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Selective Extraction of Potassium Chloride From

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Selective Extraction of Potassium Chloride From (19) TZZ _Z _T (11) EP 2 751 028 B1 (12) EUROPEAN PATENT SPECIFICATION (45) Date of publication and mention (51) Int Cl.: of the grant of the patent: C01D 3/06 (2006.01) C01D 3/08 (2006.01) 09.12.2015 Bulletin 2015/50 (86) International application number: (21) Application number: 13722048.9 PCT/IB2013/000582 (22) Date of filing: 02.04.2013 (87) International publication number: WO 2013/150363 (10.10.2013 Gazette 2013/41) (54) SELECTIVE EXTRACTION OF POTASSIUM CHLORIDE FROM SCHOENITE END LIQUOR EMPLOYING TARTARIC ACID AS SAFE, BENIGN AND RECYCLABLE EXTRACTANT SELEKTIVE EXTRAKTION VON KALIUMCHLORID AUS SCHÖNIT- ENDFLÜSSIGKEIT MIT EINER WEINSÄURE ALS SICHEREM, GUTARTIGEM UND WIEDERVERWENDBAREM EXTRAKTIONSMITTEL EXTRACTION SÉLECTIVE DE CHLORURE DE POTASSIUM À PARTIR D’UNE LIQUEUR FINALE DESCHOENITE UTILISANT DE L’ACIDE TARTRIQUE COMME AGENT D’EXTRACTION SÛR, SANS DANGER ET RECYCLABLE (84) Designated Contracting States: • SOLANKI, Jignesh AL AT BE BG CH CY CZ DE DK EE ES FI FR GB Bhavnagar 364 021 Gujarat (IN) GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO • BRAHMBHATT, Harshad, Raman PL PT RO RS SE SI SK SM TR Bhavnagar 364 021 Gujarat (IN) • CHUNAWALA, Jatin, Ramesh (30) Priority: 02.04.2012 IN DE06062012 Bhavnagar 364 021 Gujarat (IN) • ERINGATHODI, Suresh (43) Date of publication of application: Bhavnagar 364 021 Gujarat (IN) 09.07.2014 Bulletin 2014/28 • PAUL, Parimal Bhavnagar 364 021 Gujarat (IN) (73) Proprietor: Council of Scientific & Industrial Research (74) Representative: Fairbairn, Angus Chisholm New Delhi 110 001 (IN) Marks & Clerk LLP 90 Long Acre (72) Inventors: London • MAITI, Pratyush WC2E 9RA (GB) Bhavnagar 364 021 Gujarat (IN) • GHOSH, Pushpito Kumar (56) References cited: Bhavnagar 364 021 Gujarat (IN) WO-A1-2007/054953 WO-A1-2008/020457 • GHARA, Krishna, Kanta DE-C- 694 480 US-A- 2 617 710 Bhavnagar 364 021 Gujarat (IN) US-A- 2 710 789 US-B2- 7 041 268 Note: Within nine months of the publication of the mention of the grant of the European patent in the European Patent Bulletin, any person may give notice to the European Patent Office of opposition to that patent, in accordance with the Implementing Regulations. Notice of opposition shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention). EP 2 751 028 B1 Printed by Jouve, 75001 PARIS (FR) 1 EP 2 751 028 B1 2 Description implementation of the process poses serious operational & environmental issues owing to hazardous nature of FIELD OF THE INVENTION dipicryl amine. [0007] Thus a need was felt to devise a process to [0001] The present invention provides safe and effi- 5 selectively extract potassium from bittern & other K bear- cient extraction process for the recovery of near saturat- ing aqueous solutions for production of potassic fertiliser ed solution of KC1, free of impurities useful for production using a recyclable, benign & environmentally safe ex- of sulphate of potash (SOP) and ammonium sulphate tractant. using bittern, ammonia & hydrochloric acid as raw ma- [0008] It was quite well known that potassium bitartrate terials and employing tartaric acid as the safe, benign, 10 (cream of tartar) has substantially lower solubility than recyclable & selective extractant for recovery of potassi- sodium bitartrate. Cream of tartar, a derivative of wine um from intermediate process stream. More particularly, industry attracted lot of attention, particularly in regard to the invention eliminates the need for natural/solar evap- recovery of tartaric acid & potassium salts. oration of intermediate streams for recovery of potassium [0009] Reference may be made to US patent no. chloride and thereby reduces dependency on seasonal 15 957,295, May 10, 1910 by Alberti A. et al. which teaches weather variations & land resources. Further the present about process of recovering potash salts from wine lye invention derives beneficial synergies and advantages (raw cream of tartar). Reference may be made to US of integrated approach of the process. patent no. 2,710,789, June 14, 1955 by Boeri G. et al. which teaches about method for preparing substantially BACKGROUNDAND PRIOR ARTOF THE INVENTION 20 pure potassium nitrate from raw tartaric materials. [0010] Reference may be made to US patent no. [0002] Potassium bearing aqueous solutions, viz., sea 3,069,230, Dec 18, 1962 by Pescarolo B. et al. which bittern left after recovery of common salt in solar salt work teaches about process for extracting Tartaric Acid and is a rich source of the element (20-25 g/lit potassium chlo- Potassium in form pure potassium nitrate in the cold from ride). Similarly, the natural bittern of Greater Rann of25 tartaric acid, without the need of previous roasting of the Kutchh (Gujarat, India) is a perennial source of potassi- tartaric raw material. um. Evaporite based technologies rely on solar evapo- [0011] The above mentioned inventions used wine ration of bittern and require large amount of land area lees (raw cream of tartar - crude potassium bitartrate) as apart from favourable climatic conditions for consistent the potash bearing raw material. Moreover, the aforesaid production of the potassic feedstock. 