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Uranium Recovery from Wet-Process Phosphoric Acid

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Uranium Recovery from Wet-Process Phosphoric Acid United States Patent p9] [li] 4,180,545 McCullough et al. [45] Dec. 25, 1979 [54] URANIUM RECOVERY FROM 3,835,214 9/1974 Hurst et al 423/15 WET-PROCESS PHOSPHORIC ACID 3,880,980 4/1975 Warnser 423/15 3,961,027 6/1976 Crossley 423/15 [75] Inventors: John F. McCullough; John F. 3,966,873 6/1976 Elikan et ai 423/15 Phillips, Jr.; Leslie R. Tate, all of 3,975,178 8/1976 McCullough et al 71/34 Florence, Ala. 4,002,716 1/1977 Sundar 423/15 [73] Assignee: Tennessee Valley Authority, Muscle Primary Examiner—Edward A. Miller Shoals, Ala. Attorney, Agent, or Firm—Robert A. Petrusek [21] Appl. No.: 827,517 [57] ABSTRACT [22] Filed: Aug. 25, 1977 A method of recovering uranium from wet-process phosphoric acid wherein the acid is treated with a mix- Related U.S. Application Data ture of an ammonium salt or ammonia, a reducing agent, and then a miscible solvent. Solids are separated from [63] Continuation of Ser. No. 781,216, Mar. 25, 1977, now the phosphoric acid liquid phase. The solid consists of a Defensive Publication No. T970,007. mixture of metal phosphates and uranium. It is washed [51] Int. C1.2 C01G 43/00 free of adhering phosphoric acid with fresh miscible [52] U.S. CI 423/8; 423/10; solvent. The solid is dried and dissolved in acid where- 423/11; 423/15 upon uranium is recovered from the solution. Miscible [58] Field of Search 423/10, 15, 8, 11 solvent and water are distilled away from the phos- [56] References Cited phoric acid. The distillate is rectified and water dis- carded. All miscible solvent is recovered for recycle. U.S. PATENT DOCUMENTS 2,860,031 11/1958 Grinstead 423/10 5 Claims, 2 Drawing Figures WET PROCESS PHOSPHORIC ACID /•vJ REDUCING AGENT £ AMMONIA OR AMMONIUM BICARBONATE REACTOR 1/ 23 24 /V CONDENSER n 17 122 ,14 18 FILTRATION 15 WASHER A,!9 DRYING REACTOR UNIT UNIT UNIT 16 110 /v •20 9 < o- 2/ DISTILLATION PHOSPHORIC ACID SOLVENT UNIT >70% P205 EXTRACTION UNIT hi 12 ' /v ,13 RECTIFICATION UNIT • WATER PRECIPITATION OF URANIUM CONCENTRATE FROM WET PROCESS PHOSPHORIC ACID WITH RECOVERY OF CONCENTRATED PHOSPHORIC ACID J^L WET PROCESS PHOSPHORIC ACID REDUCING AGENT nA AMMONIA OR AMMONIUM BICARBONATE REACTOR Xi 23 24 CONDENSER e\ 17 1.22 .8 14 18 ns jO^L FILTRATION 15 WASHER 19 DRYING REACTOR Jk. UNIT UNIT UNIT 7/0 5 16 A: 220 2! DISTILLATION PHOSPHORIC ACID SOLVENT UNIT >70% P205 EXTRACTION UNIT In 12 Jk1 13 RECTIFICATION UNIT •*» WATER PRECIPITATION OF URANIUM CONCENTRATE FROM WET PROCESS PHOSPHORIC ACID WITH RECOVERY OF CONCENTRATED PHOSPHORIC ACID Fig. I U.S. Patent Dec. 25, 1979 Sheet 2 of 3 4,180,736 EFFECT OF SULFURIC ACID CONCENTRATION ON METHANOL PRECIPITATED CAKE DISSOLUTION Fiq. 2 4,180,545 made from uncalcined rock are black and more objec- URANIUM RECOVERY FROM WET-PROCESS tionable because they contain partially decomposed PHOSPHORIC ACID organic material derived from the rock; however, be- cause their production does not require energy input for The invention herein described may be manufactured 5 a calcining operation their costs are substantially lower. and used by or for the Government for governmental The 1976 wet-process acid production was 6.88 X106 purposes without the payment to us of any royalty tons P2O5 {pert. Trends 1977). This wet-process acid therefor. contained approximately 3,000 tons of yellow cake and This is a continuation of our copending application represents 30 percent of current U.S. yellow cake de- Ser. No. 781,216, filed Mar. 25, 1977, for URANIUM 10 mand which in 1975 was 10,000 tons [Hogerton, J. F., RECOVERY FROM WET-PROCESS PHOS- Nucl. News 19 (8), 73-76 (1976)]. The magnitude of this PHORIC ACID now Defensive Publication No. uranium source, coupled with the recent dramatic ura- T970,007. nium price increase, has greatly stimulated interest in Our invention relates to a method of separating and uranium recovery from phosphoric acid. isolating uranium from phosphoric acid; more particu- 15 Prior art shows that solvent extraction with organo- larly it relates to a process whereby uranium is copre- phosphates is a preferred method of recovering uranium cipitated along with metal phosphates from wet-process from wet-process acid. Capryl pyrophosphate [Cronan, phosphoric acid by addition of ammonia or an ammo- C. S„ Chem. Eng. 66 (9), 108-111 (1959)] as well as nium salt, methanol, and a reducing agent; and still octyl, amyl, and butyl pyrophosphate esters (Long, R. more particularly it relates to a process whereby the 20 S., U.S. Pat. No. 2,882,123) were used for this purpose uranium is recovered in a concentrated form as a solid but have since been abandoned because the esters which is well suited for further concentration and puri- proved to be very unstable and easily decomposed. fication by conventional solvent extraction techniques. Hurst and Crouse [Ind. Eng. Chem. Process Des. De- Uranium oxide, U3O8, or yellow cake as it is often velop. 