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Aa-2A. at ATTORNEY March 24, 1959 G. E. Macwood ET AL 2,879,130 PROCESS FOR RECOWERING URANIUM Filed Dec. ll, 1945 5 Sheets-Sheet 1 INVENTORS. GAOeGa f. A/40 WO22 CO/A/MAM/ A WAAA/ BY TA4//?o 4/7/M4// -aa-2a. AtATTORNEY. March 24, 1959 G. E. MACWOOD ETAL 2,879,130 PROCESS FOR RECOWERING URANIUM Filed Dec. ll, 1945 5 Sheets-Sheet 2 COWDAWSA7A scRUBBING AND WASHING 25.2% PARTS OF CALUTRON 24SA/ SOAV7/OW SOA/A /MAU/AP/7/AS MAAE UA h S E V N G --> Wa/AAR amaramates TO DSCARD CONDENSING WASA/ SOLU7/OM OR SALVAGE O X D Z N G Uttt --Uoatt SOL/A UO 2* - UO2' s /MAUAP/7/ES U(OH)4-e-UO2' FILTE R N G CUO -- Cutt navataras Cuc -- cut Cu2O -->CU Fett - - Fett TO DSCARD OR SALVAGE AARAC/A/747A C FILTER ING TO DSCARD - OR SALVAGE EVAPORATING EVAPORATING TO FURTHER TO FURTHER TREATMENT TREATMENT INVENTORS. GAOAOff A. W46 M/OOA s CO/AAW4W A). A1/AAAA A. y 2 BY Z4i/d 4/774W 4-16 at-1-ATTORNEY. March 24, 1959 G. E. MACWOOD ETAL 2,879,130 PROCESS FOR RECOVERING URANIUM Filed Dec, ll, 1945 5 Sheets-Sheet 3 DISSOLVING URANUM METAL DEPOSITED ON STANLESS STEEL COLLECTOR IN (i.) HOT SOLUTION HNO3 (12%) oR (2) SOLUTION HCI 2%8, H2O2 (0.5%) or (3)SOLUTION H2SO4 (8%)& H2O2 (0%) COWAAMSA 7A AWO MAAA UA //) A WO, or (2) AC/ & Aeole or (3)Al2SO & Ade O2 SOAV7/OAV CON DENS NG (1) At WO or (2) AC/ & Ale O2 (3) H2 SO & Aeole EVAPORATING . COWCAAV7APA 7AA) SOAV7/OAW Uo A “ff C. fff W. TO FURTHER TREAT MENT INVENTORS. GAOAGA A. Wao M/OOA A.7., 5 CO/AA/4A/ A. M/// AAA BY -224-4-4- all-s-s-s-s-a-ATTORNEY. March 24, 1959 G. E. Macwood ETAL 2,879,130 PROCESS FOR RECOWERING URANIUM Filed Dec, ll, 1945 5 Sheets-Sheet 4 MATERA FROM PROR TREATMENT SHOWN ON FIGS. 2 and/or 3 WAfg PRECIPITATING a co- free - AN A/A re Whi OH cu(NH3)4* Ni (NH3)4 P REC PTATE -- ar (NH4)2 U2O7 Fe(OH)3 To DSCARD Cr(OH) OR SALVAGE -a- F As H a a B O L E R WAAOA - /AAOA We or CrC/t, w VCAs, VC/4, CO2 AeC/U CAs CrC/, AeC/3 - conDEN SER is.& To CALUTRON collector SOL/D UC/ U C/s SMOAA SOAA Crc/s, ELECTROSTAT1C AeC/ PRECIPTATOR SOAAA -Cl UC/5 R E A C T O R TO DISCARD seascassasserasa N SOL/A UC/ OR SALVAGE 4. T INVENTORS A.47 4 CAUTRON GAOaGa A. A/46 WOOA BY -ael-2-aa. at-e-a-1ATTORNEY. March 24, 1959 G. E. MACWOOD ETAL 2,879,130 PROCESS FOR RECOVERING URANIUM Filed Dec. ll, 1945 5 Sheets-Sheet 5 g/// /º// 9://22:// 2,879,130 United States Patent Office Patented Mar. 24, 1959 1. 2 from metallic impurities and to reconvert said uranium 2,879,130 into a calutron charging stock by the minimum number PROCESS FOR RECOVERING URANUM of process steps and manipulation. George E. MacWood, Berkeley, Calif., Coleman D. Accordingly, it is an object of the invention to provide Wilder, Oak Ridge, Tenn., and David Altman, Pasa an improved process for reclaiming uranium from solu dena, Calif., assignors to the United States of America tions thereof. as represented by the United States Atomic Energy Another object of the invention is to provide an im Commission proved process of reclaiming uranium from solutions of Application December 11, 1945, Serial No. 634,312 the character above-mentioned that may be readily carried 12 Claims. (C. 23-14.5) 10 out on a commercial scale and in an economical manner. This invention relates to the purification of uranium Another object of the invention is to provide an im and more particularly to an improved reclamation process proved process for recovering the residue of a uranium that is especially useful for recovering uranium from compound which has been subjected to treatment in a wash solutions derived from calutrons employed in the calutron from the parts of a calutron disposed in the calutron method of producing uranium enriched with source region thereof upon which the residue is deposited. U235. A further object of the invention is to provide an im In the copending application of Ernest O. Lawrence, proved process of recovering metallic uranium enriched Serial No. 557,784, filed October 9, 1944, now U.S. Patent with U235 from the collector of a calutron upon which 2,709,222, issued May 24, 1955, there is disclosed a “calu the enriched metallic uranium is deposited. tron,' a machine designed to separate the constituent iso 20 A still further object of the invention is to provide an topes of an element containing several isotopes, in order improved process of purifying uranium which has been to produce the element enriched with a selected isotope. recovered from a calutron. More specifically, the calutron mentioned is especially Still another object of the invention is to provide a designed to produce uranium enriched with the isotope process of reclaiming uranium from a wash solution de U235. 