Processes for preparing niobium alkoxides, and niobium alkoxides prepared thereby
View Patent ↗Processes for preparing high-purity niobium alkoxides, especially niobium ethoxide, are described which include: (a) providing a crude niobium alkoxide starting material comprising at least one compound of the general formula (I) Nb(OR) 5 (I) wherein each R independently represents a linear or branched C 1-12 alkyl group; and (b) contacting the crude niobium alkoxide starting material with a treatment medium comprising a component selected from the group consisting of (i) one or more alcohols of the general formula (II) in an amount of 0.01 to 5% by weight, (ii) air or an oxygen-containing gas, and (iii) combinations thereof; R 1 OH (II) wherein each R 1 independently represents a linear or branched C 1-12 alkyl group.
1. A process comprising: (a) providing a crude niobium alkoxide starting material comprising at least one compound of the general formula (I)
Nb(OR) 5 (I)
wherein each R independently represents a linear or branched C 1-12 alkyl group; and (b) contacting the crude niobium alkoxide starting material with a treatment medium comprising a component selected from the group consisting of (i) one or more alcohols of the general formula (II) in an amount of 0.01 to 5% by weight, (ii) air or an oxygen-containing gas, and (iii) combinations thereof;
R 1 OH (II)
wherein each R 1 independently represents a linear or branched C 1-12 alkyl group.
2. The process according to claim 1 , further comprising distilling the crude niobium alkoxide starting material subsequent to contacting with the treatment medium.
3. The process according to claim 1 , wherein each R independently represents a linear or branched C 1-6 alkyl group.
4. The process according to claim 1 , wherein each R represents an identical linear or branched C 1-6 alkyl group.
5. The process according to claim 1 , wherein each R represents an ethyl group.
6. The process according to claim 1 , wherein the treatment medium comprises an alcohol of the general formula (II) and wherein R 1 represents a linear or branched C 1-6 alkyl group.
7. The process according to claim 1 , wherein the treatment medium comprises an alcohol of the general formula (II) and wherein R 1 represents an ethyl group.
8. The process according to claim 5 , wherein the treatment medium comprises an alcohol of the general formula (II) and wherein R 1 represents an ethyl group.
9. The process according to claim 1 , wherein the treatment medium comprises dry air or a dry oxygen-containing gas.
10. The process according to claim 1 , wherein the crude niobium alkoxide starting material has a halogen content of less than 100 ppm by weight.
11. The process according to claim 1 , wherein providing the crude niobium alkoxide starting material comprises: (i) providing an initial niobium alkoxide material having a halogen content of greater than 100 ppm, wherein the halogen content comprises a mono- or polynuclear halogen-containing metal alkoxide; (ii) mixing the initial niobium alkoxide material with not more than 30% by weight, based on the total amount of the initial alkoxide material, of an alcohol R 2 OH where R 2 independently represents a linear or branched C 1-12 alkyl group; and (iii) subsequently or simultaneously, adding an excess of ammonia to the mixed initial material and alcohol, the excess based on the mono- or polynuclear halogen-containing metal alkoxide.
12. The process according to claim 8 , wherein providing the crude niobium alkoxide staffing material comprises: (i) providing an initial niobium alkoxide material having a halogen content of greater than 100 ppm, wherein the halogen content comprises a mono- or polynuclear halogen-containing metal alkoxide; (ii) mixing the initial niobium alkoxide material with not more than 30% by weight, based on the total amount of the initial alkoxide material, of an alcohol R 2 OH where R 2 independently represents a linear or branched C 1-12 alkyl group; and (iii) subsequently or simultaneously, adding an excess of ammonia to the mixed initial material and alcohol, the excess based on the mono- or polynuclear halogen-containing metal alkoxide.
13. The process according to claim 11 , wherein the alcohol R 2 OH is mixed with the initial niobium alkoxide material in an amount of 4 to 12% by weight.
14. The process according to claim 11 , wherein the initial niobium alkoxide material has a halogen content of greater than 200 ppm.
15. The process according to claim 1 , wherein the crude niobium alkoxide starting material is contacted with one or more alcohols of the general formula (II) in an amount of 0.01 to 5% by weight and air or an oxygen-containing gas.