Mesoporous oxide of titanium
View Patent ↗This invention pertains to mesoporous oxide of titanium and processes of making mesoporous oxide of titanium particularly crystalline oxide of titanium.
1. A process for making a mesoporous oxide of titanium, comprising:
(a) forming a mixture by combining starting materials comprising:
(i) a titanium oxychloride
(ii) a base selected from the group consisting of ammonium hydroxide, ammonium carbonate, ammonium bicarbonate, tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide or mixtures thereof, and
(iii) a solvent selected from the group consisting of ethanol, n-propanol, i-propanol, dimethyl acetamide, alcoholic ammonium halide and aqueous ammonium halide or mixtures thereof
wherein the mixture has a pH in the range of about 4-10 and forms a precipitate comprising a chloride salt and a hydrous titanium oxide,
(b) heating portions of the precipitate at a temperature greater than about 300° C. to remove the chloride salt, and
(c) recovering
a mesoporous oxide of titanium having a pore volume of at least about 0.5 cc/g and an average pore diameter of at least about 200 Å.
2. The process of claim 1 wherein the chloride salt is ammonium chloride.
3. The process of claim 1 wherein the chloride salt is selected from the group consisting of ammonium chloride, tetramethyl ammonium chloride or tetraethyl ammonium chloride or mixtures thereof.
4. The process of claim 1 wherein more than about 50 weight percent of the chloride salt precipitates from the mixture, the weight percent based on the total amount of the chloride salt that can form from the mixture.
5. The process of claim 1 wherein more than about 70 weight percent of the chloride salt precipitates from the mixture, the weight percent based on the total amount of the chloride salt that forms from the mixture.
6. The process of claim 1 wherein more than about 90 weight percent of the chloride salt precipitates from the reaction mixture, the weight percent based on the total amount of the chloride salt that forms from the mixture.
7. The process of claim 1 wherein the mixture has a pH in the range of about 5-9.
8. The process of claim 1 wherein the mixture has a pH in the range of about 6-8.