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Process for the Manufacture of Monopotassium Phosphate

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Process for the Manufacture of Monopotassium Phosphate iropaisciitsa mieiuai"> Office Publication number: v m.-r** — ~- QjM Europeaniropean Patent i^J; A2 Officeffice europeen des brevets PATENT APPLICATION ) EUROPEAN © Int. CI.*: C 01 B 25/30 ) Application number: 87107175.9 ) Date of filing: 18.05.87 © cant HAIFA CHEMICALS LTD. 5) Priority: 04.06.86 IL 79019 APP» : ' Haifa-Bay P.O. Box 1809 Haifa 31018IIL) 3) Dateofpublicationofapplication: ^ Manor.u-». Shalom,ck.i«m Dr.nr 09.12.87 Bulletin 87/50 © lnvent01/ 39 Harishonlm Street 4) Designated Contracting States: Kiryat-Halm(IL) DE ES FR GB IT NL @ p.pko Grjgori> Dr 28/22 Klebanov Street Haifa(IL) @ Inventor: Langham, Adrian 39a Einstein Street Haifa(IL) @ Inventor: Friedman, Nitza 6 Ben-Gurion Avenue Kiryat-Bialik(IL) @ Inventor: Steiner.Amalia 29 Netiv Hen Street Haifa(IL) @ Representative: Rottmann, Maximilian R. c/o Rottmann, Quehl & Zimmermann AG Glattalstrasse 37 CH-8052Zurich(CH) @ Process for the manufacture of Monopotassium Phosphate. invention relates to a process for the manu- aII I III IO IS I C^jUl IUI UIW« Ml ■« ■ w— j "~ — — 9 I © The present bases calcium oxide, calcium car- phosphate using solvent extrac- esxamples of suitable are facture of monopotassium thereof. The monopotassium phosphate According to the invention, the reaction b3onate or mixtures CM tion technique. jbtained is characterized by its high purity. between phosphoric acid and potassium chloride at a o < occurs of temperature between 0 and 100 degrees C. in the presence organic solvent comprising long chain primary, secondary an and 28 if) or tertiary amine, each chain containing between 6 CM carbon atoms. The lower phase containing the mono- , less potassium phosphate is cooled by at least 10 degrees 00 than the reaction temperature whereby pure crystals of monopotassium phosphate are separated and removed. The amine- CM upper phase which contains the organic solvent, hydrochloric acid as well as most of the impurities originally © present in the starting reagents, is treated with a base at a the temperature in the range of 20 to 100 degrees C. whereby UA , , t 1 ( • ' t I t > ■ f ["]■': : :024$2£'7 1 BACKGROUND OF THE INVENTION The present invention relates to a new process for the manufacture of monopotassium phosphate. More particularly, the present invention relates to a new process for the manufacture of 5 monopotassium phosphate using the raw material KC1 as a source of potassium. The direct neutralization of phosphoric acid by potassium hydroxide or carbonate is readily seen to be uneconomic, if the product is to be used as a fertilizer and therefore most of the 10 known methods are based on the utilization of potassium chloride as starting material. The known methods for the manufacture of monopotassium phosphate, from phosphoric acid and potassium chloride, are based t. on the thermal reaction between the two reagents in which the 15 following reaction occurs : H PO + KC1 KH PO + HC1 . 3 4 2 4 However the yield of the said reaction is poor unless a large excess of phosphoric acid is used, in which case the solid product obtained is a double salt: KH PO .H PO which requires a further step for 2 4 3 4 20 its decomposition and recovery of the excess of phosphoric acid. A further drawback in the thermal process is the need for pure starting — e. — materials, as all impurities present in the feed potassium chloride and phosphoric acid are carried through to the solid product. Lastly, the thermal process requires temperatures above 160 degrees lead to the formation C, which cause problems of corrosion and could 5 of insoluble potassium metaphosphate, unless special precautions are * taken such as that proposed in the U.S. Patent Number 3,393,044 wherein organic substances are added to the reaction mixture so as to expel the hydrogen chloride at a lower temperature. However, even the with that improvement the reaction temperature remains in range corrosion remain. .0 of 120 to 160 degrees C, so that the problems Another approach for the manufacture of monopotassium described in the U.S. Patent phosphate at ambient temperature, was wherein chloride is No. 2,902,341 (Baniel et.al.), potassium acid and the mixture of reacted with large excess of phosphoric in the reaction) and the excess of L5 hydrochloric acid (resulted solvent extraction using water phosphoric acid are removed by phosphate is immiscible organic sdlvents. The monopotassium solution resulting after the removal crystallized from the aqueous of this on a commercial of the acids. The implementation process in view of the high'costs 20 scale is questionable, particularly and required to involved concerning the organic solvents energy the hydrochloric acid. separate phosphoric acid from ■ lit I - T- I I f ... < .. • . ' I " < 1 According to U.S. Patent No. 3,661,513 a process is disclosed acid for the manufacture of monopotassium phosphate from phosphoric with and potassium chloride, wherein