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Dykurnn SN2 a //3- a 2 April 24, 1956 A. D. WEBB E.T A. 2,743,158 PROCESS FOR PRODUCING URANIUM PENTACHLORIDE Filed May 26, 1944 2 Sheets-Sheet l // 8 //? (19 /16 / //a (3/2735 rt DykURNn SN2 a //3- A 2 1846 42.47 41 % sins. C 48 444549 is Jo U+ 13 as /3 Z27, Z. INVENTORS. ALBERT D.WEAB BY HUGHA. KYLE ATTORNEY. April 24, 1956 A. D. WEBEB ET AL 2,743,158 PROCESS FOR PRODUCING URANIUM PENTACHLORIDE Filed May 26, 1944 2 Sheets-Sheet 2 34? INVENTORS, ALBERT D. We BB BY HUGH ARYLE 1411-4 a sella-la-11 ATTORNEY. 2,743,158 United States Patent Office Patented Apr. 24, 1956 2 vation view, partly in section, of the reaction vessel and its associated feeding mechanism and collector for the 2,743,158. final product; Fig. 2 is a diagrammatic side elevation PROCESS FOR PRODUCING URANIUM view, partly in section, of one form of apparatus for PENTACHLORDE eliminating the uranium pentachloride, in the form of a Albert D. Webb, Oak Ridge, Tenn., and Hugh P. Kyle, dust, from the gas leaving the collector before recircula Los Altos, Calif., assigao's ta the United States of tion of the chlorine gas through the reaction zone; Fig. America as represented by the United States Atomic 3 is a diagrammatic side elevation view, partly in section, Energy Commission of a modified form of apparatus for separating the solid 0. particles from the unused chlorinating gas before re Application May 26, 1944, Serial No. 537,524 circulation of the same through the reaction chamber; and Fig. 4 is a diagrammatic side elevation view, partly in section, of another modified form of apparatus for separating the fine particles from the chlorine before This invention relates to the manufacture of uranium 5 pentachloride, especially by a continuous process. More recirculation of the same over fresh quantities of uranium particularly, it appertains to the conversion of uranium tetrachloride. tetrachloride to uranium pentachloride by sending a The apparatus employed comprises a reaction vessel stream of such material in granulous form through a heat embodying means for propelling the granulous uranium ed zone in an environment of chlorine. tetrachloride being treated along the reaction vessel, a A need for large quantities of uranium pentachloride 20 feeder embodying means for supplying a continuous exists in industry. Each of the processes heretofore avail stream of uranium tetrachloride to the reaction vessel, a able for its preparation was unsatisfactory for one or more biower for producing a flow of chlorinating gas through reasons, such as being wasteful of reactants, being diffi the apparatus, a receiver for the reaction product, UCls, cult to carry out, being inconveniently slow, being a batch and a dust collector for separating the fine solid par wise operation and giving undesirably low percentages of 25 ticles from the gases issuing from the receiver. coVerSO. Referring now to Fig. 1 of the drawing, the reaction This invention has for an object the continuous pro vessel comprises a horizontal tube 10 constructed of duction of uranium pentachloride. Other objects are to glass or other chlorine-resistant material, about which is decrease the time required to produce uranium penta set a heater 11. The heater illustrated is of the electric chloride, to improve the yields in the manufacture of 30 resistance type having a heating coil 12. The tube 10 uranium pentachloride, to increase the purity of uranium has a gastight ground glass joint 13 to facilitate assembling, pentachloride obtained in large-scale manufacturing proc cleaning, etc, The reaction vessel has an adit 14 for esses, to produce uranium pentachloride more economical the pulverulent raw material (uranium tetrachloride) ly, to decrease the loss of final product in the manufacture and adits 15 and 16 for chlorine or other chlorinating gas. of uranium pentachloride, to increase the production rate 35 These adits or ducts are, preferably, tubular extensions in the manufacture of uranium pentachloride, to obtain a of the tube 10. Emaximum heat transfer in the conversion of uranium com Operating inside the reaction vessel to plow and propel pounds to uranium pentachloride, to increase the yield per 17, preferably of some material such as glass which is unit volume of reactor unit in the chlorination of a lower 40 not affected by the reactants. The helix 17 is integral uranium chloride to uranium pentachloride, to provide with or otherwise rigidly secured to a shaft 18 and is maximum Feaction surface in the conversion of uranium rotated thereby. The shaft 18 extends through a tubular tetrachloride te uranium pentachloride, to transport urani extension 19 and a plug 41. The plug 4 filling the urn pentachloride away from the reaction zone as fast as it space between the shaft 18 and the sidewall closes the it formed, to chlorinate uranium tetrachloride to uranium mouth