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US2940823.Pdf June 14, 1960 A. H. REDIES ETAL 2,940,823 PRODUCTION OF POTASSIUM MANGANATES Filed Oct. i0, 1956 MnO2 AC. KO blo VAPOR KMNO-KOH Son Aq KOH Fitrate INVENTORS: ARNO H. REDIES MLTON B. CARUS >27--ee,BY 9-1-1-1 4-e (2-4 ATT'YS 2,940,823 United States Patent Office Patiented June 14, 1960 1. 2 mercial scale. This is very likely due to the fact that during the process, the mixture gets very thick or viscous, so that it is extremely difficult to disperse the oxygen suf 2,940,823 ficiently for the reaction and a very large provision of PRODUCTION OF POTASSUMMANGANATES 5 power is required in order to agitate the reaction mass at Arno H. Reidies and Milton B. Carus, La Salle, Ill., as all. This thickening occurs within a period of several signors to Carus Chemical Company, La Sale, Ill., a hours, even with a much reduced quantity of manganese corporation of Illinois dioxide in the melt. We have now provided a process which overcomes Filed Oct. 10, 1956, Ser. No. 615,033 O the foregoing difficulty of the prior melt oxidation proc ess, and in doing so, have discovered the reasons for the 14 Claims. (C. 23-58) difficulty and have provided a solution to the problems. We have found that, apparently, the principal source of trouble is that the manganese dioxide swells up to The invention relates to the production of potassium 5 many times its original volume after a short period of manganates by oxidation of manganese compounds in an time. Even a small excess of manganese dioxide will aqueous potassium hydroxide melt. More particularly, swell up to convert the already somewhat viscous liquid the invention relates to the production of potassium into a thick paste. manganate (V) KMnO, and to the production of po We have discovered that the key to the solution of the tassium manganate (VI) K2MnO, by oxidation com 20 problem is to add a manganese oxide to an aqueous mencing with an oxidic manganese compound. The in potassium hydroxide melt at a rate of addition which is vention provides a process which renders production in not substantially greater than its rate of oxidation to a such manner commercially practicable. valence above 4. In the new process, an oxidic man Prior to the invention, potassium manganate KMnO, ganese compound having a manganese valence of less has been produced for many years, and several methods 25 than 5 is oxidized to KMnO, wherein manganese has of production have been devised. A large part of the a valence of 5, the oxidic manganese compound being potassium manganate produced is subsequently converted added at a rate not substantially greater than its rate of to potassium permanganate. Fundamentally, the reac oxidation to KMnO4. tions involved in the prior production of potassium man We have further discovered that oxidation of an oxidic ganate and potassium permanganate are represented by 30 manganese compound having a manganese valence of the following equations: less than 5, to KMnO4 is very desirably effected by reaction with a potassium manganate having a manganese (1) MnO2--2KO-2O-KMnO-H2O valence of greater than 5, i.e., potassium manganate (VI) (2) electr. or potassium permanganate. The latter decomposes to KMnO-H-I-O-KMnO-KO-36H 35 potassium manganate (VI) very quickly under the re The present invention is concerned with the production action conditions, according to the equation of K2MnO, according to different equations, which also involve the production of KMnO. The latter com pound may be recovered for use as such or for produc In this manner, the oxidation of the manganese oxide is tion of KMnO4 therefrom. 40 not dependent upon oxidation with a gas, such as air, Of the several methods proposed for manufacturing and a favorable relatively low temperature may be em K2MnO4, the primary commercial method apparently is ployed for optimum results. the roasting method. This involves mixing hot concen The KaMnO4 produced is further oxidized to KMnO. trated potassium hydroxide and manganese dioxide, cool The further oxidation may take place in the same re ing and grinding the mixture. The concentrated potas s action zone or vessel, concomitantly with or subsequent sium hydroxide starting material is produced by evaporat to the oxidation of the manganese compound having a ing water from aqueous potassium hydroxide up to 385 valence below 5. Preferably, the oxidation of KMnO, C. Alternatively, a slurry of 50% KOH and manganese to K2MnO4 is carried out in a separate reaction zone or dioxide is sprayed into a hot oven, and the product is vessel, after removing the KMnO, from the first reaction cooled and ground. The ground product is then roasted SO Zone, preferably at a rate comparable to its production. at about 225 C. with air, while intermittently spray In prior chemical studies, KaMnO4 had been produced ing water