25 rived from a calutron in which the uranium, together with In the copending application of James M. Carter and metallic impurities, is precipitated from said solution, the Martin D. Kamen, Serial No. 532,159, now U.S. Patent resulting precipitate is chlorinated at an elevated temper 2,758,006, issued August 7, 1956, filed April 21, 1944, ature such that the chlorides of uranium and of metal im there is disclosed an improved process of producing ura purities exist largely in the vapor phase, and the uranium nium enriched with U235 employing the calutron method 30 chloride is then separated from the remaining metallic and comprising first-stage and second-stage calutrons. In chlorides present in the vapor mixture by fractional con accordance with this process, uranium of natural or nor densation by virtue of the differences in their relative mal isotopic composition is treated in a first-stage calutron volatilities. in order to produce as a product uranium singly enriched A still further object of the invention is to provide a with U235, which uranium singly enriched with U235 is 35 process of purifying uranium contained in a wash solu treated in a second-stage calutron in order to produce as tion derived from a calutron in which the uranium, to a product uranium doubly enriched with U235, which ura gether with certain of the metal impurities, is precipitated nium doubly enriched with U285 may be used commer by ammonia away from the remaining metal impurities in cially. In the operation of either a first-stage calutron or the wash solution and the uranium is then separated from a second-stage calutron the compound UCl4 is treated, 40 the metal impurities in the precipitate by chlorination of whereby a residue of the UCl4 is deposited on the parts the precipitate and fractional condensation of uranium of the calutron disposed in the source region thereof, chloride from the more volatile metallic chlorides thus metallic uranium enriched with U235 is deposited in the obtained. first pocket of the calutron, and metallic uranium im A still further object of the invention is to provide an poverished with respect to U235 is deposited in the second 45 improved process of reclaiming uranium from a wash pocket of the calutron. The deposit of UCl4 is recovered solution derived from a calutron and converting the by a water wash step and the deposits of metallic ura uranium so reclaimed into a suitable compound for re nium are separately recovered by acid wash steps; and the charging a calutron. three wash solutions are separately purified, if required, A still further object is to provide an improved process to produce three separate batches of a given compound of 50 for treating uranium in a calutron in which uranium and uranium. In this process, a first batch of the uranium impurities such as iron, copper, nickel, and chromium compound mentioned, produced from the water wash contained in a wash solution derived from the calutron derived from a first-stage calutron, is then converted back are separated, and the separated uranium is converted to UCl4 for re-treatment in the first-stage calutron, and into a suitable charge for further calutron treatment. a second batch of the uranium compound mentioned, 55 A still further object of the invention is to provide a produced from the water wash derived from a second process of reclaiming uranium from a calutron wash solu stage calutron, is then converted back to UCI for re tion containing metallic impurities in which uranium and treatment in the second-stage calutron. certain metallic impurities are precipitated with ammonia, In view of the minute quantities of the isotope desired the resulting precipitate is chlorinated and converted into recovered by the calutron process, it is of extreme im 60 volatile metal chlorides by contacting said precipitate portance to increase the uranium recovery to the highest with carbon tetrachloride at an elevated temperature and possible percentage. Such recovery treatment is particu uranium chloride is separated from the resulting volatile larly important in conjunction with the filtrate obtained metallic chlorides by fractional condensation. from the wash water solution derived from the second Still another object of the invention is to provide a stage calutron, in view of the fact that said wash solution 65 process of reclaiming uranium from a calutron wash constitutes a relatively large volume and the uranium con solution containing iron, copper, nickel, and chromium tained therein has been singly enriched with U235 due to as impurities in which uranium, iron, and chromium are the previous treatment thereof in the first-stage calutron.
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