Method for Making Mesoporous or Combined Mesoporous and Microporous Inorganic Oxides

Abstract

A method for making a mesoporous or combined mesoporous/microporous inorganic oxide includes reacting a source of inorganic oxide with a complexing agent at a complexation temperature to provide a complex; decomposing the complex to provide a porous material precursor having an inorganic oxide framework containing at least some organic pore-forming agent; and removing the organic pore forming agent from the inorganic oxide framework by solvent extraction and/or calcination.

1 - 28 . (canceled) 
     
     
         29 . A method for making a mesoporous or combined mesoporous/microporous inorganic oxide comprising the steps of:
 a) reacting a source of inorganic oxide with an organic complexing and pore-forming agent at a complexation temperature to provide at least one complex, wherein said source of inorganic oxide is an inorganic compound;   b) decomposing the at least one complex to provide a porous material precursor having an inorganic oxide framework containing at least some organic complexing and pore-forming agent;   c) recovering and recycling at least a major portion of the organic complexing and pore-forming agent from the inorganic oxide framework by solvent extraction; and   d) calcining the inorganic oxide framework.   
     
     
         30 . The method of  claim 29  wherein the source of inorganic oxide comprises at least one inorganic oxide of at least one element of one of Groups IVB, VB, VIB, VIIB, III, IB, IIB, IIIB, VIII, VA, IIIA, IVA, IIA and lanthanide of the Periodic Table of the Elements. 
     
     
         31 . The method of  claim 30  wherein the inorganic oxide comprises at least one oxide of at least one element selected from the group consisting of Si, Al, Ti, V, Cr, Zn, Fe, Sn, Mo, Ga, Ni, Co, Zr, Cu, Mg, Bi, Nb, Mn, Zr, Sb, La, Ce, Te and W. 
     
     
         32 . The method of  claim 29  wherein the source of inorganic oxide is selected from hydrated or unhydrated oxides, hydroxides, nitrates, carbonates, or ammonium salts of at least one metal selected from the group consisting of Si, Al, Ti, V, Cr, Zn, Fe, Sn, Mo, Ga, Ni, Co, Zr, Cu, Mg, Bi, Nb, Mn, Zr, Sb, La, Te, Ce and W. 
     
     
         33 . The method of  claim 29  wherein the source of inorganic oxide is silica source, selected from the group consisting of silica gel, silica hydrogel, silica aerogel, and fumed silica. 
     
     
         34 . The method of  claim 29  wherein the source of inorganic oxide is aluminum hydroxide or alumina. 
     
     
         35 . The method of  claim 29  wherein the source of inorganic oxide is selected from the group consisting of magnesium oxide and magnesium hydroxide. 
     
     
         36 . The method of  claim 29  wherein the organic complexing and pore-forming agent is an organic compound having amino groups. 
     
     
         37 . The method of  claim 36  wherein the organic complexing and pore-forming agent is an alkanolamine. 
     
     
         38 . The method of  claim 37  wherein the alkanolamine is selected from the group consisting of thiethanolamine, tri-isopropanolamine, tripropanolamine, tris-hydroxymethyleneaminomethane, N,N-dimethylethanolamine and combinations thereof. 
     
     
         39 . The method of  claim 29  wherein the step (b) of decomposing the complex comprises hydrolysis of the complex with an acidic, basic or neutral pH aqueous fluid. 
     
     
         40 . The method of  claim 29  wherein the step (b) of decomposing the complex comprises calcining the complex at a temperature of from about 251° C. to about 400° C. 
     
     
         41 . The method of  claim 29  wherein the solvent extraction comprises immersing the porous material precursor in a solvent selected from the group consisting of water, alcohols, ethers, ketones, esters and combinations thereof. 
     
     
         42 . The method of  claim 29  wherein the calcination of step (c) comprises heating the porous material precursor to a temperature of from about 401° C. to about 1100° C. for a period of time ranging up to about 48 hours. 
     
     
         43 . The method of  claim 29  further comprising the step of aging the porous material precursor at a temperature of from about 20° C. to about 120° C. for a period of time ranging up to about 48 hours. 
     
     
         44 . The method of  claim 29  further comprising the step of drying the porous material precursor after ageing the porous material precursor. 
     
     
         45 . The method of  claim 29  further comprising the step of heating the porous material precursor under above atmospheric pressure for a period of time of up to about 4 days. 
     
     
         46 . The method of  claim 29  further comprising the step of adding a zeolite to the complex of step (a). 
     
     
         47 . The method of  claim 46  wherein said zeolite is selected from the group consisting of zeolite Y, zeolite X, zeolite L, zeolite A, zeolite beta, mordenite, SSZ-32, ZSM-5, ZSM-11, ZSM-22, ZSM-23, ZSM-48, ZSM-58, MCM-22, MCM-36, PSH-3, silicalite-1 and silicalite-2. 
     
     
         48 . A method for making a mesoporous or combined mesoporous/microporous inorganic oxide comprising the steps of:
 a) reacting an inorganic oxide with the organic complexing and mesopore-forming agent at a complexation temperature to provide at least one complex wherein the organic complexing and mesopore-forming agent is combined with a glycol solvent;   b) decomposing the at least one complex to provide a porous material precursor having an inorganic oxide framework containing at least some organic complexing and mesopore-forming agent; and   c) removing at least a major portion of the organic complexing and mesopore-forming agent from the inorganic oxide framework by solvent extraction and/or calcination.   
     
     
         49 . The method of  claim 48  wherein the organic complexing and pore-forming agent is an alkanolamine. selected from the group consisting of triethanolamine, tri-isopropanolamine, tripropanolamine, tris-hydroxymethyleneaminomethane, N,N-dimethylethanolamine and combinations thereof. 
     
     
         50 . The method of  claim 49  wherein the organic complexing and mesopore-forming agent is triethanolamine and the glycol solvent is ethylene glycol. 
     
     
         51 . The method of  claim 48  wherein the inorganic oxide framework is characterized by an X-ray diffraction pattern having at least one peak at 0.3 to 3.5 degrees in 2 ⊖.