11 (1), 122-128 (1972)] of Oak Ridge National called, is used primarily for electric power production. 25 Laboratory have developed and tested on a small scale All forecasts show the demand for yellow cake will a uranium solvent extraction process which uses two increase during the remainder of this century [Hoger- extraction cycles with a mixture of di-(2-ethylhexyl) ton, J. F„ Nucl. News 19 (8), 73-76 (1976); Gordon, phosphoric acid and tri-n-octylphosphine oxide dis- Emanuel, Eng. and Min. J. 176 (3), 213-217 (1975); solved in kerosene. These same workers [Ibid, 13 (3), Electr. World 107 (4), 30-33 (1975)]. 30 286-291 (1974)] later developed a similar two-cycle There is considerable doubt about the ability of U.S. extraction process which uses a mixture of mono- and domestic reserves to satisfy this demand [Min. Congr. J. dioctylphenylphosphoric acids dissolved in kerosene 62 (1), 14 (1976); Lieberman, M. A., Sci. 192, 431-436 for the first extraction cycle followed by di-(2-ethyl- (1976); Electr. World 107 (4), 30-33 (1975); Energy Re- hexyl) phosphoric acid and tri-n-octylphosphine oxide sources Report 4 (28), 272 (1976)] and, therefore, it is 35 in the second cycle. , prudent to look for alternate yellow cake sources. Several commercial solvent extraction units are also One such source is wet-process phosphoric acid. The in operation on a limited scale [Ross, R. C., Eng. Min. J. uranium in the phosphoric acid is derived from that 176 (12), 80-85 (1975)]. Although exact details of these contained in the phosphate rock raw material. The ura- processes are not available, they are believed to be nium content in domestic phosphate rock ranges from a 40 based on technology developed at Oak Ridge, supra. low of 12 mg/Kg rock to as high as 399 mg/Kg rock The aforementioned solvent extraction processes [Menzel, R. G., J. Agric. Food Chem. 16 (2), 231 (1968)]. have several disadvantages and defects. As noted, black The uranium concentration in the phosphate ore bodies wet-process acid contains a complex array of rock- now actively mined is about 125 mg/Kg. U.S. phos- derived organic materials. Because these organics emul- phate rock reserves minable by present technology are 45 sify the extractant, their presence in black acid delays or estimated to be near five billion tons and, therefore, the prevents phase disengaging and thus causes losses of the potentially recoverable uranium is near 625,000 tons. valuable extractant to the acid raffinate. Therefore, all Not all phosphate rock is converted to wet-process black acid extraction processes must employ an acid acid, but nevertheless, the uranium in this rock repre- cleanup step prior to uranium extraction. In spite of this sents an impressively large potential uranium reserve. 50 cleanup step, some of the expensive extractant and its When phosphate rock is converted to wet-process kerosene diluent is inevitably lost to the acid where it phosphoric acid by sulfuric acid acidulation, much of may subsequently attack the rubber lining of some pro- the valuable uranium in the rock passes into the phos- cess vessels or cause foaming during the concentration phoric acid. Although the initial oxidation state of the of filter-grade acid to merchant-grade. Although these uranium is variable, air oxidation may convert some of 55 difficulties do not occur when green acids are used, the uranium (IV) to U(VI), the uranyl form. The initial green acids, unfortunately, comprise a small portion of product acid produced by the wet-process method con- total acid production and often contain less uranium tains about 32 percent P2O5 and is known as filter-grade (Hurst, F. J. and Crouse, D. J., 1974, supra). acid. The uranium concentration in the filter-grade acid The inability of these solvent extraction processes to generally lies in the range of 0.1 to 0.2 g/1 [Hurst, F. J. 60 successfully treat the more concentrated merchant- and Crouse, D. J., Ind. Eng. Chem. Process Des. Develop. grade phosphoric acids constitutes another disadvan- 13 (3), 286-291 (1974)]. tage. The requirement that dilute filter-grade acid be Filter-grade acids are frequently concentrated by used means that large volumes of expensive solvent evaporation up to 54 percent P2O5 and are then known extraction reagents are required. as merchant-grade acids. Further concentration to 70 65 Prior art also teaches that precipitation methods may percent P2O5 produces superphosphoric acids. Acids be used to directly recover uranium from phosphoric made from rock which has been calcined at high tem- acid.
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