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Nov. 29, 1966 A. V. HENRICKSON 3,288,570 PRECIPITATE Zr (CO)

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Nov. 29, 1966 A. V. HENRICKSON 3,288,570 PRECIPITATE Zr (CO) Nov. 29, 1966 A. V. HENRICKSON 3,288,570 PROCESS FOR THE SELECTIVE RECOVERY OF URANIUM, ZIRCONIUM AND MOLYBDENUM Filed Aug. 16, 1963 2 Sheets-Sheet |OOO LBS. PREGNANT CARBONATE LIQUOR 25 LBS. U30s O LBS. Mo 2.5 LBS. Zr 4 LBS. NaOH -- ADJUST pH TO O PRECIPITATE Zr (CO) BY DIGESTING AT 95F FILTER AND WASH -- Zr PRODUCT 2.45 BS. Zr 9 LBS. No OH--- PREC PTATE YELLOW CAKE FILTER AND WASH-UO PRODUCT 25 LBS. U30s 5 LB. Zr 57 LBS, HSO - ACDIFY TO pH 1.5 ABSORB Mo ON CHARCOAL-e-BARREN EFFLUENT AND 8 LBS. NaOH-e-ELUTE |O LBS. HCL -- ADJUST pH TO pH 7 |4 LBS. CaCl2--PRECIPITATEI CoMo.O. FILTER AND WASH-B-Mo PRODUCT O BS. Mo i. e NVENTOR. ANGUS V HENRICKSON BY ATTORNEYS Nov. 29, 1966 A. V. HENRICKSON 3,288,570 FROCESS FOR THE SELECTIVE RECOWERY OF URANIUM, ZIRCONIUM AND MOLYBDENUM Filed Aug. 16, 1963 2. Sheets-Sheet 2 PREGNANT CARBONATE 25 LBS. U30s 8.5 LBS. HSO4. 5 LBS. Mo 48 LBS. H2SO4--ADJUST tTO pH 3.5 O PREC PTATE URANYL MOLYBDATE DIGEST 6 HRS. AT 25°C FLTRATE FILTER - NO WASH-25 LBS. UOs LB. Mo PRECIPITATE 25 LBS. U3O8 4 LBS. Mo 4 LBS. NaOH -e- DISSOLVE Mo DIGEST | H R AT 8OC PREC PTATE F LTER - NO WASH-> 25 LBS. UOs t O2 LBS. MO FLTRATE 4 B.S. Mo 4O LBS. No OH-e-PRECIPITATE YELLOW CAKE H 3 LBS. HCL -- ADJUST pH TO 8.O FILTER 8. WASH 18 LBS. CaCl-e-PRECIPITATE CoMo.O4. YELLOW CAKE FLTERT t WASH PRODUCT CaMoo PRODUCT INVENTOR. ANGUS W HENRICKSON BY 54-4-2 - 52-ca. ATTORNEYS 3,288,570 United States Patent Office Patented Nov. 29, 1966 2 that the presence of zirconium during charcoal adsorption 3,288,570 of molybdenum seriously poisons the charcoal against PROCESS FOR THE SELECTIVE RECOVERY OF molybdenum adsorption and thus renders such adsorption URANUM, ZERCONEURM AND MOLYBEDENUM prohibitive in its presence. Uranium can be precipitated Angus W. Heinrickson, Golden, Colo., assignor, by mesne assiganents, to Susquehanna Western, Enc., Denver, directly from the pregnant strip carbonate solution with Colo., a corporation of Wisconsin Sodium hydroxide or it can be precipitated after destroy Fied Aug. 16, 1963, Ser. No. 302,627 ing the carbonate; however, such precipitation also pre 19 Clains. (C. 23-328) cipitates zirconium as zirconium hydroxide and this com pound ends up as an impurity in the yellow cake. This invention relates to a method for the selective re IO Accordingly, it is an object of this invention to provide covery of uranium, zirconium and molybdenum from a process for the selective recovery of uranium, zirconium composite ores containing these metals together; more and molybdenum from composite ores in which they exist particularly, it relates to the process for the selective re together. covery from relatively low grade carbonaceous minerals It is another object of this invention to provide a process of the metals uranium, molybdenum and zirconium exist 5 for the selective recovery of uranium, zirconium and ing together in the minerals. -molybdenum existing together in ores having a high con The invention is illustrated by its application to car tent of carbonaceous or organic material, such as, lignite bonate strip liquors resulting from the treatment of lignite OreS. ores by conventional processes. More specifically, the It is still another object of this invention to provide a invention is illustrated by its application to the selective 20 process for the selective recovery of the metals uranium, recovery of uranium, zirconium and molybdenum from Zirconium and molybdenum from carbonate solutions in carbonate strip liquors resulting from solvent extraction general and from carbonate liquors and leach solutions of carbonate leach liquor of lignite ore. The invention formed by treatment of carbonaceous ores. is not limited in its application to carbonate strip liquor so It is a further object of this invention to provide a formed but is applicable to carbonate strip and leach 25 process as Stated which is commercially feasible and which liquors of the three metals in general. Likewise, it is not produces the metals in a form meeting standard require limited in its application to strip or leach liquors but can ments of purity. be applied to carbonate solutions in general containing The above objects of the invention are accomplished the three metals, and particularly to liquors formed by by a process in which zirconium is first selectively re leaching ores with alkali metal carbonates and bicar 30 covered from a carbonate solution containing the three bonates. metals, followed by selective separation of uranium and The process of the invention is particularly useful for moiybdenum. The process includes two modifications. the selective recovery of uranium, zirconium and molyb In accordance with modification (1) of the process of the denum from ores associated with various carbonaceous invention, in step (1) zirconium is precipitated as the materials, for example, coal, lignite, oil shale and others. 