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(12) Patent Application Publication (10) Pub. No.: US 2014/0255278 A1 Bakke Et Al US 20140255278A1 (19) United States (12) Patent Application Publication (10) Pub. No.: US 2014/0255278 A1 Bakke et al. (43) Pub. Date: Sep. 11, 2014 (54) METHODS TO RECOVER CESIUMOR (60) Provisional application No. 61/772,946, filed on Mar. RUBDIUM FROMISECONDARY ORE 5, 2013. (71) Applicant: Cabot Corporation, Boston, MA (US) Publication Classification (72) Inventors: Bart Bakke, The Woodlands, TX (US); (51) Int. Cl. Claude Deveau, Pinawa (CA) C22B 26/10 (2006.01) BO2C23/08 (2006.01) (73) Assignee: Cabot Corporation, Boston, MA (US) (52) U.S. Cl. CPC ................. C22B 26/10 (2013.01); B02C 23/08 (21) Appl. No.: 14/277.914 (2013.01) USPC ............ 423/202; 209/552; 209/10; 209/44.1; (22) Filed: May 15, 2014 241/24.1 (57) ABSTRACT Related U.S. Application Data A method to recover cesium, rubidium, or both from second (63) Continuation of application No. 14/191,468, filed on ary ore is described and involves using scans and sorting Feb. 27, 2014. techniques. Refined secondary ore is further described. : Si.23 C. c. c. g. WSg. ...c. 4 3 4. 3 - Chute or Moving Bett 2. Vibratory Pan ------------------------- -------...---------- -------------------------...--- --- - - -va-voom myr v. m- , 4-x-ray sensor r“s ; ry 5 image? - \,-- W---m i Signal Y 3. A. m t www.------------ - Processor & Dual Energy Beam --- ...i 4. - . NW --- \ - N-D - a3 ?y\l- 2 ww...w-xwr- . 6. High Speed Air Jet --A - 7 - 7-Separated Process Streams 8- Remote User interface Patent Application Publication Sep. 11, 2014 Sheet 1 of 4 US 2014/0255278 A1 Fig. 1 19 10 - a as a 14 12 divide ore into size fractions Calibrate/train Sorter with training sets of size fractions pass respective size fractions through calibrated first sorter and separate into Grade 1 or Grade 2 pieces 16 18 Grade 1 pieces Grade 2 pieces (in size fractions) 2O 22 further crushing pass respective Grade and/or calcining 2 size fractions through Second Sorter and separate into Grade 2A O and Grade 2B pieces calcining and/or tailings/recycle? 34 acid treatment of further Crushing Grade 1 and/or or sort again Grade 2A pieces k - - - - - - 32 36 recover Cs2O from slurry Convert to One Or more Cesium Salts 40 Convert to Cs make brine with 42 formate CS formate 44 Patent Application Publication Sep. 11, 2014 Sheet 2 of 4 US 2014/0255278 A1 Fig. 2 s: x. 5. E. : :. -. 3.. 3-chute or Moving Belt 2. Vibratory Pan ----------------------------------- - - -------------------------- --al-Masuluw-W------a ----------------------------- ---....... ----------u-...-, s: mm. f -------4. X-Ray Sensor f y 3 --- y 5 image? -- --- \- Signal N- H A. m - -------...------------------ Processor & Dual Energy Bean www.www.m. j --------- Y, 7-Separated Process Streams User interface Patent Application Publication Sep. 11, 2014 Sheet 3 of 4 US 2014/0255278 A1 s Patent Application Publication Sep. 11, 2014 Sheet 4 of 4 US 2014/0255278 A1 : & S. $83.88 &n Sis: si' s 38s issy $838ts as Six sess US 2014/0255278 A1 Sep. 11, 2014 METHODS TO RECOVER CESUMOR cessing of the ore (e.g., beginning with acid digestion). Add RUBIDIUM FROMISECONDARY ORE ing to this challenge is the variable presence of the levels of these lighter alkalis, as introduced with the ore prior to wet 0001. This application claims the benefit under 35 U.S.C. chemical processing. S119(e) of prior U.S. Provisional Patent Application No. 0007. These same problems also can exist with rubidium 61/772,946, filed Mar. 5, 2013, which is incorporated in its containing ore or ore containing cesium and rubidium. entirety by reference herein. 0008 Accordingly, there is a need in the industry to develop methods for recovering the highly sought and valued BACKGROUND OF THE INVENTION minerals bearing cesium, rubidium, or both, from secondary 0002 The present invention relates to cesium or rubidium ore, also referred to as cesium-containing secondary ore. or both and the recovery of these elements from secondary There is a further need to create methods that will signifi ore. The present invention further relates to a purified ore that cantly reduce the content of minerals bearing lithium, and the contains cesium and a unique combination of others minerals other lighter alkali, impurities and other mineral and/or metal and/or elements. impurities in the recovered cesium, rubidium, or both, so as to 0003 Cesium salts, such as cesium formate, are increas avoid the significant challenges of wet chemical processing, ingly being discovered as useful components or additives for as well, the viability of brine products, as per those problems a variety of industrial applications, such as in the hydrocarbon described above. recovery areas. However, deposits of “primary' ore, that is, ore that contains high amounts of cesium with insignificant SUMMARY OF THE PRESENT INVENTION amounts of undesirable impurities, are rare, and operators 0009. A feature of the present invention is to provide a have long sought techniques to enhance recovery of cesium method to effectively recover cesium, rubidium, or both, from and/or rubidium from known deposits of secondary ore con secondary ore. taining cesium and/or rubidium. 