on the mixture. The roasting is carried out by the following reaction carried out with powdered ma in large rotary drums or tubes. This operation requires terials in the dry state at about 800° C. a very large amount of equipment, with accompanying dry high capital investment, power, heat, labor and main SS (3) 2MnO2-6R. OH+40- a 2K Mino-3H,o tenance requirements. Furthermore, the process is slow, inconsistent and difficult to supervise. The reaction can The compound had also been produced by a high tem not be carried to completion. This is apparently because perature decomposition of K2MnO, as follows: of the difficulty in supplying sufficient water to the re actants and because sufficient potassium hydroxide can 60 not be supplied. As regards the former condition, the Both of these methods are technically impractical and presence of water is necessary for the reaction although result in an anhydrous product. it does not appear on the left of the equation. The The present invention is based upon the following re potassium hydroxide quantity is limited, because over a actions: certain ratio to manganese dioxide, the product ag 65 (5) KO-HO son glomerates seriously and prevents further oxidation. MnO--4KOH--KMnO------>2KsMnO2HO A number of years ago, a process was devised wherein 170-81.0° C. (6) KOB-IO son manganese dioxide was oxidized to KMnO, with air in 2Ks MnO4-3-3O2--HO- -->2KMnO-2KOH a concentrated aqueous potassium hydroxide melt. De 70 40-310° C. spite the potential attractiveness of such a process, it has So far as known, this represents the first time a process apparently never been successfully employed on a com has been based upon Equation 5, which is especially sig 2,940,823 - 4. nificant as employed in the production of KMnO4. The droxide melt at a temperature of about 170 C. to 310 C., equation represents reaction in an aqueous melt at a preferably about 220° C. to 260° C. The reaction rate relatively low temperature, which provides a practical is greater at the higher temperatures, while corrosion is commercial process producing an aqueous product which reduced at the lower temperatures. Further increase in is readily further processed, and the operating conditions, 5 temperature is preferably avoided, to avoid possible de such as temperature, pressure and concentration are com composition of K2MnO4. The potassium hydroxide con mercially attractive. Reaction 6 represents a very use : centration is preferably about 65% to 90%, by weight. ful and economic process of manufacturing K2MnO4; - However, the concentration and reaction temperature may starting with KMnO, advantageously the product of be varied. - Equation 5. O It is also preferred: that the melt contain an excess of Each reaction may be carried out at a favorable rela potassium hydroxide over the 'theoretical molar ratio to tively low temperature, which is especially advantageous manganese dioxide of 4:1. A considerable molar excess in materially reducing corrosion. Also, the solids and of potassium hydroxide, is-preferably employed, on the solutions are handled and processed with less difficulty, order of 30 to 60:1 or greater, which provides a melt and construction, maintenance and operation of the ves 15 of suitable viscosity. In this connection, it will be ap sels, filters, pumps and other equipment are facilitated. parent that Equation 5 will be appropriately varied when Reaction 6 may take place in the same reaction zone the manganese oxide is other than manganese dioxide, and with Reaction 5, furnishing an adequate supply of oxygen ... the potassium hydroxide and potassium manganate re for that purpose and removing the KMnO, which crys quirements will be adjusted accordingly. - tallizes, as it is produced. Reaction 6 may take place 20 The reaction proceeds with vigorous agitation while pro while Reaction 5 occurs with the continued addition of viding a potassium manganate having a manganese valence the manganese oxide. Alternatively, Reaction 5 may be of greater than 5 in the melt. A quantity of the manganate completed without substantial production of KMnO ac is added initially, and further manganate is added con cording to Reaction-6, and thereafter, the KaMnO may tinuously or intermittently as the reaction proceeds. The 25 potassium manganate is very advantageously supplied by t be oxidized to KMnO, according to Reaction 6. cycling part of the KMnO, produced by oxidation of i A It is preferred in the invention to withdraw the KMnO, KMnO. While a slight excess of the manganese oxide produced in Reaction 5. at a rate comparable to or ap maybe tolerated, it is preferred to continually maintain proximately the same as its rate of production, and oxidize the average manganese valence in the melt at a value of it in a separate second zone according to reaction 6.
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