3 5 carbonate by adjusting the pH of the carbonate strip liquor It is illustrated herein by its application to ignite ores. to a point just below the incipient precipitation of ura Ore grade uraniferous lignite exists in commercial nium and the precipitate recovered by filtration. In step quantity in Montana and the Dakotas. Experience has (2) uranium is removed from the filtrate of step (1) shown that uranium recovery from lignite ores has a containing uranium and molybdenum by precipitation as marginal profit potential using available recovery proc 40 yellow cake followed by filtration. In step (3) molyb esses, and that burning the ore before leaching offers the denum is removed from the filtrate of step (2) by adsorp best possibility for processing. The ore contains sufficient tion on charcoal and recovered by Stripping from the carbonaceous materials to support combustion and the charcoal and precipitation from the stripping solution as residue is more susceptible than the ore to treatment with calcium molybdate. an aqueous leaching solution, such as, a strong mineral 45 In modification (2) of the invention, after step (1) acid or an alkali metal carbonate. The ash contains in which zirconium is precipitated as basic zirconium molybdenum and zirconium in addition to uranium, and carbonate as above, in step (2) the filtrate of step (1) the separation of these elements from the uranium is is treated by pH adjustment and heating to precipitate necessary in order to meet yellow cake specifications. the molybdenum as uranyl molybdate, followed by filtra These specifications include a limit for molybdenum of 50 tion. The filtrate from step (2) is treated to recover .6% of the UOa, and will include a limit for zirconium uranium not used in step (2') as yellow cake for the main of 2% of the UOs. Aside from the fact that molyb stream recovery. In step (3') the molybdenum is dis denum and zirconium must not contaminate the yellow Solved from the precipitate of uranyl molybdate of step cake, their separation and recovery in saleable form would 55 (2) and recovered from the solution as a calcium molyb increase the income from the process and contribute to date precipitate. The precipitated uranium of step (2') its commercial feasibility. which remains after molybdenum is dissolved out is con There are a number of disadvantages attendant to the verted to yellow cake and re-cycled to maintain sufficient selective separation of uranium, molybdenum and Zir percentage of uranium in the pregnant carbonate for the conium from carbonate leach or strip liquors in which succeeding precipitation of uranyl molybdate. they exist together. For example, it is known that zir 60 An improvement of the process comprises the oxidation conium can be precipated free of uranium through pH of molybdenum to its highest valence state before its re control. Unfortunately the required pH range (2.5-3.5) covery. A further improvement of modification (2), results in uranium loss as uranium molybdate if molyb the uranyl molybdate precipitation procedure, includes denum is present because this compound is insoluble in 65 the treatment of the precipitate of step (3) containing the same pH range. It would be possible to remove the Sodium diuranate and some Zirconium hydroxide, with molybdenum from the leach liquor by charcoal adsorption Sulfuric acid at the required pH value to separate the zir before solvent extraction of the uranium, but this would conium from the uranium. The separation can alterna require a large installation and high capital cost in order tively be accomplished by completely dissolving both the to treat approximately 250 gallons per minute, the approxi sodium diuranate and the zirconium hydroxide at pH 1 mate rate of treatment required for commercial feasibility. 70 and separating the two compounds by re-precipitating the Further, as will be pointed out hereinafter, it is known zirconium as the basic sulfate. 3,288,570 al s 4. The detailed description of the operation of the proc A solution of sodium hydroxide is preferable for the ess, including both modifications, is presented herein in pH adjustment to flake caustic because it tends to minimize conjunction with the flow sheets of Figs. 1 and 2, Fig. 1 localized precipitation of sodium diuranate. Any local being the flow sheet for modification (1) and Fig. 2 precipitation which does occur during addition of sodium being the flow sheet for modification (2), that is that 5 hydroxide must be allowed to re-dissolve completely be feature of the invention which is applied to the filtrate fore the temperature is increased, otherwise separation remaining after removal of zirconium as zirconium car from uranium will be poor.
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