Method for making molybdenum and sulfur containing compounds

Claim 1

A method for preparing molybdenum and sulfur containing compounds of the general formula X 2 Mo 2 S 12 .yh 2 O, where X is a cation selected from the group consisting of Na+, K+, R 4 N+, R 3 NH+, R 2 NH 2 +, RNH 3 +, NH 4 +, R 4 P+, R 4 As+, (R 3 P) 2 N+, R is a C 1 -C 30 alkyl, C 6 -C 30 aryl, C 7 -C 30 aralkyl or C 2 -C 30 alkoxyalkyl group, and mixtures thereof, and y is from 0 to 2, comprising: (a) preparing an ammonium sulfide solution containing from about 9 wt. % to about 13 wt. % sulfur; (b) contacting the sulfide solution of step (a) with an appropriate amount of elemental sulfur and a hydroxide to form a polysulfide solution; (c) adding a molybdenum compound selected from the group consisting of molybdic acid, a molybdate and molybdenum trioxide to the polysulfide solution for a time and a temperature sufficient to form a precipitate in the solution; (d) separating the precipitate from the solution to obtain a precipitate-free solution; (e) contacting the precipitate-free solution with additional ammonium sulfide solution, containing from about 9 wt. % to about 13 wt. % sulfide sulfur, in an amount and for a time and at a temperature sufficient to form (NH 4 ) 2 Mo 2 S 12 .yH 2 O; and, (f) when X is to be other than NH 4 +, the (NH 4 ) 2 Mo 2 S 12 .yH 2 O formed in step (e) is separated, dried and then contacted with a solution of cation exchange compound containing a cation selected from group consisting of Na+, K+, R 4 N+, R 3 NH+, R 2 NH 2 +, RNH 3 +, R 4 P+, R 4 As+, (R 3 P) 2 N+, where R is a C 1 -C 30 alkyl, C 6 -C 30 aryl, C 7 -C 30 aralkyl or C 2 -C 30 alkoxyalkyl group, and mixtures thereof, and an anion selected from the group consisting of Cl-, Br-, F-, I-, BF 4 -, PF 6 -, OH-, Br 4 -, where R is a C 1 -C 30 alkyl, C 6 -C 30 aryl, C 7 -C 30 aralkyl; C 2 -C 30 alkoxyalkyl group, and mixtures thereof, and for a time sufficient to form a precipitate of the general formula X 2 Mo 2 S 12 .YH 2 O, where X is not NH 4 +.

Claim 2

A method for preparing molybdenum and sulfur containing compounds of the general formula X 2 Mo 2 S 12 .yh 2 O, where X is a cation selected from the group consisting of Na+, K+, R 4 N+, R 3 NH+, R 2 NH 2 +, RNH 3 +, NH 4 +, R 4 P+, R 4 As+, (R 3 P) 2 N+, R is a C 1 -C 30 alkyl, C 6 -C 30 aryl, C 7 -C 30 aralkyl or C 2 -C 30 alkoxyalkyl group, and mixtures thereof, and y is from 0 to 2, comprising: (a) preparing an ammonium sulfide solution containing from about 9 wt. % to about 13 wt. % sulfur; (b) contacting the sulfide solution of step (a) with an appropriate amount of elemental sulfur and a hydroxide to form a polysulfide solution; (c) adding a molybdenum compound selected from the group consisting of molybdic acid, a molybdate and molybdenum trioxide to the polysulfide solution for a time and a temperature sufficient to form a precipitate in the solution; (d) separating the precipitate from the solution to obtain a precipitate-free solution; (e) contacting the precipitate-free solution with additional ammonium sulfide solution, containing from about 9 wt. % to about 13 wt. % sulfide sulfur, in an amount and for a time and at a temperature sufficient to form (NH 4 ) 2 Mo 2 S 12 .yH 2 O; and, (f) when X is to be other than NH 4 +, the (NH 4 ) 2 Mo 2 S 12 .yH 2 O formed in step (e) is separated, dried and then contacted with a solution of cation exchange compound containing a cation selected from group consisting of Na+, K+, R 4 N+, R 3 NH+, R 2 NH 2 +, RNH 3 +, R 4 P+, R 4 As+, (R 3 P) 2 N+, where R is a C 1 -C 30 alkyl, C 6 -C 30 aryl, C 7 -C 30 aralkyl or C 2 -C 30 alkoxyalkyl group, and mixtures thereof, and an anion selected from the group consisting of Cl-, Br-, F-, I-, BF 4 -, PF 6 -, OH-, Br 4 -, where R is a C 1 -C 30 alkyl, C 6 -C 30 aryl, C 7 -C 30 aralkyl; C 2 -C 30 alkoxyalkyl group, and mixtures thereof, and for a time sufficient to form a precipitate of the general formula X 2 Mo 2 S 12 .YH 2 O, where X is not NH 4 +.

Claim 10

A method for preparing (NH 4 ) 2 Mo 2 S 12 .yH 2 O where y is from 0 to 2, comprising: (a) preparing an ammonium sulfide solution, containing from about 9 wt. % to about 13 wt. % sulfide sulfur; (b) contacting the ammonium sulfide solution with elemental sulfur and ammonium hydroxide to form an ammonium polysulfide solution; (c) adding ammonia molybdate to the polysulfide solution and stirring the combination for about 1 hour to about 24 hours at room temperature (25° C.) and atmospheric pressure to form a precipitate in the solution; (d) separating the precipitate from the solution to obtain a precipitate free solution; (e) contacting the precipitate free solution with an ammonium sulfide solution, containing from about 9 wt. % to about 13 wt. % sulfide sulfur, in an amount and for a time sufficient to form (NH 4 ) 2 Mo 2 S 12 .yH 2 O.

Claim 11

A method for preparing (NH 4 ) 2 Mo 2 S 12 .yH 2 O where y is from 0 to 2, comprising: (a) preparing an ammonium sulfide solution, containing from about 9 wt. % to about 13 wt. % sulfide sulfur; (b) contacting the ammonium sulfide solution with elemental sulfur and ammonium hydroxide to form an ammonium polysulfide solution; (c) adding ammonia molybdate to the polysulfide solution and stirring the combination for about 1 hour to about 24 hours at room temperature (25° C.) and atmospheric pressure to form a precipitate in the solution; (d) separating the precipitate from the solution to obtain a precipitate free solution; (e) contacting the precipitate free solution with an ammonium sulfide solution, containing from about 9 wt. % to about 13 wt. % sulfide sulfur, in an amount and for a time sufficient to form (NH 4 ) 2 Mo 2 S 12 .yH 2 O.