Alloys or metallic compositions – Containing over 50 per cent metal but no base metal
Reexamination Certificate
1996-08-05
2002-02-26
Andrews, Melvyn (Department: 1742)
Alloys or metallic compositions
Containing over 50 per cent metal but no base metal
C420S587000, C420S590000, C075S351000
Reexamination Certificate
active
06350408
ABSTRACT:
BACKGROUND OF THE INVENTION
(1) Field of the Invention
The present invention relates to a process and compositions including a finely divided metal, metal oxide coated metal, metal oxide and other oxidized metal produced by the use of alkalides and electrides to reduce a soluble metal salt in an organic solvent. In particular, the present invention relates to a process which produces the finely divided metal, metal oxide coated metal or metal oxide or other oxidized metal depending upon the oxidizability of a metal initially produced by the process.
(2) Prior Art
Homogeneous reduction of noble metal salts by mild reducing agents, even in aqueous solution is well known. Solid alkali metals and suspensions of alkali metals are also often used as reductants. The use of homogeneous strong reducing agents in aprotic solvents to produce finely divided metals has been limited to reduction by aromatic radical anions and/or aromatic dianions such as sodium naphthalenide (Rieke, R., Science 246, 1260-1264 (1989)). Often the reductions are slow and must be done at the reflux temperatures of THF. The most common source of solvated electrons is found in metal-ammonia and metal-amine solutions. Indeed, these solutions are commonly used in industry and research to reduce organic compounds (Birch reductions). The problem encountered with transition metal reductions by metal-ammonia solutions is the formation of metal amides and imides by deprotonation of the solvent. Complex mixtures result from such reactions and one seldom gets the transition metal itself.
Examples of metal particle production are:
1. Mild reduction of noble metals in the presence of soluble polymers to yield 10-50 Å particles. H. Hirai, Y. Nakao and N. Toshima,
J. Macromol. Sci-Chem.,
A12, 1117 (1978); A13, 727 (1979); H. Hirai, ibid, A13, 633 (1979).
2. Zero-valent compounds such as Fe(CO)
5
can be thermally decomposed in polymers to yield colloidal dispersions of metal. T. W. Smith and D. Wychick,
J. Phys. Chem.,
84, 1621 (1980).
3. Metal vapor deposition in a solvent matrix can give small metal particles, M. Kilner, N. Mason, D. B. Lambrick, P. D. Hooker and P. L. Timms,
J. Chem. Soc. Chem. Comm.,
356 (1987). K. Kimura and S. Bandow,
Bull. Chem. Soc. Jpn,
56, 3578 (1983); K. Kimura, ibid, 57, 1683 (1984); 60 3093 (1987).
4. Heterogeneous reduction by alkali metals in ethers with or without an aromatic compound present as an electron carrier has been used to prepare metals. R. D. Rieke et al.,
J. Am. Chem. Soc.,
96, 1775 (1974);
J. Org. Chem.,
40 2253 (1975); ibid 44, 3069 (1979); ibid, 46, 4323 (1981).
Research with alkalides and electrides as described in:
(1) U.S. Patent No. 4,107,180 to Dye;
(2) J. Am. Chem. Soc. 96, 608-609 (1974);
(3) J. Physical Chem. 79, 3065-3070 (1975);
(4) Angew. Chem. Int. Ed. Engl. 18, 587-598 (1979);
(5) Alkali Metals McGraw-Hill Yearbook of Science and Technology 87-89 (1981);
(6) Inorganic Chem., 21, 1966-1970 (1982);
(7) J. Am. Chem. Soc. 105, 6490-6491 (1983);
(8) Chemistry in Britain 20 210-215 (1984);
(9) Progress in Inorganic Chemistry, John Wiley & Sons 32, 327-441 (1984);
(10) J. Physical Chem. 88, 3852-3855 (1984);
(11) J. Am. Chem. Soc. 108, 3534-3535 (1986);
(12) J. Am. Chem. Soc. 109, 5561-5563 (1987);
(13) J. Am. Chem. Soc. 101, 7203-7204 (1987);
(14) Valency and-Charge Distribution, In Alkalide and Electride Salts, Proceedings of The Robert A. Welch Foundation Conference on Chemical Research XXXII Valency, pg 65-91 (1988);
(15) Nature 331, 599-601 (1988);
(16) J. Coord Chem. 18, 121-128 (1988);
(17) J. Am. Chem. Soc. 111, 935-938 (1989);
(18) J. Am. Chem. Soc. 111, 5957-5958 (1989);
(19) Pure & Appl. Chem. 61, 1555-1562 (1989); and
Ann. Rev. Phys. Chem. 38, 271-301 (1987); showed that relatively concentrated solutions (>0.1 M in many cases) are obtained which contain e
s
−
and/or M
−
in aprotic solvents such as dimethyl ether. This research provided the possibility to carry out reductions in the absence of proton sources other than the highly non-acidic —CH
2
— and —CH
3
protons of the solvent and complexant; however, the means for accomplishing such a reaction was not known.
