Claims
- 1. A method of preparing a storage stable solution of a catalytically active complex of molybdenum with a primary straight chain or branched chain alkanol containing 6 to 13 carbon atoms in said alkanol which comprises:
- reacting an ammonium molybdate with said alkanol in the presence of water, within the range of about 7 to about 20 mols of alkanol per gram atom of molybdenum sufficient to form a storage stable molybdenum/alkanol complex, said reaction being initiated in the presence of about 1 to about 4 mols of water per gram atom of molybdenum, said reaction being continued at atmospheric pressure at a temperature of about 120.degree. to about 190.degree. C. for a period of time with the range of about 3 to about 8 hours sufficient to substantially completely remove ammonia and water and to provide a liquid reaction product having said molybdenum/alkanol complex dissolved in unreacted alkanol and about 0.001 to about 0.1 wt. % of water,
- and recovering a clarified, storage stable solution of said catalytically active molybdenum/alkanol complex in said alkanol, and containing from about 4 to about 10.5 wt. % of dissolved molybdenum.
- 2. A method as in claim 1 wherein the mole ratio of alkanol to gram atoms of molybdenum is within the range of about 8.5 to about 15 and the reaction temperature is within the range of about 150.degree. to about 185.degree. C.
- 3. A method as in claim 2 wherein the alkanol is a hexyl alcohol.
- 4. A method as in claim 2 wherein the alkanol is iosoctyl alcohol.
- 5. A method as in claim 2 wherein the alkanol is decyl alcohol.
- 6. A method as in claim 2 wherein the alkanol is tridecyl alcohol.
- 7. A method of preparing a storage stable solution of a catalytically active complex of molybdenum with 2-ethyl hexanol in 2-ethyl hexanol which comprises:
- reacting ammonium heptamolybdate tetrahyderate with 2-ethyl hexanol in amount within the range of from about 7 to about 20 mols of said 2-ethyl hexanol per gram atom of molybdenum; said reaction being initiated in the presence of about 1 to about 4 mols of water per gram atom of molybdenum said reaction being continued at atmospheric pressure at a temperature of about 120.degree. to about 190.degree. C. for a period of time within the range of about 3 to about 8 hours sufficient to substantially completely remove ammonia and water and to provide a liquid reaction product comprising said molybdenum/2-ethylhexanol complex dissolved in 2-ethyl hexanol and containing about 0.001 to about 0.1 wt. % of water, and
- recovering a clarified, storage stable solution of said catalytically active molybdenum/2-ethyl hexanol complex in 2-ethyl hexanol, and containing about 4 to about 10.5 wt. % of dissolved molybdenum.
- 8. A method as in claim 7 wherein the 2-ethyl-1-hexanol is present in an amount sufficient to provide a mole ratio of about 8.5 to about 15 moles of 2-ethyl-1-hexanol per gram atom of molybdenum.
- 9. A method as in claim 8 wherein the temperature is within the range of about 150.degree. to about 185.degree. C.
- 10. A method as in claim 8 wherein the temperature is within the range of about 175.degree. to about 185.degree. C.
CROSS-REFERENCE TO RELATED APPLICATION
This application is a continuation-in-part of copending application Ser. No. 06/687,710 filed Dec. 31, 1984 and entitled "Improved Synthesis of Molybdenum/Alcohol Complexes Useful as Epoxidation Catalysts" now abandoned.
US Referenced Citations (10)
Continuation in Parts (1)
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Number |
Date |
Country |
Parent |
687710 |
Dec 1984 |
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