Jan. 15, 1952 C. D., WLDER 2,582,941 PROCESSES OF PRODUCING URANIUM CHLORIDES Filed Oct. 2, 1944 d S Q Q Q t 2. INVENTOR. 6ozEMAW Z. WZZZOER ATTORNEY . Patented Jan. 15, 1952 2,582,941 UNITED STATES PATENT OFFICE 2,582,941 PROCESSES OF PRODUCING URANUM CHELORDES - Coleman D. Wilder, Oak Ridge, Tenn., assignor to the United States. of America, as represented bysion the United States Atomic Energy Commis Application October 12, 1944, Serial No. 558,452 8 Claims. (C1. 23-145) 2. - This invention relates to the manufacture of a pating carbon tetrachloride vapor in a speedy uranium chloride product, and more particularly stream of dry air, passing the resultant mixture re of uranium pentachloride over an uranium compound heated to the neigh - - - - - a . g a substantial proportion of borhood of 550° C. whereby uranium pentachlo uranium hexachloride, by a process for chlorinat: ride is formed and vaporized into the current, ing various, compositions comprising uranium moving the resulting vaporous mixture into a compounds, with carbon tetrachloride vapor car collecting receptacle so that most of the uranium ried by a Swift current of air. chloride will condense and settle out, and send This invention has for an object the rapid pro ing the gas stream through a dust separator to duction of a uranium chloride product compris strip it of the residual uranium-containing par ing a large proportion of uranium pentachloride ticles. and various proportions of uranium hexachlo The apparatus employed comprises a device ride. for supplying carbon tetrachloride, a device for A further object of the invention is to provide supplying dry air, a flash boiler in which the a high-yield, low-loss process for the production 5 carbon tetrachloride is vaporized and mixed with of uranium pentachloride which is economical the air, a reaction chamber in which the ai and suitable for large scale production of said carbon tetrachloride admixture is reacted with chloride. m the uranium-containing raw material, a heater A further object of the invention is to provide about the reaction chamber, a delivery duct for - a process for the production of uranium penta 2 conducting the vaporous reaction product from chloride and more or less uranium hexachloride the reaction chamber to collecting means, a re by means of a continuous reaction wherein vari ceiver for collecting the bulk of the principal ous compounds of uranium are reacted with product (uranium pentachloride, with or without vaporous, carbon tetrachloride which is carried uranium hexachloride) and an electrostatic sep by a rapid current of air. 2. 5 arator for removing the remainder of the reac A further object of the invention is to pro tion product that, in dust-like form, has been vide a process for the production of uranium carried through the receiver by the air stream. pentachloride and more or less uranium hexa Referring now to the drawing, there is shown chloride wherein a large effective reaction sur near the center a reaction vessel which comprises face and maximum heat transfer is obtained 30 a horizontal heat resistant cylindrical tube if, through employment of a high velocity of the constructed of Pyrex glass or the like, about 4. chlorinating mixture of carbon tetrachloride and inches in diameter and about 4 feet long. Lo 2. cated in the tube is an open-ended boat or A process has now been discovered and ap tray 3 containing a charge 3 of uranium com paratus designed for treating uranium com pound. For raw material such as uranium tri pounds, especially oxides and lower chlorides, Ox uranium tetrachloride, a charge of 10. with carbon tetrachloride in a swift current of 'o 15 kg. is commonly used. A heater compris air, whereby uranium pentachloride is formed, ing a refractory, shell is and a wound electrical vaporized, rapidly swept out of the reaction zone, resistance heating element 5 having two leads 6. and quickly cooled. 40 and a surrounds the tube . A tube 21 extends How the foregoing objects and related ends through a plug 22 of some heatresistant material, are accomplished will be apparent from the fol such as asbestos, into, the interior of the tube. lowing exposition, in which are disclosed the it at its a dit end, to provide ingress for the principle, the organization and divers embodi gases utilized in the treatment of the source mas ments of the invention, including the best mode terial. An iron-constantan, thermocouple (not contemplated for carrying out the same. Parts shown), inserted between the heater and the tube are given by weight throughout the written de it, is used to measureas: the