of the extension 19 in a gastight manner. The pentachloride, to react chlorine with uranium tetrachlo bearing surfaces are pressure lubricated. The granulous ride to form uranium pentachloride, to secure optimum uranium tetrachloride, advanced by the helix 37 into the chlorine velocity in the chlorination of uranium tetra heated reaction zone, is converted to uranium pentachlo chloride, to recirculate chlorine gas in the process of ride which leaves the reaction zone in vaporous form chlorinating uranium tetrachloride to uranium pentachlo 50 and, upon cooling, forms solid particles which fall by ride, to remove solid particles from the exit gas in the gravity from the reaction vessels through an exit of chlorination of uranium tetrachloride to uranium penta delivery tube. 22. chloride, to convert uranium tetrachloride to uranium A pulley 44 fixed in position by a set screw 45 threaded pentachloride in glass apparatus, and to simplify the ap through its hub onto the shaft 18 and operated by a belt paratus required in the production of uranium penta 55 (not shown) rotates the helix 17. The shaft 8 is sup chloride. A general advance in the art and other objects ported by two bearings 46 and 47 and positioned laterally which will appear hereinafter are also contemplated. therein by two collars 48 and 49. The bearings 46 and A process has now been discovered and apparatus de 47 are bolted to a fixed support 42. signed whereby the operations of chlorinating uranium To prevent clogging of the exit 22 by material stick tetrachloride to uranium pentachloride, separating the 60 ing to the inner walls thereof, a rotating scraper device solid particles from the noncondensing gases issuing from comprising a series of blades 23 carried on a vertical the reaction zone and recirculating the unused chlorinat rod or shaft 25 is provided. A plug 26 serves as a guide peditiously.ing gas can be carried Qut easily, economically and ex for the rod 25 and as a gastight closure for the mouth of a tubular extension 27 of the reaction vessel, A How the foregoing objects and related ends are ac fixed support 28 earries two bearings 29 and 31 for the complished will be apparent from the following exposi shaft 25. A pulley 32 located between these bearings tion in which are disclosed the principle, the organiza and operated by a belt (not shown) rotates the scraper. tion and divers embodiments of the invention, including This pulley is secured by a set serew 33 threaded threugh the best mode contemplated for carrying out the same. its hub onto the shaft. The spacing of the pulley and Parts are given by weight throughout the written de 70 bearings is such that the scraper can be lifted entirely scription, which is amplified by the accompanying out of the delivery tube 22 when desired. The scraper drawings, in which Figure 1 is a diagrammatic side ele is vertically adjustable by means of a manual grip or 2,748,158 3. 4 hand wheel 35. It is held in any desired position by device. The fluid stream from the tube 175 passes thrust collars 37 and 39. Thumb screws 36 and 38 through a series of tubes 210, 211, 212 and 213 con permit easy release of these collars for vertical adjust nected by U-tubes such as 215 and 216 into the line ment of the scraper. 125 which is connected to the intake side of the pump In order to provide continuous and regulated flow 5 ii. The diameter of the horizontal tubes and the length of uranium tetrachloride into the reaction vessel, a hop of the path the chlorine gas travels is adjusted so that per or feeder device embodying a helical impeller is the UCls dust particles settle out. The horizontal tubes used. This feeding device comprises a tube 51 of glass are ordinarily cylindrical and about two inches in di or other chlorine-resistant material in which a helix 52 ameter. - of similar material rotates. This screw-conveyor-like O In the somewhat more intricate scrubbing device shown forwarding device receives the raw material from an in Fig. 3 the line 175 from the receiver 171 is con adit tube 53 and transmits it to an exit tube or duct nected at 311 with an extension 312 on a vessel 313 54. This tube 54 is connected in a gastight manner serving as a sump. This vessel at 314 is connected to the adit 14 at a joint 55. Chlorine gas enters the with a scrubber 315 containing a loose packing 316 of tube 51 through a tubular extension 56 and flows con glass beads or some similar chlorine-resistant material. current with the raw material into the reactor and keeps The UCls dust laden chlorine gas passing up this scrub a satisfactory environment in this part of the apparatus, ber flows counter to a suitable scrubbing liquid such The incoming mass of uranium tetrachloride hinders or as carbon tetrachloride, which is preferred, or an equiva precludes escape of the chlorine through the adit 53.
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