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United States Patent Office Patented July 6, 1954 2,683,075 UNITED STATES PATENT OFFICE 2,683,075 DIGESTION OF PHOSPHATE ROCK Paul Caldwell, Evergreen Park, I., assignor, by mesne assignments, to Cannac Research and Development Company, Thornwood, N. Y., a joint venture No Drawing. Application June 5, 1951, Serial No. 230,07 Cains, (C. 23-09) 2 This invention relates to the digestion of phOS vention is further characterized by the elimina phate rock and, more particularly, to the recoV tion of a substantial portion of any fluorine con ery of the phosphatic value of such rock. The ponent of the phosphate rock so treated With the invention includes a method of recovering trical result that the end product is particularly Suit cium phosphate from phospate rock in a form 5 able for use as livestock feed Without requiring which is useful both as a fertilizer and as live pyrolytic treatment of the rock or of the final stock feed as well as a method of producing Such product for the elimination of fluorine pursu tricalcium phosphate in admixture with other ant to conventional practice. compounds of known fertilizer Value, and further The method of recovering a non-hygroscopic includes the novel products obtained thereby. O tricalcium phosphate product from phosphate It is conventional practice to recover the phos rock in accordance with my invention comprises phatic value of phosphate rock by digestion of dissolving the tricalcium phosphate component of the rock with Sulfuric acid. Regardless of the rock in an inorganic nitrogenous acid, Sep Whether this digestion is carried Out With Suf arating the resulting phosphorus- and calcium ficient acid to form a product consisting pre 5 containing solution from the acid-insoluble ima dominantly of monocalcium acid phosphate or terial, adding to said solution potassium chloride, with a lesser annount of acid to form a superphos Sodium chloride or sodium sulfate, neutralizing phate, the digestion requires the use of large the resulting phosphorus-, calcium- and potas quantities of the Sulfuric acid. This fact has sium- or SOdium-containing Solution with ann prompted numerous prior investigations to find 20 monia, and recovering the resulting precipitated an alternative reagent or procedure for recover tricalcium phosphate product. The added al ing the phosphatic value of phosphate rock. The kali metal Salt effects precipitation of a large recent critical shortage of Sulfuric acid has placed portion of any fluorine component of the rock a further prennium on the development of a phos in the form of potassium fluosilicate, the latter phate rock digestion operation which does not 25 being advantageously separated from the aque depend upon the use of this acid. ous phase prior to the ammonia-neutralizing step. All previous studies of this problenn have led The precipitated tricalcium phosphate product to the conclusion that such alternative phosphate may be recovered in a form largely free of other rock digestion reagents produce less satisfactory Compounds, or the ammonium and potassium end products than the product obtained by Sull 30 Or Sodium salts present in the solution from furic acid digestion. For example, attempts to which the tricalcium phosphate is precipitated produce a Suitable phosphatic material by diges may be crystallized therefrom so as to form an tion of phosphate rock with nitric acid have been addition to the precipitated tricalcium phosphate. thwarted by the substantial amount of calcium The novel phosphatic product of my invention. nitrate formed along the resulting acid phosphate 35 comprises a.. non-hygroscopic and substantially or Superphosphate. The hygroscopic nature of fluorine-free tricalcium phosphate obtained by calcium nitrate is largely responsible for the wet dissolving the tricalcium phosphate component of and gunny consistency of the phosphate product, phosphate rock in an inorganic nitrogenous acid, and has defeated prior attempts to produce a adding potassium chloride, sodium chloride or phosphatic material from phosphate rock by di 40 Sodium sulfate to the resulting acid solution to gestion with nitric acid. remove fluorine therefrom in the form of pre I have now devised a method of recovering cipitated potassium or sodium fluosilicate, and the phosphatic value of phosphate rock by a pro neutralizing the resulting solution with ammonia, cedure involving digestion of the rock with an to precipitate the tricalcium phosphate product. in Organic nitrogenous acid, such as nitric acid, This product may further contain, in accordance which is nevertheless characterized by the elim With the invention, an ammonium salt and po ination from the phosphatic end product of any taSSium or sodium nitrate obtained by crystal hygroScopic salts which might interfere With the lization from the ammonia-neutralized solution Stability and free flowing characteristics of this from which the tricalcium phosphate is precipi product. The method of my invention effects tated. The resulting product containing these Sequestering of the calcium component of the compounds comprises a highly effective, stable phosphate rock substantially only in the form of and non-hygroscopic fertilizer composition. the ultimate phosphatic compound which, as ex The product obtained by the method of my plained further herein, comprises essentially tri invention is Substantially non-hygroscopic in the calcium phosphate. The novel method of my in 55 accepted sense that it does not absorb a signifi 2,683,075 3. 