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Unite States Patent ?Ice Patented Apr ' assent Unite States Patent ?ice Patented Apr. 23, 1963 l 2 magma, the amounts of sodium carbonate and phosphoric _ , 7 3,086,844 PROCESS, FQR THE MANUFACTURE 0F NEU acid required are alternately introduced in portions into TRALIZATIGN PRODUCTS FROM PHO8 a vessel provided with a stirring means. The sodium car PHORIC ACE AND SODIURT CARBONATE bonate is always introduced as the ?rst component which Klaus Beitz and Franz Rodis, Knapsack, near Coiogue, is suspended in a sodium phosphate solution or suspen Germany, assignors to Knapsack-Griesheim Airtim sion neutralized to the NazHPOlp-stage and uniformly geseilschaft, Knapsack, near Coiogne, Germany, a cor stirred. The phosphoric acid is introduced as ‘the sec poration of Germany ond component in an amount equivalent to the sodium No Drawing. Filed June 7, 1%0, Ser. No. 34,350 Claims priority, application Germany, June 13, 1959 carbonate proportion in order to obtain Na2HPO4. 10 In view of the fact that NazHPOé-solutions or sus 1 Claim. (Cl. 23-4137) pensions do not react with the sodium carbonate with The present invention relates to a process for the manu splitting off of CO2, the sodium carbonate is ?rst mixed facture of neutralization products from phosphoric acid with and ?nely distributed in the liquid mixture and then and sodium carbonate. reacted with phosphoric acid with splitting off of CO2, Phosphoric acid and anhydrous sodium carbonate are 15 whereby the formation of lumps of sodium carbonate is frequently used in industry as starting materials for mak completely avoided. It is admitted that a foam does also ing sodium phosphates, especially condensed sodium form upon adding phosphoric acid to the sodium car phosphates, such as tetrasodium pyrophosphate and so bonate-sodium phosphate suspension, but this foam is not dium tripolyphosphate. In other instances, thermal phos very voluminous and has a very short lifetime as com phoric acid which is obtained by the combustion of ele 20 pared with the ‘foam which is obtained by neutralizing mentary phosphorus is used. The concentration of ther concentrated phosphoric acid with dry sodium carbonate. mal phosphoric acid is very high and generally varies The process of this invention avoids all those di?iculties between 60 and ‘90% H3PO4. which are involved in that case where acid and sodium It is, however, rather di?icult to neutralize such highly carbonate are continuously and jointly added to a solution concentrated phosphoric acid with sodium carbonate. 25 or suspension of disodium orthophosphate, whereby a When the two reactants are mixed with one another, for mixture is obtained that continuously evolves CO2 so that example in a molar ratio of P2O5:Na2O of 3:5 or 1:2, the introduction of sodium carbonate into such mixture the neutralization proceeds initially rather rapidly, but results in lump formation and annoying foam formation. with the formation of a large amount of voluminous In accordance with this invention, phosphoric acid and foam, so that large apparatus provided with ef?cient stir 30 sodium carbonate are neutralized in stepwise manner. ring means have to be employed. In the end, a viscous, The ?rst step is to prepare a small quantity of a solution foamy magma of sodium phosphate solution, crystals of or suspension of disodium orthophosphate, which may monosodium and disodium orthophosphate and unreacted emanate from a previous batch or may be prepared by sodium carbonate, which due to its being in contact with neutralizing phosphoric acid with sodium carbonate while the aqueous phase is agglomerated to form tough lumps, 35 adding water. The aforesaid small amount of disodium is obtained. These lumps of sodium carbonate react ex orthophosphate solution or suspension serves to suspend tremely slowly. In other words, the reaction which and ?nely distribute the ?rst portion of sodium carbon should proceed in the manner illustrated by the summa ate. The sodium carbonate so “wetted” is then neutral tion Equations 1 or 2 below comes prematurely to a ized by adding the ?rst portion of phosphoric acid. This standstill. 40 cycle is repeated until the batch has the desired volume. When the last portion of acid is added, the desired ratio of Na2O:P2O5 is exactly adjusted. The neutralization products prepared by the process of this invention from phosphoric acid and sodium car 45 bonate constitute suspensions of sodium orthophosphates The subsequent reaction of the heterogeneous magma so in a saturated sodium orthophosphate solution. The sus obtained with splitting ol‘r~ of CO2 and a further forma pensions so obtained can be processed in known man tion of sodium phosphate proceeds the more rapidly the ner. Thus, for example, a suspension of disodium ortho more water is present and the higher the temperature. phosphate in saturated disodium orthophosphate solution In order to eliminate these difficulties water is added 50 can be heated to a