0010. A further feature of the present invention is to pro 0004. However, cesium-containing secondary ore, while vide methods to utilize the cesium, rubidium, or both, recov available, presents major problems with regard to recovering ered from secondary ore in the production of cesium-contain the cesium from Such ore. For instance, the expense of recov ing fluids, such as cesium formate and the like. ering significant amounts of cesium from low yield ore can be 0011. An additional feature of the present invention is to quite time consuming and expensive based on known meth provide a method to recover cesium, rubidium, or both, from ods. Also, with known techniques, it is very difficult and secondary ore and yet control the amount of lithium and/or expensive to separate cesium from certain undesirable metals metals or minerals that would be otherwise present in the or minerals that can typically be found with deposits of recovered ore. cesium-containing secondary ore. For instance, many 0012. A further feature of the present invention is to pro cesium-containing secondary ore deposits have significant vide a crushed cesium-containing purified ore that contains lithium containing minerals, such as, but not limited to, phos high amounts of cesium and controlled amounts of lithium or phate minerals, such as Amblygonite, Montebrasite, and/or lithium ions and having desirable cesium oxide-to-phospho cesium-Substituted Lithiophosphates. If the phosphate min rus oxide weight ratios. erals which contain significant amounts of lithium, and fre 0013 Additional features and advantages of the present quently sodium, are not significantly separated from the sec invention will be set forth in part in the description that ondary ore, the lithium can then present serious impediments follows, and in part will be apparent from the description, or to the commercial use of the cesium-containing fraction of may be learned by practice of the present invention. The the secondary ore in a variety of industries, such as in the features and other advantages of the present invention will be hydrocarbon recovery area with regard to fluids, such as realized and attained by means of the elements and combina drilling fluids, completion fluids, packer fluids, and the like. tions particularly pointed out in the description and appended 0005. In more detail, one beneficial use of cesium is as claims. cesium formate in solution to create high density well fluids 0014) To achieve these and other advantages, and in accor which are extremely useful in deep drilling oil and gas wells. dance with the purposes of the present invention, as embodied If the lithium is present at excessive levels in the fluids, the and broadly described herein, the present invention relates to fluid cannot be manufactured with a sufficient amount of a method to recover cesium, rubidium, or both from second cesium in Solution to achieve the high fluid density required ary ore. The secondary ore can contain 25 wt % Cs-O or less for well drilling fluids. If the lithium levels exceed critical based on overall weight of the secondary ore (such as 15 wt % parameters, the cesium-containing salt will precipitate out of or less or 10 wt % or less) and the majority of the secondary Solution before reaching the needed density to work as a ore can include pieces having at least one dimension that is suitable well fluid, which will make the fluid unsuitable for over 5 inches. The method can include crushing the secondary hydrocarbon recovery. ore to obtain crushed ore comprising individual pieces. Each 0006. In using primary ore sources, the presence of lithium individual piece has a size capable of passing through a mesh/ is not a significant problem because the cesium-containing screen or barfscreen of 3 inches. Or, one can start with the primary ore deposits, namely, pollucite, can be recovered crushed ore from a source or supplier. The method includes without any significant levels of lithium-containing phos passing the crushed ore through a first sorter to conduct a first phate minerals being present. Thus, this problem is unique to sorting at a feed rate of at least 1 ton/hour, wherein the first cesium-containing secondary ores. In addition, if the lithium sorter determines whether each individual piece of crushed is not substantially removed from the secondary ore before ore is a “Grade 1 piece' or "Grade 2 piece.” based on the first chemical processing to recover cesium, the lithium, as well as Sorter conducting at least one scan of each individual piece any Sodium, can be excessively challenging to remove from and determining or calculating atomic number and/or mate the cesium during traditional downstream wet chemical pro rial density of each individual piece, wherein said “Grade 1 US 2014/0255278 A1 Sep.
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