Valve metal oxide powders and process for the production thereof
View Patent ↗A process for the production of a valve metal oxide powder, in particular an Nb 2 O 5 or Ta 2 O 5 powder by continuous reaction of a fluoride-containing valve metal compound with a base in the presence of water and calcination of the resultant product, wherein the reaction is performed in just one reaction vessel and at a temperature of at least 45° C. Valve metal oxide powders obtainable in said manner which exhibit a spherical morphology, a D 50 value of 10 to 80 μm and an elevated BET surface area.
1. A process for the production of a valve metal oxide powder which comprises continuous reacting a fluoride-containing valve metal compound with a base in the presence of water at a temperature of at least 450° C. and calcination of the resultant product, wherein the fluoride-containing valve metal compound is employed as an aqueous solution at a concentration of 0.3 mol/l to 1.2 mol/l, based on the amount of valve metal, wherein the base is an aqueous ammonia solution with a concentration of 3 weight percent to 15 weight percent and the reaction is carried out continuously, wherein the volumetric flow ratios are adjusted such that the ratio of the volumetric flow rate of an aqueous solution of the fluoride-containing valve metal compound to the volumetric flow rate of the aqueous solution of the base is from 1:0.9 to 1:2, and wherein the molar concentration ratio of fluoride-containing valve metal compound, calculated as valve metal, to base is adjusted to from 1:5.6 to 1:8.5 and the, reaction is performed in a single reaction vessel.
2. The process according to claim 1 , wherein the residence time in the reaction vessel is between 30 minutes and 3 hours.
3. The process according to claim 1 , wherein the fluoride-containing valve metal compound and the base used are in each case used in the form of an aqueous solution or suspension.
4. The process according to claim 1 , wherein the fluoride-containing valve metal compound is H 2 NbF 7 or H 2 TaF 7 .
5. The process according to claim 1 , wherein the reaction of the fluoride-containing valve metal compound with the base is performed at a pH value, measured at reaction temperature, of 7 to 14.