temperature above 200° C., whereby in carrying out the neutralization reaction on an indus tetrasodium pyrophosphate is obtained. A suspension, trial scale so that the preponderant proportion or the to which contains monosodium and disodium phosphate in tal amount of the neutralization products, ie the primary a molar ratio of 1:2 (which includes the total amount and secondary sodium orthophosphates, are obtained in of the two phosphates), can be heated to a temperature the form of their aqueous solutions. As already men above 300° C. whereby sodium triphosphate is obtained. tioned above, the water has the effect of eliminating the Phosphate suspensions of other composition yield on be difficulties described above. The water may be added by ing heated condensed phosphates of corresponding com diluting phosphoric acid with water prior to neutraliza position or mixtures of condensed phosphates. tion, or by suspending sodium carbonate in water or by Aqueous sodium orthophosphate suspensions can be introducing phosphoric acid, sodium carbonate and water 60 converted by heating into condensed sodium phosphates into one reaction vessel. In processing the sodium phos using apparatus of the most various design or more es phate solutions so obtained in order to produce anhy pecially a rotary kiln or a spraying tower. drous phosphates, especially condensed phosphates, the The following statements show that the process of this water previously added has to be removed by evapora invention is distinctly superior to the known processes tion. The heat balance of such process is therefore un 65 of treating sodium orthophosphate solutions. satisfactory. A disodium orthophosphate solution saturated at ‘90° We have now found that concentrated phosphoric acid C. contains 25.1% P205, 21.9% NaZO and 53.0% H2O. and sodium carbonate can be made into a crystalline In order to prepare from that solution 1 kg. anhydrous magma of sodium orthophosphate without adding water tetrasodium pyrophosphate, 1.13 kg. H2O must be evapo or adding only a small amount of water. The crystalline rated. Contrary thereto, a disodium orthophosphate sus magma is free from sodium carbonate lumps and has pension prepared by the process of this invention con substantially reacted. ‘In order to obtain said crystalline tains, for example, 37.0% P205, 32.3% NaZO and 30.7% 3,086,844 3 4. H2O. In order to prepare from that suspension ll kg. an 197. kg. phosphoric acid hydrous tetrasodium pyrophosphate, 0.443 kg. H2O must 170 kg. sodium carbonate be evaporated, i.e. scarcely 40% of the amount necessary 197 kg. phosphoric acid for processing the solution. When the phosphoric acid had been added in each case, The process of this invention can be used with advan the whole was allowed to stand for 10-15 minutes dur tage in all cases where condensed sodium phosphates are ing which time the sodium carbonate reacted with the prepared from a phosphoric acid which contains H3PO4 phosphoric acid while stirring. After all had been added, in a concentration above 40% or more especially above the suspension was stirred for about 30 minutes; the 50%. Less concentrated phosphoric acids react with suspension was then substantially free from carbon di sodium carbonate with the formation of aqueous solu 10 oxide and could be processed without dii?culty. Alto~ tions of orthophosphates. With the use of a phosphoric gether about 80 kg. water evaporated. The suspension acid of higher concentration, it was hitherto necessary to contained 37.5% P205 and 32.5% NazO, and was con add water in order to obtain sodium orthophosphate verted into anhydrous tetrasodium pyrophosphate in the solutions which are used as intermediates for the produc manner described in Example 1. tion of condensed phosphates. The water added had 15 then to be removed by evaporation. The technical ad Example 3 vance achieved by the process of this invention resides in the fact that no water or only immaterial amounts of In order to prepare sodium tripolyphosphate, a sodium water have to be used. This means that heat energy is orthophosphate suspension was prepared which contained saved during the subsequent heating which is carried out 20 monosodium orthophosphate and disodium orthophos to obtain condensed phosphates. In addition thereto, phate in a molar ratio of about 1:2. The suspension the production capacity of the plant used, for example was prepared in the manner described in Example 2 with a spraying plant or rotatory kiln plant, is considerably the exception that the acid added as last portion was increased. added in an amount greater than indicated in that ex The process of this invention can also be used for 25 ample in order to obtain the desired composition. The manufacture of solid orthophosphates. In this case, the reaction partners were added as follows: suspensions obtained must only be dried. Alternatively, 250 liters water the hot suspensions are allowed to cool, whereby the 450 kg.
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