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Process for the Manufacture of Monopotassium Phosphate

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Process for the Manufacture of Monopotassium Phosphate Patentamt 0 208 422 JEuropaischesEuropean Patent Office Tf) Publication number: B1 Office europeen des brevets EUROPEAN PATENT SPECIFICATION Date of publication of patent specification: 25.04.90 Intel.5: C01 B 25/30 Application number: 86304442.6 Date of filing: 10.06.86 Process for the manufacture of monopotassium phosphate. Priority: 10.07.85 IL 75767 Proprietor: NEGEV PHOSPHATES LTD. P.O. Box 435 Dimona (IL) Date of publication of application: 14.01.87 Bulletin 87/03 Inventor: losef, Alexander 5/12 Hakanaim Street Publication of the grant of the patent: Arad (IL) 25.04.90 Bulletin 90/17 Inventor: Bar-On, Menachem 53/15 Elazer Ben-Yair Street Arad (IL) Designated Contracting States: AT BE CH DE FR GB IT LI NL Representative: Bankes, Stephen Charles Digby etal References cited: BARON & WARREN 18 South End Kensington DE-A-1943 591 London W85BU(GB) US-A-3 697246 US-A-4191734 CM CM 00 o CM o Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall Q. be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been LU paid. (Art. 99(1) European patent convention). Courier Press, Leamington Spa, England. EP 0 208 422 B1 Description 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 direct manufacture of pure 5 monopotassium phosphate which does not involve the use of organic solvents. Monopotassium phosphate is considered a most valuable fertilizer because of its high content of both potassium and phosphate in an available form. The total plant food of this fertilizer is 86.8%, which is higher than most of the other known fertilizers. Besides its very high plant food content, monopotassium phosphate possesses a very low salt index (8.4) compared with 46 for potassium sulfate, 116.3 for 10 potassium chloride and 29.9 for monoammonium phosphate. Another important property of this fertilizer is its very high water solubility (26.6 g/100 g water at 25 degrees C). The significance of high water-solubility for the agricultural value of phosphate fertilizers was proven by field experiments and found especially important for crops with short growing seasons. Monopotassium phosphate was first prepared already in 1821, by the neutralization of phosphoric acid is with a solution of potassium carbonate and crystallizing out the product. Of course this method has only a theoretical interest and can not be considered applicable on a commercial scale for fertilizer purposes. There are known a series of Patents for the manufacture of monopotassium phosphate by heating potassium chloride with phosphoric acid, in various molecular proportions, whereby a double salt of monopotassium phosphate+phosphoric acid resulted. The phosphoric acid is removed by an organic 20 solvent and thus the desired monopotassium phosphate is obtained. Some modification of this method consisted in adding equimolecular proportions of potassium chloride and phosphoric acid into a saturated solution of phosphoric acid and monopotassium phosphate whereby a complete transformation of potassium chloride into potassium phosphate was obtained at 200 degrees C, if an excess of phosphoric acid was used over the ratio of 1 :1. The costs of production according to these methods is comparatively 25 high and up to now there is no commercial plant utilising this approach. The temperature parameter for the reaction between the potassium chloride and phosphoric acid was fully investigated. It was found that at atmospheric pressure, temperatures above 160 degrees C are required for a complete conversion of K+ to potassium monophosphate. However at temperatures above 200 degrees C, water insoluble potassium metaphosphate is produced and in most of the patents it is 30 suggested not to surpass this temperature. In a recent U.S. Patent No. 4,160,657 a process is described for the preparation of monocalcium phosphate and phosphoric acid. According to the process, phosphate rock is reacted with an excess of phosphoric acid, having a concentration in the range of between 25% to 55% by weight P2OS. By cooling the reaction mixture, solid monocalcium phosphate is separated and reacted with a member selected from 35 the group consisting of dipotassium sulfate, monopotassium sulfate or mixtures thereof producing monopotassium phosphate, monopotassium phosphate-phosphoric acid and gypsum. US — A — 3697246 discloses a process wherein monopotassium phosphate is produced by the reaction of phosphate rock or a solubilized form thereof such as monocalcium phosphate, dicalcium phosphate etc., potassium bisulphate, a sufficient excess of sulphuric acid to drive the reaction to completion at 40 to 90°C 40 and optionally fresh or recycled phosphoric acid. Precipitated calcium sulphate is filtered off and monopotassium