Chemistry of inorganic compounds – Boron or compound thereof – Hydrogen and metal or ammonium containing
Patent
1985-09-30
1986-08-05
Doll, John
Chemistry of inorganic compounds
Boron or compound thereof
Hydrogen and metal or ammonium containing
C01B 3500
Patent
active
046042717
ABSTRACT:
A direct low temperature process for the preparation of pure magnesium borohydride diammoniate or the deuterated analog thereof based on the addition of 90-95% of the stoichiometric amount of NH.sub.3 to an excess of Mg(BH.sub.4).sub.2.X(C.sub.2 H.sub.5).sub.2 O in a benzene reaction solvent in accordance with equation 1: ##STR1## wherein X is a numeral from about 2.0 to about 2.5; or when the reaction is conducted in an ether reaction solvent with the same quantities of reactants and under the same experimental conditions, the triammoniate or the deuterated analog thereof is formed in accordance with equation 2: ##STR2## wherein X is a numeral from about 2.0 to about 2.5. In either case the pure product is readily isolated by filtration, solvent washing to remove excess Mg(BH.sub.4).sub.2.X(C.sub.2 H.sub.5).sub.2 O, and vacuum drying at ambient temperature. Yields are 95-99%; purities are typically about 97%.
REFERENCES:
patent: 2855348 (1958-10-01), Huff et al.
V. N. Konoplev and J. A. Silina, Zr. Neorg. Khim., 30(5), 1125-1128 (1985).
Earl L. Muettertres, Boron Hydride Chemistry, Academic Press, New York, 1, pp. 441 & 445.
V. N. Konoplev, "Synthesis of Magnesium Tetrahydridoborate", Russian J. Inorg. Chem., 25(7), 1980.
Grant Louis R.
Wagner Ross I.
Bush Freddie M.
Doll John
Gibson Robert P.
Lane Anthony T.
Leeds Jackson
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