Chemistry of inorganic compounds – Sulfur or compound thereof
Patent
1990-10-25
1994-04-05
Straub, Gary P.
Chemistry of inorganic compounds
Sulfur or compound thereof
423 53, 423 56, 423DIG14, 502220, C01G 3906
Patent
active
053002741
ABSTRACT:
A method for preparing molybdenum and sulfur containing compounds of the general formula X.sub.2 Mo.sub.2 S.sub.12.yH.sub.2 O, where X is a cation selected from the group consisting of Na.sup.+, K.sup.+, R.sub.4 N.sup.+, R.sub.3 NH.sup.+, R.sub.2 NH.sub.2.sup.+, RNH.sub.3.sup.+, NH.sub.4.sup.+, R.sub.4 P.sup.+, R.sub.4 As.sup.+,(R.sub.3 P).sub.2 N.sup.+, R is a C.sub.1 -C.sub.30 alkyl, C.sub.6 -C.sub.30 aryl, C.sub.7 -C.sub.30 aralkyl or C.sub.2 -C.sub.30 alkoxyalkyl group and mixtures thereof, and y is from 0 to 2. The method comprises preparing a sulfide solution that contains from about 9 wt. % to about 13 wt. % sulfide sulfur; contacting the solution with elemental sulfur and a hydroxide; adding a molybdenum compound for a time and at a temperature sufficient to form a reaction mixture and a precipitate; separating the precipitate; and contacting the remaining reaction mixture with additional sulfide solution to form (NH.sub.4 ).sub.2 Mo.sub.2 S.sub.12.yH.sub.2 O. When compounds containing cations other than NH.sub.4.sup.+ are to be produced, the (NH.sub.4).sub.2 Mo.sub.2 S.sub.12.yH.sub.2 O is contacted with a cation exchange compound containing a desired substitute cation selected from above and an anion selected from the group consisting of Cl.sup.-, Br.sup.-, F.sup.-, I.sup.-, BF.sub.4.sup.-, PF.sub.6.sup.-, OH.sup.-, BR.sub.4.sup.- where R is a C.sub.1 -C.sub.30 alkyl, C.sub.6 -C.sub.30 aryl, C.sub.7 -C.sub.30 aralkyl or C.sub.2 -C.sub.30 alkoxyalkyl group, and mixtures thereof, in the presence of a solvent and for a time and at a temperature sufficient to form X.sub.2 Mo.sub.2 S.sub.12.yH.sub.2 O, where X is other than NH.sub.4.sup.+.
REFERENCES:
patent: 3860419 (1975-01-01), Weber
patent: 3965041 (1976-06-01), van Klinken
patent: 4430442 (1984-02-01), Sawyer
"Synthesis, Interconversions, & Structural Characterization of the [(S.sub.4)2MOS].sup.2-, [(Mo.sub.2 S.sub.10).sup.2- ] and [(Mo.sub.2 S.sub.12).sup.2- ] Anions" M. Graganjac et al. Inorg. Chem. 1982, 21, 3321-3332.
"(NH.sub.4).sub.2 [(S.sub.2).sub.2 Mo(S.sub.2).sub.2 Mo(S.sub.2).sub.2 ].2H.sub.2 O, A Novel Sulfur-Rich Coordination Compound With Two Nonequivalent Complex Anions Having the Same Point Group but Different Structures: Crystal & Molecular Structures" A. Muller et al. Inorg. Chem., 1980, 19, 2835-2836.
"[(S.sub.2).sub.2 Mo(S.sub.2).sub.2 Mo(S.sub.2).sub.2 ].sup.2-, A Novel Complex Containing Only S.sub.22- Ligand and a Mo-Mo Bond" A. Muller et al. Angew. Chem. Int. Engl. vol. 17, p. 279 (1978).
Coyle Catherine L.
Halbert Thomas R.
Stiefel Edward I.
Wei Liwen
Dvorak Joseph J.
Exxon Research and Engineering Company
Straub Gary P.
Vanoy Timothy C.
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