30 patents do not teach us about recycling of the extractant, [0003] Reference may be made to U S patenti.e., tartaric acid. 7,041,268, May 9, 2006 by Ghosh P. K. et al. which teach- [0012] Reference may be made to the paper "Adapta- es about an integrated process for the recovery of sul- tion of the bitartrate method for the estimation of potas- phate of potash (SOP) from sulphate rich bittern. How- sium in sea bittern" by Shukla, B. K. et.al (http://www.csir- ever, this process depends on evaporation of intermedi- 35 central.net/index.php/record/view/88029) which teaches ate streams for production of potassium chloride, re- about the method for estimation of potassium content of quired in the process. This creates additional demand bittern, by precipitating potassium as potassium for large amount of land area apart from need effective bitartrate. Although developed as a method for analysis, integration of plant & field operations. the main disadvantages for practising this process are [0004] Selective extraction of potassium offers a prac- 40 that it requires addition of methanol/ethanol, & sodium tical & implementable alternative to overcome the afore- hydrogen tartrate apart from tartaric acid for precipitation mentioned impediments faced by evaporite based tech- of potassium bitartrate. nologies. [0005] Reference may be made to U S patentOBJECTS OF THE INVENTION 2,617,710, Nov 11, 1952 by Kielland J. et al. which teach- 45 es an efficient method for extraction of potassium from [0013] The main object of the invention is to devise a dilute solution, e.g., sea water, using dipicryl amine as safe and efficient extraction process for the recovery of extractant. However, commercial implementation of the near saturated KCl solution, free of impurities, from sch- process poses serious operational & environmental is- oenite end liquor (SEL), obtained from the decomposition sues owing to hazardous nature of dipicryl amine. 50 of kainite mixed salt into schoenite as disclosed in the [0006] Reference may be made to WO-A-prior art, thereby eliminating the need for i) evaporation 2007/054953 (U S patent 8,182,784, May 22, 2012 by of intermediate process stream, i.e., SEL and ii) down- Paul P. et al.) which teaches an efficient method for ex- stream processes for recovery of potassium chloride, traction of potassium from SEL, the potassium rich inter- viz., evaporite harvesting, carnallite decomposition, hot mediate stream generated upon decomposition of kainite 55 leaching of crude potash etc. type mixed salt, as described in U S patent 7,041,268, [0014] Another object is to selectively precipitate po- in the form of potassium chloride, using dipicryl amine tassium from SEL, as potassium bitartrate, with high re- as extractant. However, in this instance also, commercial covery efficiency. 2 3 EP 2 751 028 B1 4 [0015] Another object is to use tartaric acid and salts Figure 1 represents improved process for recovery thereof as safe, benign and recyclable extractant. of sulphate of potash (SOP) from kainite mixed salt [0016] Another object is to take advantage of optically with selective extraction of potassium chloride from active isomers of tartaric acid to reduce impurity in po- schoenite end liquor employing tartaric acid as safe, tassium bitartrate & to enhance recovery of near saturat- 5 benign and recyclable extractant. ed KCl solution from solid potassium bitartrate. Figure 2 represents process for recovery of residual [0017] Another object is to carry out the core process tartaric acid from intermediate streams. steps at ambient temperature. [0018] Anotherobject isto generate near saturatedKCl SUMMARY OF THE INVENTION solution, by reacting potassium bitartrate with magnesi- 10 um hydroxide & magnesium chloride. [0029] Accordingly, present invention provides a safe [0019] Another object is to reuse the magnesium tar- and efficient extraction process for the recovery of near trate, obtained during production of near saturated KCl saturated solution of potassium chloride (KCl), free of solution, for subsequent cycles of selective precipitation impurities wherein said process comprises the steps of: of potassium from SEL. 15 [0020] Another object is to selectively precipitate po- i. providing schoenite end liquor (SEL) containing tassium from potassium rich aqueous solutions, includ- 4.0-5.5% w/v K + obtained from the decomposition of ing but not limited to, bittern, seaweed Kappaphycus( kainite mixed salt into schoenite by known method; alvarezii) sap etc., as potassium bitartrate. treating schoenite end liquor containing 4.0-5.5% [0021] Another object is to minimise tartaric acid loss 20 w/v K+ as obtained in step (i) with a sub-stoichiomet- in the potassium depleted SEL & potassium bitartrate ric amount of tartaric acid half-neutralized with washings by precipitating the same as calcium tartrate, Mg(OH)2, to obtain potassium bi-tartrate and potas- using calcium carbonate, calcium chloride, gypsum etc.
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