4 cant amount of moisture from the atmosphere. fluorine component of the rock is largely in the The product does adsorb atmospheric noisture form of a calcium salt, and inasmuch as the rock to some extent but this adsorbed moisture does generally contains other calcium SaitS Such as not impart to the product any significant tend the carbonate, the solution which is neutralized ency to become wet, cake-like or gummy. Al 5 with annonia, will contain an excess of Calcium though the product obtained with the use of over and above that which will combine With the the potassium salt pursuant to the invention is phosphorus to precipitate tricalcium phosphate. less hygroscpic than that, obtained with the use Accordingly, the precipitated product Will Con of the sodium salt, both products can be accu tain other non-hygroscopic calcium compounds rately characterized as substantially non-hygro such as calcium hydrate or possibly tetracaiciun scopic under average United States Weather con phosphate, or both. If, as described an Ore fully ditions. hereinafter, the solution from which the trical The product of my invention is characterized cium phosphate product is precipitated is further by this non-hygroscopicity in the unwashed but suitably concentrated, an annonium Salt and dry state. If the precipitated product were 5 aikali metal nitrate are obtained either for Sepa washed, it Would be expected that it would he rate use or for addition to the precipitated tri non-hygroscopic, but drying of the washed pre calcium phosphate product in the preparation of cipitate causes a Substantial reversion of the a complete fertilizer material. In the latter phosphatic precipitate to an insoluble form event, the annoniura sat and the nitrate both whence it is not readily available for fertilizer 20 provide available nitrogen for the fertilizer, and value. However, when the precipitate is dried where potassium chloride is used as the added without Washing, there is no significant reversion alkali metal salt the resulting potassium initrate of its phosphatic content to an insoluble form forms a particularly Suitable Source of potash. and the resulting dried product is nevertheless The method of my invention is applicable to substantially non-hygroscopic. 25 the treatment of any phosphate rock. Prepa Digestion of the phosphate rock with the in ration of the rock for digestion. With nitric acid Organic nitrogenous acid effects dissolution of is substantially the Sarine as that which prevails the tricacium phosphate component of the rock in the conventional digestion of such rock With with the resulting production of a solution con Sulfuric acid. Thus, Satisfactory resultS can be prising phosphoric acid and calcium nitrate. 30 obtained with rock ground to such a degree Of The acid-insoluble cornponents of the rock settle fineness that, 80-90% will paSS through a 60 aesh out of this Solution and are preferably renoved screen (Tyler standard), although the rock inay before further treatnant of the phosphoric acid be more finely ground so that up to about 95% calciurn nitrate solution. The separated solu Will pass through a 100 resh Screen. As in the tion will further contain most if not all of any 35 case of other aethods of digesting phOSphate florine component of the rock in the form of rock, the degree of Subdivision of the rock is of fluosilicic acid. When the potassium chloride importance only in so far as it affects the late or sodium chloride or sulfate is added to this of its reaction. With the digesting agent. Where Solution in accordance with the invention, a the Speed of reaction can be Sacrificed Sonewhat large portion of this fluorine component of the 40 for ease in Separating the acid-inSouble poi Solution is removed in the form of a precipitate tion of the rock, a coarser starting material Such of the corresponding alkali metal fluosilicate. aS 20 resh rock can be used. The alkali metal salt (an expression which will The digesting agent used in the practice of the be used hereinafter to refer generically to the invention cornprises such inorganic nitrogenous potassium chloride, sodium chloride or sodium 45 acids aS nitric acid or the acid or acid iiixtutes Sulfate) is added in amount not only substan obtained by the passage of gaseous nitrogen tially equivalent stoichiometrically to the fluo Oxides through an aceous redill). Thus, the rine Component of the phosphoric acid solution nitrogenous acid may comprise nitric acid for but also in annount substantially equivalent a commercial Source or it may coprise it;og Stoichiometrically to the calcium nitrate content, 50 enous acids produced at the Site of the digestion of the acid Solution.
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