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United States Patent Office Patented Aug 3,459,514 United States Patent Office Patented Aug. 5, 1969 2 quired is smaller than the requirements of the prior art. 3,459,514 It is still a further object of the present invention to pro METHOD FOR PREPARING ALKAL vide a process whereby the amount of by-product pro METAL BOROHYDRDES James D. Johnston and Albert P. Giraitis, Baton Rouge, duced is less than that produced by the prior art. Other La., assignors to Ethyl Corporation, New York, N.Y., a objects will become apparent from the ensuing descrip corporation of Virginia tion. No Drawing. Continuation-in-part of applications Ser. No. The above objects are accomplished by the provision 308,691, Sept. 13, 1963, and Ser. No. 322,054, Nov. 7, of a process for producing an alkali metal borohydride 1963. This application Oct. 1, 1964, Ser. No. 400,888 which comprises reacting together an alkali metal hy ret, C. C01b 6/14 O dride, desiccated borax, hydrogen, and silicon at a tem U.S. C. 23-362 6 Claims perature within the range of from about 200 C. to about 900° C. The alkali metal present during the course of the re ABSTRACT OF THE DISCLOSURE action is a member selected from Group I-A of the A method of preparing alkali metal borohydrides com Periodic Chart of the Elements, Fisher Scientific Com prising reacting an alkali metal or alkali metal hydride, pany, 1955. The alkali metals include lithium, sodium, desiccated borax, hydrogen, and silicon, in an inert hy potassium, rubidium, and cesium. Sodium is a preferred drocarbon at about 250° C. to 500 C. and 15 to 500 alkali metal from an economic standpoint and in view of p.S.1. the fact that sodium borohydride is a preferred product 20 of the instant invention. The reaction mixture can initially comprise an alkali The present invention relates to a new process for the metal either in the form of its hydride or its metallic production of alkali metal borohydrides. state. Thus, the reaction mixture can comprise initially This application is a continuation in part of our co an alkali metal in the form of: lithium, sodium, potas pending applications Ser. No. 308,691 (filed Sept. 13, 25 sium, rubidium, cesium, lithium hydride, sodium hydride, 1963) and Ser. No. 322,054 (filed Nov. 7, 1963), now potassium hydride, rubidium hydride, or cesium hydride, abandoned of the same title. or any mixture of such materials. Whether employing an A large number of publications have described the pro alkali metal hydride or an alkali metal as the source of duction of boranates or alkali metal borohydrides in the alakali metal, the reaction should be conducted in which the starting materials include boron halides, boron 30 the presence of free hydrogen for reasons as brought out halide complexes, organic boron compounds, or boric hereinafter. However, when employing an alkali metal acid. All of these materials are either expensive, danger hydride the reaction can be conducted utilizing less free ous to handle or result in low yields of the desired prod hydrogen since some of the necessary hydrogen values llct. can be supplied from the alkali metal hydride. The latter One typical method of producing alkali metal borohy approach which offers no technical advantage suffers an drides is set forth in U.S. Patent 2,461,661, issued on economic disadvantage inasmuch as excessive quantities Feb. 15, 1949 to Schlesinger et al. This method com of sodium hydride are required. It is preferred in the prises reacting an alkali metal alkoxyborohydride and process of this invention to employ the alkali metal and diborane in accordance with the following equation: hydrogen as separate and distinct reactants since high 40 yields of the alkali metal borohydride are obtained in wherein Me is an alkali metal and R is a hydrocarbon short reaction or cycle times. radical. The reaction materials required in this process A more preferred embodiment of the instant invention are extremely expensive which consitutes a definite dis is the process comprising reacting together an alkali advantage. metal, desiccated borax, hydrogen, and silicon at a tem 45 pearture within the range of from about 200° C. to about More recently, U.S. Patent 3,077,376, which issued on 900 C. An even more preferred embodiment is a process Feb. 12, 1963 to Schubert et al., describes a method of for producing sodium borohydride which comprises re preparing alkali metal borohydrides by reacting borax, acting together sodium, desiccated borax, hydrogen, and sodium and hydrogen in the presence of substances such silicon at a temperature within the range of from about as silica which react chemically with the metal oxide 50 200° C. to about 