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The Two Tortoitu Muuuuuuuuu THETWO TORTOITUUSMUUUUUUUUU 20180111839A1 ( 19) United States (12 ) Patent Application Publication ( 10) Pub . No. : US 2018 /0111839 A1 CHASTAIN et al. (43 ) Pub . Date : Apr. 26 , 2018 ( 54 ) METHODS FOR THE PRODUCTION OF Publication Classification POTASSIUM SULPHATE FROM (51 ) Int . CI. POTASSIUM - CONTAINING ORES AT HIGH COID 5 / 10 (2006 .01 ) AMBIENT TEMPERATURES COID 5 / 16 ( 2006 . 01) COIF 5 / 40 ( 2006 .01 ) (71 ) Applicant: Yara Dallol BV , HJ Sluiskil (NL ) (52 ) U . S . CI. (72 ) Inventors: Richard W . CHASTAIN , Montreal CPC . .. .. C01D 5 / 10 ( 2013. 01 ) ; C01F 5 /40 (CA ) ; Ingrid T . BUCKHURST , (2013 .01 ) ; C01D 5 / 16 (2013 . 01 ) Porsgrunn (NO ) ; Antoine LEFAIVRE , (57 ) ABSTRACT Montreal ( CA ) ; Thomas H . NEUMAN , There are provided methods for the production of potassium Montreal (CA ) sulphate . The methods comprise contacting an aqueous potassium - and sulphate -containing composition with mag nesium chloride (MgC1 , ) , thereby obtaining a composition ( 73 ) Assignee : Yara Dallol BV , HJ Sluiskil (NL ) comprising kainite ; optionally concentrating the kainite from the composition ; reacting the kainite with magnesium (21 ) Appl . No. : 15 /569 , 207 sulphate (MgSO4 ) and potassium sulphate ( K ,S02 ) so as to convert the kainite into leonite (K2SO4 .MgSO4 . 4H20 ) ; (22 ) PCT Filed : May 4 , 2016 optionally contacting the leonite with water to remove excess MgSO4; and contacting the leonite with water so as ( 86 ) PCT No. : PCT /EP2016 / 059952 to leach the MgSO4, contained in the leonite , and to at least $ 371 (c )( 1 ), substantially selectively precipitate potassium sulphate ( 2 ) Date : Oct. 25 , 2017 (K2SO4 ) . The method according to the invention can be operated at higher temperatures , in particular at tempera ( 30 ) Foreign Application Priority Data tures above 35° C . and does not require a cooling step at 20 to 25° C . The method produces potassium sulphate with a May 8 , 2015 (NO ) .. .. 20150571 low amount of chloride. Patent Application Publication Apr . 26 , 2018 US 2018 / 0111839 A1 Solution mining brine ( K ,Mg2 + , Nat, cl, 5042) S. Kalnite MgCl2 Purge Evaporation , formation , . concentration . > Halite Tailings (Halite , Further Kainite concentration : MgSO4) crushing , slurrying and flotation Tailings8 S wash 5 Kainite ,halite ,MgSO4 Conversion into Leonite (K , SO , *MgSO * 4H20 ) Part of the flow (Excess MgSO4 ) Leonite Purge Brine - - - Leonite wash (Excess MgSO4Y) K , 50 Mother Liquor K , SO , Crystallization Sweet water K SO Fig . 1 US 2018 /0111839 A1 Apr. 26 , 2018 METHODS FOR THE PRODUCTION OF and crude carnallite is produced as an intermediate using a POTASSIUM SULPHATE FROM cooling step at ambient temperature ( 25º C . ) . POTASSIUM -CONTAINING ORES AT HIGH [0011 ] None of the known processes is able to operate AMBIENT TEMPERATURES entirely at temperatures above 35° C . , using a minimum of water as well as electrical power , and can be operated with TECHNICAL FIELD different potassium deposits or a mixture thereof. [0012 ] The current invention discloses a method which [0001 ] The present disclosure relates to improvements in could be operated at higher temperatures , in particular at the field of methods for preparing potassium sulphate from temperatures above 35° C . and which does not require a potassium -containing ores. process step operated at a temperature below 35° C ., in particular a cooling step at 20 to 25° C . Although the use of BACKGROUND OF THE DISCLOSURE the method according to the invention is not limited to said [ 0002 ] Potassium is the third major plant and crop nutrient temperatures, the method according to the invention can be after nitrogen and phosphorus. It has been used since antiq advantageously used in mining areas which are situated in uity as a soil fertilizer (about 90 % of its current use ) . It is warm or hot climates (such as the Dallol region in Ethiopia ) . mined throughout the world from potassium deposits , either Furthermore , the method of the invention is very energy in underground or surface mines , wherein potassium is efficient as it does not use mechanical cooling , nor heating found in different chemical forms, such as carbonate , chlo devices, and it uses low amounts of freshwater. Therefore , ride , sulphate and nitrate . Each of these chemical forms the method according to the invention is especially suitable requires a different chemical procedure to extract and con for use in remote location where access to energy and centrate the potassium from the deposits . auxiliary systems is difficult . Furthermore , the method [0003 ] Since potassium sulphate (K2SO4 ) does not contain according to the invention may start from a solution , chloride , it is the preferred choice for crops , which