phosphate is recovered from the filtrate by concentration and filtration or, more preferably, by extraction with an organic solvent. In order to complete the state of the art in this field, it would perhaps be interesting to mention the process for the manufacture of monopotassium phosphate from potassium chloride and phosphoric acid 45 (as described in Israeli Patent No. 9539) carried out at ambient temperature. According to this process, a great excess of phosphoric acid is utilized, and the mixture of phosphoric acid and hydrochloric acid is removed by solvent extraction using water immiscible organic solvents. The monopotassium phosphate is crystallized from the aqueous solution resulting after removal of the acids. The process is indeed quite elegant, but its implementation on a commercial scale is quite questionable particularly in view of the high so costs involved concerning the organic solvents and energy required to separate the phosphoric acid from the hydrochloric acid. It is an object of the present invention to provide a simple process for the manufacture of monopotassium phosphate which does not require the use of organic solvents for separation of phosphoric acid, and which does not require temperatures above 100°C, and thus avoids completely the 55 danger of metaphosphate production. The present invention consists in a process for the manufacture of substantially pure monopotassium phosphate without the use of organic solvents which comprises the steps of: (a) reacting, at a temperature in the range from 40 to 100°C, monopotassium sulphate with a phosphate constituent comprising phosphate rock, dicalcium phosphate or a mixture thereof in the presence of 60 phosphoric acid to form a slurry containing phosphoric acid, monopotassium phosphate and calcium sulphate and separating out the calcium sulphate to obtain a filtrate containing phosphoric acid and monopotassium phosphate; and (b) recovering monopotassium phosphate from the filtrate, characterized in that (i) the reaction of step (a) is carried out in at least two stages, comprising a first stage wherein 65 monopotassium sulphate reacts with part of the phosphate constituent in the presence of phosphoric acid EP 0 208 422 B1 and in the absence of free sulphuric acid, and a second stage wherein the reaction product from the first stage is reacted with a further portion of phosphate rock or dicaicium phosphate to produce the said slurry; (ii) the amount of phosphoric acid in the filtrate is in a range from 5 to 35% of the total P2O5 present at the end of step (a) and s (iii) step (b) is carried out by neutralizing at a pH from 3 to 7 the filtrate obtained in step (a) with a calcium-containing compound comprising Ca(OH)2, CaO, CaCO3 or a mixture thereof to obtain a slurry containing dicaicium phosphate and separating out the dicaicium phosphate to leave a filtrate from which substantially pure monopotassium phosphate is crystallized. The preferred amount of phosphoric acid in step (a) should be in the range of 10 to 35% of the total 10 . P2O5 present at the end of the step. Above 35% the process is still operable, but any excess above this value is actually a waste of P2O5. The concentration of the P2O5 is not critical and can be selected in a very broad range. Using the above steps, the product obtained will not be accompanied by phosphoric acid (double salt monopotassium phosphate-phosphoric acid) as encountered in the prior art methods. One of the characteristics of the system in the present invention is the absence of monocalcium is phosphate. This is a result of an excess of the sulphate ion which is present therein, which excludes the formation of monocalcium phosphate, due to the formation of the insoluble calcium sulphate. The excess of sulphate ion has also a beneficial effect on the generation of well-shaped crystals of gypsum with the consequence of their easy filtration, washing and separation. The starting reagent for the present invention is monopotassium sulphate. As is known/this salt is 20 easily obtained in the reaction between potassium chloride and sulphuric acid. As appears from the reactions presented below, the reaction between potassium chloride and sulphuric acid occurs in two distinct steps: — (1) KCI+H2S04-»KHS04+HCI (AH=-3.91 Kcal/mole). 25 (2) KCI+KHSO4-*K2SO4+HCI (AH=+17.1 Kcal/mole). The first reaction for the formation of monopotassium sulfate occurs smoothly and is much more easily performed (being exothermic) than the second one of dipotassium sulfate formation (which is 30 endothermic). The proper conditions for the preparation of monopotassium sulfate are well known from the prior art, its preparation being not considered part of the present invention. As known, the temperatures at which it takes place are low enough to permit the use of corrosion-resistant plastics, thus reducing the capital costs.
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