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United States Patent (19) 11) Patent Number: 4,545,974 Thompson (45) Date of Patent: Oct

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United States Patent (19) 11) Patent Number: 4,545,974 Thompson (45) Date of Patent: Oct United States Patent (19) 11) Patent Number: 4,545,974 Thompson (45) Date of Patent: Oct. 8, 1985 (54) PROCESS FOR PRODUCING ALKALI METAL FERRATES UTILIZING HEMATITE OTHER PUBLICATIONS AND MAGNETTE Bailar et al., "Comprehensive Inorganic Chemistry', Pergamon Press, N.Y., vol. 3, 1973. 76 Inventor: John A. Thompson, Nassau, The Primary Examiner-H. T. Carter Bahamas Attorney, Agent, or Firm-Kenyon & Kenyon 57 ABSTRACT (21) Appl. No.: 590,567 Alkali metal iron (IV) and iron (VI) ferrates are pro duced by forming a particulate mixture of reactants (22 Filed: Mar. 16, 1984 including an alkali metal nitrogen oxygen compound and an iron material selected from the group of iron oxide, Fe2O3, Fe3O4 and an iron compound which self (51) Int. Cl." .............................................. C01G 49/00 reacts at a temperature less than about 1100° C. to form 52 U.S. Cl. .................................................... 423/594 Fe2O3. The mixture of reactants is subjected to a prede 58) Field of Search ......................................... 423/594 termined elevated temperature for a predetermined time duration sufficient to bring about a reaction be (56) References Cited tween the reactants which produces at least one of iron (IV) and iron (VI) ferrates. The molar ratio of alkali U.S. PATENT DOCUMENTS metal nitrogen oxygen compound to the iron material is 2,835,553 5/1958 Harrison et al. .................... 423/594 preferably in the range extending between about 4:1 and about 8:1. FOREIGN PATENT DOCUMENTS 1013272 1/1958 Fed. Rep. of Germany ...... 423/594 23 Claims, No Drawings 4,545,974 1. 2 duced in these methods are in solution and require a PROCESS FOR PRODUCING ALKAL METAL crystallization therefrom in order to avoid the obvious FERRATES UTILIZING HEMATITE AND handling, shipping and storage disadvantages associated MAGNETITE with aqueous solutions. BACKGROUND OF THE INVENTION SUMMARY OF THE INVENTION (a) Field of the Invention It is an object of the present invention to provide a The present invention relates to alkali metal ferrates method for the direct preparation of iron (IV) and iron and, in particular, to methods for the preparation of (VI) alkali metal ferrates from readily available starting alkali metal ferrates where the iron therein has a valance 0 materials. of -- 4 or -6. A further object of this invention is to provide a Although the most common and familiar forms of simple method for the preparation of alkali metal iron iron in combination with other elements are those (IV) and iron (VI) ferrates. wherein iron has a valence or oxidation state of +2 or A further object of this invention is to provide a +3, other compounds of iron such as iron (IV) and iron 15 method for the preparation of alkali metal iron (IV) and (VI) are known in the art. Two of the more useful iron iron (VI) ferrates wherein the ferrate is produced in a (IV) and iron (VI) compounds are the ferrates, i.e., salts non-aqueous state. of iron (IV) and iron (VI). Iron (IV) ferrates (sometimes referred to as “perferrites”) (Fe032-) and iron (VI) DETAILED DESCRIPTION OF THE ferrate (Fe042) are generally useful in a variety of INVENTION chemical reactions as oxidizing agents. Iron (VI) fer In accordance with the invention, alkali metal fer rates, in particular are very strong oxidizing agents in rates are formed by reacting: aqueous solution, and stable, water soluble ferrates such (a) either alkali metal nitrate or alkali metal nitrite as potassium or sodium ferrate are, therefore, particu with larly useful in removing electrons (i.e., oxidizing) from 25 (b) either an ore known as hematite (primarily com other chemical species. A limiting factor in the broader prised of Fe2O3), an ore known as magnetite (primarily utilization of iron (IV) and iron (VI) ferrates is the un comprised of Fe3O4), or an iron compound which self availability of an inexpensive and simple means for the reacts via thermal decomposition to form Fe2O3. Synthesis of the pure forms of these compounds in rela The significance of these reactions of the invention tively high yield. 