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US 6,872,375 B2Granted
Synthesis of hexammine cobaltic salts
AssigneeAutoliv ASP, Inc.
InventorsDouglas R. Tingey, Robert G. Smith
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Abstract
The invention provides an effective and efficient method of making a hexammine cobaltic salt, such as hexammine cobaltic nitrate, in a consistent fashion through the control of one or more selected parameters of manufacture. Specific parameters considered and evaluated as a part of the invention included: order of addition of reactants, reaction temperature, oxidation, air or oxidant flow, catalyst content, and amount of ammonia.
Claims32
A method of making a hexammine cobaltic salt, the method comprising:
- (a) providing a reaction vessel containing an aqueous solution of at least one ammonia source selected from the group consisting of ammonium hydroxide, ammonia-containing gas and combinations thereof;
- (b) introducing a solution of Co(X)2 and a solution of NH4X, wherein X is at least one selected from the group consisting of chloride, bromide, perchlorate, and nitrate, into the reaction vessel whereby the introduced cobalt encounters an excess amount of ammonia preventing cobalt complex formation and to form reaction vessel contents comprising a first product precursor;
- (c) introducing an oxygen-containing gaseous oxidizer to the reaction vessel contents of (b) to form an at least partially oxidized second product precursor;
- (d) heating the at least partially oxidized second product precursor to form a third product precursor;
- (e) adding a surface active catalyst to the third product precursor;
- (f) continue introducing an oxygen-containing gaseous oxidizer to the catalyst-containing reaction mixture of (e) while maintaining the temperature at a temperature selected to result in product formation of a desired particle size;
- and
- (g) cooling the mixture from (f) and recovering the hexammine cobaltic salt therefrom as an admixture with the surface active catalyst.
5 more elements
A method of making a hexammine cobaltic nitrate having a particle size in the range of about 35 microns to about 60 microns, the method comprising:
- (a) providing a reaction vessel containing an aqueous solution of at least one ammonia source selected from the group consisting of ammonium hydroxide, an ammonia-containing gas and combinations thereof;
- (b) introducing a solution of Co(NO3)2 and NH4NO3 into the reaction vessel to form reaction vessel contents comprising a first product precursor comprising Co(NH3)5(H2O)(NO3)2;
- (c) heating the first product precursor to a temperature in the range of 95° F. to 120° F.;
- (d) introducing an oxygen-containing gaseous oxidizer to the heated first product precursor in (c) to form an at least partially oxidized reaction mixture having an absorbance @ 505 nm of at least about 1.5 AU;
- (e) adding a surface active catalyst of activated carbon to the reaction mixture of (d);
- (f) continue introducing an oxygen-containing gaseous oxidizer to the catalyst-containing reaction mixture of (e) while maintaining the temperature within a range of about 95° F. to about 120° F. and which temperature is selected to result in to result in the hexammine cobaltic nitrate having a desired particle size;
- and
- (g) cooling the mixture from (f) and recovering the hexammine cobaltic nitrate therefrom as an admixture with the surface active catalyst.
5 more elements
A method of making a hexammine cobaltic nitrate having a selected particle size, the method comprising:
- (a) providing a reaction vessel containing an aqueous solution of at least one ammonia source selected from the group consisting of ammonium hydroxide, ammonia-containing gas and combinations thereof;
- (b) introducing a solution of Co(NO3)2 and NH4NO3 into the reaction vessel to form reaction vessel contents comprising Co(NH3)5(H2O)(NO3)2;
- (c) introducing an oxygen-containing gaseous oxidizer to the reaction vessel contents of (b) to form μ-peroxobis;
- (d) heating the μ-peroxobis to form pentammine-aqua cobaltic nitrate;
- (e) adding a surface active catalyst of activated carbon to the pentammine-aqua cobaltic nitrate;
- (f) continue introducing an oxygen-containing gaseous oxidizer to the catalyst-containing reaction mixture of (e) while maintaining the temperature at a selected temperature in the range of about 95° F. to about 120° F. to result in the hexammine cobaltic nitrate having a selected particle size in the range of about 35 microns to about 60 microns;
- and
- (g) cooling the mixture from (f) and recovering the hexammine cobaltic nitrate therefrom as an admixture with the surface active catalyst.
5 more elements
A method of making a hexammine cobaltic salt, the method consisting essentially of:
- (a) providing a reaction vessel containing an aqueous solution of at least one ammonia source selected from the group consisting of ammonium hydroxide, ammonia-containing gas and combinations thereof;
- (b) introducing a solution of Co(X)2 and a solution of NH4X, wherein X is at least one selected from the group consisting of chloride, bromide, perchlorate, and nitrate, into the reaction vessel to form reaction vessel contents comprising a first product precursor;
- (c) introducing an oxygen-containing gaseous oxidizer to the reaction vessel contents of (b) to form an at least partially oxidized second product precursor;
- (d) heating the at least partially oxidized second product precursor to form a third product precursor;
- (e) adding a surface active catalyst to the third product precursor;
- (f) continue introducing an oxygen-containing gaseous oxidizer to the catalyst-containing reaction mixture of (e) while maintaining the temperature at a temperature selected to result in product formation of a desired particle size;
- and
- (g) cooling the mixture from (t) and recovering the hexammine cobaltic salt therefrom as an admixture with the surface active catalyst.
5 more elements
Dependencies are inferred from the claim text.