Mesoporous amorphous oxide of titanium

Abstract

This invention pertains to a mesoporous amorphous oxide of titanium and processes of making a mesoporous amorphous oxide of titanium. This is not the same as Title

1 . A process for making a mesoporous amorphous hydrous oxide of titanium, comprising: 
 precipitating an ionic porogen and a hydrolyzed compound comprising titanium; and    removing the ionic porogen from the precipitate to recover a mesoporous hydrous oxide of titanium, the ionic porogen being in sufficient amount and the conditions of precipitating being effective for producing a mesoporous hydrous oxide of titanium having a surface area of at least about 400 m 2 /g and a pore volume of at least about 0.4 cc/g.    
   
   
       2 . The process of  claim 1  wherein the ionic porogen is a halide salt.  
   
   
       3 . The process of  claim 1  wherein the ionic porogen is ammonium chloride.  
   
   
       4 . The process of  claim 1  wherein the halide salt is ammonium halide, tetramethyl ammonium halide or tetraethyl ammonium halide or mixtures thereof.  
   
   
       5 . The process of  claim 1  wherein the ionic porogen is removed by washing.  
   
   
       6 . The process of  claim 1  wherein the oxide of titanium further comprises a dopant.  
   
   
       7 . The process of  claim 1  wherein the hydrolyzed compound comprising titanium is derived from titanium tetrachloride, titanium oxychloride or mixture thereof.  
   
   
       8 . The process of  claim 1  wherein at least 2 moles of the ionic porogen precipitates for each mole of the hydrolyzed compound comprising titanium that precipitates.  
   
   
       9 . The process of  claim 7  wherein the ionic porogen is a halide salt and at least 3 moles of the halide salt precipitates for each mole of the hydrolyzed compound comprising titanium that precipitates.  
   
   
       10 . The process of  claim 7  wherein the ionic porogen is a halide salt and at least 4 moles of the halide salt precipitates for each mole of the hydrolyzed compound comprising titanium that precipitates.  
   
   
       11 . A process for making a mesoporous amorphous oxide of titanium, comprising: 
 precipitating an ionic porogen and a hydrous oxide of titanium from a reaction mixture comprising a titanium starting material, a base and a solvent, wherein the titanium starting material or the solvent, or both, are a source of the anion for the ionic porogen and the base is the source of the cation for the ionic porogen, the precipitating being carried out under conditions effective for recovering a mesoporous oxide of titanium having a surface area of at least about 400 m 2 /g and a pore volume of at least about 0.4 cc/g after removing the ionic porogen from the precipitate.    
   
   
       12 . The process of  claim 11  wherein the ionic porogen is a halide salt.  
   
   
       13 . The process of  claim 11  wherein the ionic porogen is ammonium chloride.  
   
   
       14 . The process of  claim 12  wherein the halide salt is ammonium halide, tetramethyl ammonium halide or tetraethyl ammonium halide or mixture thereof.  
   
   
       15 . The process of  claim 11  wherein the ionic porogen is removed by washing.  
   
   
       16 . The process of  claim 11  wherein the titanium starting material is titanium tetrachloride, titanium oxychloride, or mixture thereof.  
   
   
       17 . The process of  claim 11  wherein the base is ammonium hydroxide, ammonium carbonate, ammonium bicarbonate, tetramethyl ammonium hydroxide or tetraethyl ammonium hydroxide or mixture thereof.  
   
   
       18 . The process of  claim 11  wherein the solvent is ethanol, n-propanol, i-propanol, dimethyl acetamide, alcoholic ammonium halide and aqueous ammonium halide or mixture thereof.  
   
   
       19 . The process of  claim 11  wherein the reaction mixture is formed by the steps, in order, of contacting the base and the solvent to form a solution or a mixture and adding the titanium starting material to the solution or mixture.  
   
   
       20 . The process of  claim 11  wherein the reaction mixture is formed by contacting the titanium starting material and the solvent to form a solution or a mixture and adding the base to the solution or mixture.  
   
   
       21 . The process of  claim 12  wherein more than about 50 weight percent of the halide salt precipitates from the reaction mixture, the weight percent based on the total amount of the halide salt that can form from the reaction mixture.  
   
   
       22 . The process of  claim 16  wherein the ionic porogen is a halide salt and more than about 70 weight percent of the halide salt precipitates from the reaction mixture, the weight percent based on the total amount of the halide salt that can form from the reaction mixture.  
   
   
       23 . The process of  claim 16  wherein the ionic porogen is a halide salt and more than about 90 weight percent of the halide salt precipitates from the reaction mixture, the weight percent based on the total amount of the halide salt that can form from the reaction mixture.  
   
   
       24 . A process for making a mesoporous amorphous oxide of titanium, the process comprising: 
 forming a mixture of a solid hydrolyzed starting material comprising titanium and a liquid medium;    adding a sufficient quantity of a halide salt to the mixture to saturate the liquid medium of the mixture;    recovering the solid from the saturated liquid medium, the solid comprising a hydrolyzed intermediate comprising titanium having pores containing the saturated liquid medium; and    removing the saturated liquid medium from the solid to recover a mesoporous oxide of titanium having a surface area of at least about 400 m 2 /g and a pore volume of at least about 0.4 cc/g.    
   
   
       25 . A mesoporous amorphous hydrous oxide of titanium having a microstructure characterized by a surface area of at least about 400 m 2 /g and a pore volume of at least about 0.4 cc/g.  
   
   
       26 . The composition of matter of  claim 25  further comprising a treatment with silica, alumina or both.  
   
   
       27 . A protective coating composition comprising the oxide of titanium of  claim 26 .  
   
   
       28 . The composition of matter of  claim 25  further comprising a treatment with an organic coating agent.  
   
   
       29 . A thermoplastic composition comprising the oxide of titanium of  claim 28 .  
   
   
       30 . A catalyst composition comprising the composition of matter of  claim 25 .  
   
   
       31 . A nanoparticle precursor comprising the composition of matter of  claim 25 .  
   
   
       32 . An optical device comprising the composition of matter of  claim 25 .  
   
   
       33 . A photovoltaic cell comprising the composition of matter of  claim 25 .  
   
   
       34 . A lithium battery anode comprising the composition of matter of  claim 25.