the reaction mixture is treated the chloride ion. an immiscible secondary amine to selectively extract about 5 The solution recovered has a reduced anion content and a pH of 7. On evaporating the so-treated phosphate solution, solid mentioned monopotassium phosphate can be recovered. The advantage free to exist in this method is that the product is substantially of contaminating anions without the use of the high temperatures LO mentioned by the prior art. SUMMARY OF THE INVENTION It is an object of the present invention to provide a simple It is process for the manufacture of monopotassium phosphate. another object of the present invention to provide a simple process the L5 for the manufacture of monopotassium phosphate without employing relatively high temperatures required in the most of. the prior art methods, thus avoiding completely the danger of metaphosphate for the production. Thus, the invention consists of a process manufacture of monopotassium phosphate which comprises the steps of : 20 (a) reacting phosphoric acid with potassium chloride, in the presence of an organic solvent comprising long chain primary, secondary or at tertiary amine, each chain having between 6 and 28 carbon atoms, 024.8257 4 a temperature in the range of between 0 and 100 degrees C; (b) separating the aqueous lower phase comprising the monopotassium phosphate; and (c) cooling the separated phase obtained in step (b) by at least 10 degrees less than the reaction temperature used in 5 step (a), whereby substantially pure crystals of monopotassium phosphate are separated and removed. The upper layer which contains the organic solvent, amine-hydrochloric acid and impurities originally present in the starting reagents, is treated with a base, and especially from the economic point of view with a calcium L0 constituent selected from calcium oxide, calcium carbonate or mixtures thereof, whereby the amine is regenerated and recycled to the process. This regeneration is carried out generally at a temperature in the range of between 20 to 100 degrees Ci i. Particularly, the regeneration with calcium carbonate, reagent 15 known by its abundancy and relatively low cost, is preferred, the temperature in this case being in the range of between 60 to 100 degrees C. The invention is based on the discovery that by conducting the first step of the process, whereby phosphoric acid reacts with 20 potassium chloride in the presence of an organic solvent containing said amine, at a selected temperature in the range of between 0 and 100 degrees C, avoiding formation of crystals, it is possible to • ; .. - AJ £■ *f O 2 O / 5 phosphate upon obtain with high recovery crystals of monopotassium lease 10 degrees C, and cooling the separated aqueous phase by at below the reaction temperature. preferably between 30 and 60 degrees DESCRIPTION OF THE P?VENTI0N acid and the potassium The reaction between the phosphoric solvent containing the chloride, in the presence of the organic to its completion above mentioned groups of amines, goes smoothly 1. The hydrogen according to the reaction mentioned on page with the amine producing chloride produced thereto, will combine acid. The ratio between the D the corresponding amine-hydrochloric is not critical, but it is phosphoric acid and potassium chloride ratio, since any excess preferred to utilize a substantial equimolar the amine. of phosphoric acid will be extracted by The phosphoric acid to be reacted with the potassium source and its composition 5 ohloride, can come from any convenient substantial The wetjrocess phosphoric can vary over a rather range. acid or fertilizer acid) is acid (also called green acid or merchant being removed in-situ during particularly suitable, the impurities passing into the amine- the reaction with potassium chloride, concentration of phosphoric acid can 20 hydrochloric salt. The thus it can- range from similarly vary over a considerable range; - . 6 as low as about 5% to about 62% by weight P 0 . A 5% concentration 2 5 is somewhat diluted and requires additional processing to concentrate it. Phosphoric acid with a P 0 concentration above 2 5 62% is not readily available and although useful for the process 5 according to the present invention is not preferred. It is generally preferred to employ a phosphoric acid having a concentration of from about 20% to 4056 by weight P 0 . In this range of concentration the 2 5 agitation of the reagents is also optimal. The potassium chloride should be added as a concentrated 10 solution and preferably in a solid form, to minimize the presence of water which might interfere with the crystallization process of monopotassium phosphate. The organic solvent, consists of primary, secondary or tertiary amine containing between 6-28 carbon atoms in each chain .The amines 15 are generally aliphatic in character, although they may be partially aromatic. The aliphatic hydrocarbon groups can be straight, chained or branched chained, saturated or unsaturated, and the hydrocarbon chains (one, two or three) need not necessarily be identical.
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