30 primarily resides in their ability to produce iron (IV) or (b) Description of the Prior Art iron (VI) in high yield amounts, and from inexpensive, A typical method utilized for the production of alkali readily-available starting materials (e.g., iron oxides, metal ferrates comprises electrochemical techniques hematite, magnetite, iron compounds which form he wherein a 35-40% NaOH solution is used to convert matite, and potassium nitrate and nitrite) without the scrap iron to a concentrated solution of Na2Fe04 (iron 35 need for complicated electrochemical procedures, ini (VI)) using 10-15 cm2 electrodes with a 2 cm separation tial preparation of reactants and the like. and an initial resistance of 2-5 ohms. Another method A further significance of these reaction schemes of comprises the wet chemical oxidation of a soluble iron the invention resides in their ability to form iron (VI) (III) compound by hypochlorite, followed by chemical alkali metal ferrate directly and not in solution. precipitation of Fe042 with potassium hydroxide to 40 Prior methods used in the thermal fusion synthesis of form K2Fe04, and followed by recrystallization to ob iron(IV) ferrate involve the initial formation of alkali tain a high purity solid. Still another method comprises metal ferrite (MFeC2 or M2Fe2O4) which is the fusion the fusion of iron filings with potassium nitrate and product of Fe2O3 and a suitable alkali metal base, e.g. extracting with water. MOH or M2CO3. The alkali metal ferrite is then fused U.S. Pat. No. 2,835,553 of Harrison, et al. discloses a 45 with alkali metal oxide or peroxide to form iron(IV) multi-step process for preparing alkali metal ferrates ferrate. Other thermal fusion methods used in the syn wherein an alkali metal iron (III) ferrate (typically thesis of iron(IV) ferrate involve the thermal fusion of known as a "ferrite") is reacted at elevated temperature alkali peroxide and alkali oxides with iron oxides to in the presence of free gaseous oxygen, with an alkali form a product which is entirely iron(IV) metal ferrate. metal compound (which may be the same or different 50 The formation of iron (VI) alkali metal ferrate has than the alkali metal present in the alkali metal (III) been achieved by such reactions only as a result of the ferrate) to produce the ferrate (IV) of the alkali metal or ability of iron (IV) itself to form iron (VI) when dis metals. The alkali metal ferrate (III) itself requires syn solved in water by the following reaction; thesis from more readily available materials, e.g., iron oxide. The ferrate (IV) produced in this manner may 55 then be dissolved in water to produce ferrate (VI) ac cording to the following equation (where, e.g., the al The significance of the present reactions of the inven kali metal is sodium): tion therefore resides in the direct formation of iron (VI) ferrate without the need for procedures which 60 involve indirect production of the ferrate in solution. Preferred alkali metal compounds for use in the reac tions of the invention are those of potassium, although In the foregoing processes, electrical energy is con sodium compounds may also be used to advantage. sumed and therefore expensive procedures are em In accordance with the method of this invention, ployed (e.g., electrolysis) or complicated multi-step 65 reactions are carried out between alkali nitrates (or procedures are required to produce iron (IV) or iron nitrites) and hematite or an iron compound which ther (VI) ferrates from more readily available materials. mally decomposes to form hematite (Fe2O3), with the Moreover, in most cases, the iron (VI) ferrates pro reactants being heated to produce the desired reaction. 4,545,974 3 4 Initially the solid reagents are preferably comminuted Where an iron compound which thermally decom and formed into a mixture in proportions suitable for the poses to form hematite is used in the reaction, the molar desired reaction. The molar ratio of hematite to the ratio of iron compound to the alkali nitrate (or nitrite), alkali nitrate of the mixture is in the range extending based upon the ratio of atomic iron to nitrate (or nitrite), between about 1:2.3 and about 1:8.5, and preferably is generally is between about 1:2 and about 1:4, and prefer from about 1:4 to about 1:5. ably is from about 1:2.5 to about 1:3. Where magnetite (Fe3O4) is chosen as the iron oxide, The reaction of the reagents in carrying out the the molar ratio is preferably in the range extending method of the invention may be conducted at a substan between about 1:7 to about 1:8. tially constant temperature or, alternatively, may be Ores comprising hematite and magnetite can contain 10 conducted in a stepwise manner with gradual increases small amounts of silicon dioxide (SiO2) as well as trace in temperature until the reaction is completed. amounts of first transition metal oxides which do not The product of the reactions involving alkali nitrite is adversely affect the reaction. a black solid mass and comprises alkali metal iron (IV) Where an iron compound which thermally decom and iron (VI) ferrates, with the exact presence of the poses upon heating to form hematite is used in the reac 15 iron (VI) ferrate being unknown when the yield of the tion, the respective molar ratio of iron compound to reaction is less than about 42%. alkali nitrate, based upon the ratio of atomic iron con The reaction product remitting from the method of tent to nitrate, is preferably in the range extending from the invention when alkali nitrate or alkali nitrite is em about 1:4 to about 1:5.
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