are obtained by solution mining such that different potassium sensible to chloride , and which include coffee and several salts and mixtures thereof can be processed . It is a further fruits and vegetables. Also crops that are less sensitive to object of the process to minimize water usage , as well as to chloride may still require potassium sulphate for optimal minimize power usage and cooling water. The process can growth if the soil accumulates chloride from irrigation be operated economically in a hot, dry area that has limited water. resources available . [ 0004 ] Various methods have been proposed so far regard [0013 ] The method according to the invention is based on ing the production of potassium sulphate ( also called “ sul the finding that schoenite does not form at temperatures phate of potash ” or SOP ) and various routes have been above 35° C . , more in particular above 40° C . and under the explored . For example , solution mining of sylvinite ( a conditions of the described method , such that a method for mixture of KCl and NaCl) for the production of KC1 is the production of potassium sulphate was developed , based known and is a technology that is practiced , a . o . in cold on the formation of leonite . climate areas , for example , in Saskatchewan , Canada . [0005 ] U . S . Pat. No . 2 , 902 ,344 (SINCAT SPA , 1959 ) SUMMARY OF THE INVENTION discloses a process for the recovery of potassium sulphate [0014 ] According to one aspect of the invention , there is from kainite ore (KC1 .MgSO4 . H20 ) containing sodium provided a method for the production of potassium sulphate , chloride as an impurity . The kainite ore is converted into comprising the consecutive steps of: schoenite by mixing with the mother liquor containing some 10015 ) Ia ) contacting an aqueous potassium - and sulphate potassium sulphate at 20° C . , and further decomposed into containing composition with magnesium chloride (MgCl2 ) , SOP using warm water , preferably at about 45° C . thereby obtaining a composition comprising kainite (KC ) . [0006 ] DE 1592035 A1 (SINCAT SPA , 1970 ) discloses a MgSO4. 2 .75 H2O ) ; process for the recovery of potassium sulphate from kainite [ 0016 ] IIa ) optionally , concentrating the kainite from the ore using a langbeinite ( K ,Mg2 ( SO4) 3 ) suspension which is composition , obtained in step Ia ; processed into schoenite ( K , SO4. MgSO4 .6H2O ) and leonite 10017 IIIa ) reacting the kainite , obtained in step la or Ila , (K2S04 . MgSO4 . 4H20 ) at 20 to 35º C . with magnesium sulphate (MgSO4 ) and potassium sulphate [0007 ] U . S . Pat . No . 3 , 058 ,806 (Metallgesellschaft , 1962 ) ( K , SO . ) so as to convert the kainite into leonite ( K , SO . discloses a process for the production of SOP from kainite MgSO4. 4H20 ) ; by the dissolution of kainite in hot water , which comprises [0018 ] IVA ) optionally , contacting the leonite , obtained in a cooling step to form the schoenite crystals and reacting it step IIIa , with water to remove excess MgSO4; and with potassium chloride. [00191 Va ) contacting the leonite , obtained in step IIIa or [0008 ] U . S . Pat . No . 3 ,589 , 871 (GREAT SALT LAKE IVa , with water so as to dissolve leonite and / or leach the MINERALS , 1971 ) discloses a method of producing kainite MgSO4, contained in the leonite , and to at least substantially from natural brines containing potassium by adding MgCl, selectively crystallize potassium sulphate (K2SO4 ) . and using evaporation in solar ponds to precipitate kainite [0020 ]. According to another aspect of the invention , there and carnallite (KMgCl2 . 6 (H2O ) ) . is provided a method for the production of potassium [ 0009 ] U . S . Pat . No . 3 ,634 , 041 (GREAT SALT LAKE sulphate , comprising the consecutive steps of: MINERALS , 1972 ) discloses a process for the production of 10021 ] Ib ) contacting an aqueous potassium -containing SOP from essentially pure schoenite . composition , further comprising sodium chloride , with mag [ 0010 ] WO 05 /063626 A1 ( Indian Council of Scientific nesium chloride (MgCl2 ) , thereby obtaining a composition Industrial Research , 2005 ) discloses a process for the pro comprising kainite (KC1 .MgSO4 . 2 .75 H2O ) ; duction of SOP from bittern comprising a step wherein [0022 ] IIb ) optionally , concentrating the kainite from the kainite is converted into schoenite , aqueous CaCl, is used composition , obtained in step Ib and controlling the con US 2018 /0111839 A1 Apr. 26 , 2018 centration of sodium chloride, present in the composition [0036 ] According to one aspect of the invention , the comprising kainite so as to maintain the concentration of method according to the invention may comprise contacting sodium chloride below about 10 % by weight on dry matter one or more potassium - and
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