hot surface of the still and the tempera of uranium terminates abruptly at the COm ture of the sand bath is suitably controlled, in pound UEs, . order that the charge is maintained at a tem . The present invention is predicated upon the s perature within the range 80° to 180° C. Also, discoveries that uranium pentachloride is a bi the amount of liquid air which is applied to the nary compound of the form. UCl4. UCl6 rather cold surface of the still is such that the tempera than a monomeric compound of the form UCls ture of the cold surface is maintained at 10°C. and that in this compound the molecular bond or below. Finally, the vacuum pumping appara may be broken under certain conditions, pro tus is adjusted, so that the pressure within the ducing as two independent compounds UCl4 still between the hot surface and the cold Sur and UCls. face is maintained at a value between 106 and Accordingly, it is an object of the invention to 10-3 mm. Hg. Preferably in carrying out the provide UCls as a stable, compound. process, the space between the normal hot-sur Another object of the invention is to provide a 25 face and the normal cold surface of the still is process of producing UCls as a stable compound. evacuated to obtain the Subatmospheric preSSure Another object of the invention is to provide. a within the range mentioned, before the normal process of producing UCls which utilizes uranium hot surface is heated by the Sand bath and the pentachloride. normal cold surface is cooled by the liquid air. Another object of the invention is to provide a 30 When the charge of uranium pentachloride is process utilizing uranium pentachloride, whereby thus heated under stoatmospheric preSSure, it UCl4 and UCls are produced, and separated. is converted into UCl4 and UCl6, the UCl6 being A further object of the invention is to provide sublimed as it is produced. The UCl4 remains as a process in which the molecular bond in the bi a residue upon the hot surface. and the Sublimed nary compound UCl4. UCls is broken, whereby 35 UCls traverses the space between the hot and cold UCl4. and UCls are produced as independent surfaces to condense. upon-the cold-Surface.in the compounds. form of iridescent, darkgreen, fine-grained crys A further object of the invention is to provide tals as the temperature of the charge is above a process utilizing UCl4. UCls, whereby UCl4 and the sublimation point of UCls and below the Sub UCls are produced and UCls is sublimed away 40 lination point of UCl4. from UCl4. The process is continued until the charge of A still further object of the invention is to uranium pentachloride is substantially come provide a combination.heating and vacuum proc pletely converted, at which time the residue re ess of producing UCl4 and UClg from uranium maining - on the hot surface is Substantially pentachloride and of separating these products 45 chemically pure UCl4 and the Sublimate collected from each other. on the cold surface is substantially pure UCls. The invention, both -as to its organization and At this time, when further production and sub method of operation, together with further ob innation of UCls ceases, aid the process is Con jects and advantages thereof, will best be under plete, the UCl4, residue is removed from the hot stood by reference to the following Specification 50 surface and the UCls sublimate:is removed from taken in connection with the accompanying the cold surface. Ordinarily in carrying out the drawing, in which the single figure is a schematic process a charge of 100 grams of uranium penta illustration of apparatus-Suitable for carrying Out chloride may be substantially completely con the processes of the present invention, Verted into a residue of UCl4 and a Sublimate of Inaecordance with the present invention, a 55 UCl6 in approximately three hours. 2,572,156 w 3 It is virtually essential that the still be trans is considerably below that of UCl4 and that UCIs ferred to a dry cabinet containing CO2 or other has a much higher vapor pressure at a given tem inert gas before it is opened, in view of the fact perature than UCl4. Further, it is thought that that the Sublimate UCls is extremely hygroscopic the following specific reaction takes place: and readily decomposes in the presence of ordi nary atmosphere into UO2Cl2. The product UCl4. UCls--heat->UCl4--UCls UCls is then bottled in an atmosphere of CO2 Or Theoretically, one mole of the binary compound in a vacuum and Sealed for future use. The prod UCl4. UCl6 (831 grams) should yield one mole of uct UCls so produced is particularly well suited for the monomeric compound UCl4 (380 grams) and use in vacuum apparatus, in that it has a very. 10 One mole of the monomeric compound UCl6 (451 much greater vapor pressure at a considerably grams); the weight percent of chlorine in the lower temperature than other volatile chlorides residue UCl4 should be 37.34; and the weight per of uranium, such, for example, as UCl4. cent of chlorine in the sublimate UCls should be While the process may be carried out at a tem 47.19. The analyses of the residue and the sub perature below the lower end of the preferred 15 limate produced incident to carrying out the range, it is noted that in the event the temper present process checked very closely with the ature is much lower than 80 C. the yield of theoretical values indicated. For instance, in a UCls from the charge is extremely poor and typical run utilizing a charge of 100 grams of very slow. Similarly, while the process may be uranium pentachloride, when the process is. Sub carried out at a temperature above the upper 20 stantially complete analyses have indicated a end of the preferred range, it is noted that in the weight of UCl4 residue of 47 grams, a weight of event the temperature is much higher than 180 UCls Sublimate collected of 52 grams, and a C. the UCl4 produced as a residue in the charge Weight of UCl6 Sublimate lost of one gram. Also, itself begins to sublime, and the UCls is decom analyses for total uranium and total chlorine, posed to UCl4 and C2 before it can be sublimed made gravimetrically by tested procedure, indi from the hot surface. In other words, it is es cated the following for the Sublimed material: sential that the process be carried out under conditions such that the newly formed UCls is Per cent removed from the hot Zone, or region of maxi Total U------------------------------- 53.30 mum temperature, before any substantial decon 30 Quadrivalent U------------------------ (2.3). position of the product UCl6 can take place. Also, Chlorine------------------------------- 46.41: when the temperature is much higher than 180 C., the sublimate is of very low chemical purity 99.71 in that large amounts of UCl4 are mixed with Atomic ratio Cl/U---------------------- 5.85 - the UCl6, and furthermore the yield is low. 35 When allowance is made for the inevitable Of course the vapor pressure-temperature decomposition which accompanies any transfer curves of UCls and UCl4 are of usual form, the of material, except under vacuum in thoroughly vapor pressure increasing disproportionately baked-out apparatus, the analyses are so close to with temperature, whereby there is a negligible that required for UCls that there can be no serious Sublimation of UCl4. Within the normal Sublima 40 doubt that the Sublimate is Substantially chemi tion temperature range of UCl6. However, for cally pure UCls; the atomic ratio Cl/U of 5.85 practical purposes of obtaining correspondingly. obtained from the analyses is well within experi reasonable yields, it may be said that the Subli mental error of the theoretical atomic ratio mation temperature of UCls is well below that Cl/U of 6. Also, analyses of the residue yield of UCl4 as indicated below: 45 an atomic ratio of Cl/U of 3.94, clearly indicat ing that the residue is Substantially chemically Wapor Pressure pure UCl4.
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