furnace temperature. scription, which is amplified by the accompany The plug 22 is sealed to the tubes and 24 in a ing drawing of the apparatus in which the gastight manner by means of water glass or single figure is a diagrammatic side elevation view, 50 the like. partly in section, with some parts shown in con The gases passed into the reaction chambei. ventionalized form and some parts over-scale for through the tube. 2 include carbon tetrachloride. clarity. has beea thoroughly mixed with air In its broad aspect, the procedure compre a flash boiler 23, of whiwhich the tube 2 is an hended by the present invention comprises dissi extension. The lash boiler is preferably heated 2,582,941 3 - 4. by means of an electrically operated hot plate 92 in a gastight manner by means of water glass 26 controlled by a switch 27. The air enters the or similar luting compound. To prevent clogging boiler through an extension tube 24 which is of the passage for the reaction gases and to free connected to a source of Supply at the joint 25. the central portion of the cross 9 and its arm Ordinarily, the air is taken from an air pres 5 95 from any material which might accumulate sure line conventionally represented at 3. The on their interior surfaces during operation of the air passes through a joint 32 and line 33 to a apparatus, a scraper 97 carried on a rod 98 is drying device. 34 comprising an open-ended cyl provided. This rod is slidably and rotatably inder filled with calcium chloride. The line : 33 mounted in a plug 99, made of rubber or the like, extends through a plug 35 which seals the adit it) which closes the arm 93 about the rod in a ga S end of the drying device. 34. The air leaves this tight manner. A hand wheel 00 fixed on the device through a line 36 extending through a plug rod 98 serves as a means for manipulating the 37 Sealed in the exit end of the device 34. The scraper. - A simple plug 0 of rubber or the like line 36 conducts the air into a second and similar closes the arm 94 in a gastight manner. drying device 38 comprising an open-ended cyl The arm 95 extends through a plug 102 in the inder filled with anhydrous magnesium perchlo mouth of a large receiver 3, to a point near its rate. The line 35 extends through a plug 39 center. --Suitably the receiver is constructed of sealed in the adit end of the drier 38. The air glass or other chlorine-resistant material, and leaves the exit end of this device through a line has a capacity of about five gallons. The reac 40 which extends through a plug 4 sealed in the 20 tion gases pass down arm 95 into the receiver 3 exit end of the drier .33. The line 40 is con where the bulk of the uranium pentachloride set nected by means of a joint 42, with a line 43, tles out... The gas from which this material is which in turn is connected with the extension 24 separated in the receiver, escapes through a vent at the joint 25. tube to 4 also extending through the plug G2. Extending into the boiler 23 through a gastight The escaping gas passes through a joint 95, a plug 5 is a carbon tetrachloride feeder tube 52, line fos, a joint 07, a line. O8, and a side arm having on its end inside the boiler a capillary ?o for delivery to a device for removing the last nozzle 53. The tube 52 constitutes a part of a dust-like traces of uranium compound therefrom. carbon tetrachloride supplying device comprising Access to the principal part of the line 108 for a reservoir 55 and a tube 54 joining these parts. 30 cleaning purposes is gained by removing a plug The capillary nozzle 53 is of such dimensions that f09, thereby avoiding dismantlement of the appa a considerable pressure is necessary to force the ratus. carbon tetrachloride therefrom in the desired Usually, some of the uranium pentachloride is announts. Air pressure is utilized for this pur carried out of the receiver 03 by the stream of pose. It is Supplied from a source of air pressure gas passing therethrough. This transported shown conventionally at 6. The air from this material is in the form of a powder that does Source is Supplied through a joint 62 to the line not settle satisfactorily and is difficult to collect. 63, which has, as a side arm, a conventional Preferably, it is recovered by a fume remover mercury manometer 64 for indicating the air of the electrostatic type. These devices (com pressure. The line 63 is connected through a monly referred to as “Cottrell precipitators') are joint 65 to a line 66 which incorporates a pres well known in the art and need not be illustrated Sure regulating device for maintaining constant or described in great detail.