900 C. formed. The patentees state that in order to obtain op A more preferred temperature range, especially when timum results, the reactants, i.e., the borate minerals, utilizing sodium metal as a reactant, is within the range of alkali metal and hydrogen, are mixed in such proportion from about 350 C to about 600 C. that for each atom of boron present in the reaction mix The present process is preferably conducted at super ture, there are present at least four atoms of alkali metal 55 atmospheric pressure, even though atmospheric pressure and four atoms of hydrogen. Thus a typical equation ex or less can be employed, the pressure being influenced emplifying the process is as follows: mainly by the nature of the reactants as well as the type of reaction equipment employed. The partial pressure of This process, although to some extent economical, utilizes hydrogen can range from about 5 p.s.i. to about 3000 excessive quantities of sodium and silica in order to ob 60 p.s. i., preferably from about 15 p.s.i. to about 1000 p.s.i. tain sodium borohydrides, e.g., 16 moles of sodium in The total pressure in the system should normally be from order to obtain four moles of sodium borohydride prod 0 to about 500 p.s. i. higher than the hydrogen partial pres uct. Furthermore, large quantities of sodium silicate are sure, depending on the nature of the inert liquid medium produced as a by-product. and the concentration of inert gaseous diluents, such as It is therefore an object of the present invention to 65 nitrogen, neon, argon, krypton, and the like, which may provide a process for producing sodium borohydride be present. which is more economical than prior art processes. It is The borax starting material referred to hereinabove is another object of the present invention to employ cheap desiccated or dehydrated borax having the formula reactant materials which are readily available. It is a NaaB4O7. This material is obtained by heating the borax further object of the present invention to provide a proc 70 or tinkal, Na2B4H10H2O to a temperature sufficient to ess whereby the amount of the alkali metal reactant re drive the water from the naturally occurring mineral. In 3,459,514 3 4. some instances it may be more desirable to employ other metal (in the form of alkali metal or alkali metal hydride) borate minerals as the starting materials. In such cases per atom of boron is employed. It is preferred, however, borate minerals such as kernite, colemanite, boronatrocal that from about 1.5 atoms to about 3 atoms of alkali metal cite, ulexite, boracite, and mixtures thereof can be em per atom of boron be employed since yields are maximized ployed. However, it is much preferred to employ desic within this range. When employing a diluent it is preferred cated borax in the process of this invention since it is to use an excess of sodium above the stoichiometric pro readily available and hence offers a cost advantage. portions, generally from about 10 to about 60 percent in The element silicon in its pure form is preferably em excess, or from about 1.83 to about 2.66 atoms of sodium ployed as the co-reductant in the process of this invention. per atom of boron. However, if desired ferrosilicon can be employed in place 0 The amount of silicon employed can also vary over a of silicon. Ferrosilicon is readily available on the com wide range. Generally, from about 0.2 atom to about 1.5 mercial market at a rather economical price. atoms of silicon per atom of boron is employed in the A particularly preferred embodiment of this invention process of this invention. It is preferred, however, in order is to conduct the present process in a diluent which is inert to maximize yields, that an excess of silicon above the to the reactants and the reaction products. The diluent is 5 stoichiometric proportions be used, e.g. above about 0.6 beneficial inasmuch as it inhibits caking of the reaction atom of silicon per atom of boron to as much as 64 atoms mass as well as aids in the maintenance of constant tem of silicon per atom of boron (about 1000 percent excess). peratures. A diluent which is liquid at the temperature When employing a diluent, it is particularly preferred to and pressure employed is most preferred. Suitable diluents have an excess of from about 20 to about 80 percent or are aliphatic hydrocarbons, aromatic hydrocarbons, sili 20 from about 0.7 to about 1.05 atoms of silicon per atom cones, and the like. The aliphatic hydrocarbons are most of boron. preferred, especially mineral oils and oils having a similar The amount of hydrogen employed in this process will boiling point, viz. from about 300° C. to about 500 C.
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