Objects
It is therefore an object of the present invention to provide a process for the preparation of a metal, metal with an oxide coating, metal oxide or other oxidized metal depending upon the handling of the reaction product and the oxidizability of the metal. Further it is an object of the present invention to provide a process which allows the reaction to proceed with an alkalide or electride. These and other objects will become increasingly apparent by reference to the following description and the drawings.
REFERENCES:
patent: 3890455 (1975-06-01), Ballas et al.
patent: 3989674 (1976-11-01), Sinfelt et al.
patent: 4107180 (1978-08-01), Dye
patent: 4294608 (1981-10-01), Sedlak et al.
patent: 4363752 (1982-12-01), Goretta et al.
patent: 4678505 (1987-07-01), Bushey
patent: 4713110 (1987-12-01), Bogdanovic et al.
patent: 5091114 (1992-02-01), Nakajima et al.
patent: 5328501 (1994-07-01), McCormick et al.
Dye, J. L., et al., Faraday Discuss. 92, 45-55 (1991).
Rieke, R., Science 246, 1260-1264 (1989).
H. Hirai et al., J. Macromol. Sci-Chem., A12, 1117 (1978); A13, 727 (1979); H. Hirai.
T.W. Smith & D. Wychick, J. Phys. Chem., 84, 1621 (1980).
M. Kilner et al, J. Chem. Soc. Chem. Comm., 356 (1987).
K. Kimura & S. Bandow, Bull. Chem. Soc. Jpn, 56, 3578 (1983).
K. Kimura, 57, 1683 (1984); 60 3093 (1987) Bull Chem Soc Jpn.
R.D. Rieke et al., J. Am. Chem. Soc., 96, 1775 (1974).
J. Org. Chem., 40 2253 (1975).
J. Am. Chem. Soc. 96, 608-609 (1974). Hirai J Macromol SciChem A13 633 1979.
J. Physical Chem. 79, 3065-3070 (1975).
Angew. Chem. Int. Ed. Engl. 18, 587-598 (1979).
Alkali Metals McGraw-Hill Yearbook of Science & Tech. 87-89 (1981).
Inorganic Chem., 21, 1966-1970 (1982).
J. Am. Chem. Soc. 105, 6490-6491 (1983).
Chemistry in Britain 20, 210-215 (1984).
Progress in Inorganic Chemistry, John Wiley & Sons 32, 327-441 (1984).
J. Physical Chem. 88, 3852-3855 (1984).
J. Am. Chem. Soc. 108, 3534-3535 (1986).
J. Am. Chem. Soc. 109, 5561-5563 (1987).
J. Am. Chem. Soc. 101, 7203-7204 (1987).
Valency & Charge Dist., In Alkalide & Electride Salts, Proc. Robt. Welch Found. Conf. on Chem. Res. XXXII Valency, p. 65-91 (1988).
Nature 331, 599-601 (1988).
J. Coord. Chem. 18, 121-128 (1988).
J Org Chem 46 4323 (1981).
J. Am. Chem. Soc. 111, 935-938 (1989).
J Org Chem 44 3069 (1979).
J. Am. Chem. Soc. 111, 5957-5958 (1989).
Pure & Appl. Chem. 61, 1555-1562 (1989).
Ann. Rev. Phys. Chem. 38, 271-301 (1987).
Dye James L.
Ellaboudy Ahmed S.
Tsai Kuo-Lih
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