Synthesis of crystalline ultra-large pore oxide materials

Claim 1

A method for preparing a composition of matter comprising an inorganic, crystalline phase exhibiting an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing with a relative intensity of 100, and a benzene adsorption capacity of greater than about 15 grams benzene per 100 grams anhydrous crystal at 50 torr and 25° C., said method comprising the steps of: (a) forming a reaction mixture comprising an amphiphilic compound, a source of at least one oxide and water, wherein the molar ratio of amphiphilic compound to water is less than 0.004; (b) maintaining said reaction mixture under sufficient conditions to form a crystalline oxide material; and (c) recovering said crystalline oxide material.

Claim 2

A method for preparing a composition of matter comprising an inorganic, crystalline phase exhibiting an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing with a relative intensity of 100, and a benzene adsorption capacity of greater than about 15 grams benzene per 100 grams anhydrous crystal at 50 torr and 25° C., said method comprising the steps of: (a) forming a reaction mixture comprising an amphiphilic compound, a source of at least one oxide and water, wherein the molar ratio of amphiphilic compound to water is less than 0.004; (b) maintaining said reaction mixture under sufficient conditions to form a crystalline oxide material; and (c) recovering said crystalline oxide material.

Claim 7

A method for preparing a composition of matter comprising an inorganic, crystalline phase exhibiting, after calcination, an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing with a relative intensity of 100, and a benzene adsorption capacity of greater than about 15 grams benzene per grams anhydrous crystal at 50 torr and 25° C., said method comprising the steps of: (a) forming a reaction mixture comprising an amphiphilic compound, a source of at least one oxide and water, wherein the molar ratio of amphiphilic compound to water is less than 0.004; (b) maintaining said reaction mixture under sufficient conditions to form a crystalline oxide material; (c) recovering said crystalline oxide material in as-synthesized form comprising residual amphiphilic compound, said as-synthesized form of said material having an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing with a relative intensity of 100, said as-synthesized form of said material not being stable to calcination conditions sufficient to remove said residual amphiphilic compound; (d) stabilizing said material from step (c) to calcination conditions by treating said material from step (c) with a compound of the formula M'X'.sub.2 Y'm where M' is boron, aluminum, silicon or titanium; X' represents alkyl halides having from 1-6 carbon atoms and/or alkoxides having 1-6 carbon atoms; Y' represents X' and/or alkyls with 1-12 carbon atoms; and m=1-2; and (e) calcining said material from step (d) under conditions sufficient to remove residual organic compounds.

Claim 8

A method for preparing a composition of matter comprising an inorganic, crystalline phase exhibiting, after calcination, an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing with a relative intensity of 100, and a benzene adsorption capacity of greater than about 15 grams benzene per grams anhydrous crystal at 50 torr and 25° C., said method comprising the steps of: (a) forming a reaction mixture comprising an amphiphilic compound, a source of at least one oxide and water, wherein the molar ratio of amphiphilic compound to water is less than 0.004; (b) maintaining said reaction mixture under sufficient conditions to form a crystalline oxide material; (c) recovering said crystalline oxide material in as-synthesized form comprising residual amphiphilic compound, said as-synthesized form of said material having an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing with a relative intensity of 100, said as-synthesized form of said material not being stable to calcination conditions sufficient to remove said residual amphiphilic compound; (d) stabilizing said material from step (c) to calcination conditions by treating said material from step (c) with a compound of the formula M'X'.sub.2 Y'm where M' is boron, aluminum, silicon or titanium; X' represents alkyl halides having from 1-6 carbon atoms and/or alkoxides having 1-6 carbon atoms; Y' represents X' and/or alkyls with 1-12 carbon atoms; and m=1-2; and (e) calcining said material from step (d) under conditions sufficient to remove residual organic compounds.

Claim 13

A method for preparing a composition of matter comprising an inorganic, crystalline phase exhibiting, after, calcination, an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing with a relative intensity of 100, and a benzene adsorption capacity of greater than about 15 grams benzene per grams anhydrous crystal at 50 torr and 25.C, said method comprising the steps of: (a) forming a reaction mixture comprising an amphiphilic compound, a source of at least one oxide, an inorganic salt, and water, wherein the molar ratio of amphiphilic compound to water is less than 0.004; (b) maintaining said reaction mixture under sufficient conditions to form a crystalline oxide material; (c) recovering said crystalline oxide material in as-synthesized form comprising residual amphiphilic compound, said as-synthesized form of said material having an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing with a relative intensity of 100, said as-synthesized form of said material being stable to calcination conditions sufficient to remove said residual amphiphilic compound; (d) calcining said material from step (c) under conditions sufficient to remove said residual amphiphilic compound.

Claim 14

A method for preparing a composition of matter comprising an inorganic, crystalline phase exhibiting, after, calcination, an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing with a relative intensity of 100, and a benzene adsorption capacity of greater than about 15 grams benzene per grams anhydrous crystal at 50 torr and 25.C, said method comprising the steps of: (a) forming a reaction mixture comprising an amphiphilic compound, a source of at least one oxide, an inorganic salt, and water, wherein the molar ratio of amphiphilic compound to water is less than 0.004; (b) maintaining said reaction mixture under sufficient conditions to form a crystalline oxide material; (c) recovering said crystalline oxide material in as-synthesized form comprising residual amphiphilic compound, said as-synthesized form of said material having an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing with a relative intensity of 100, said as-synthesized form of said material being stable to calcination conditions sufficient to remove said residual amphiphilic compound; (d) calcining said material from step (c) under conditions sufficient to remove said residual amphiphilic compound.