Synthetic mesoporous crystalline materials

Claim 1

A method for preparing a composition of matter comprising an inorganic, porous, non-layered crystalline phase material exhibiting, after calcination, an X-ray diffraction pattern with at least one peak at a d-spacing greater than 18 Angstrom Units and having a benzene adsorption capacity of greater than 15 grams benzene per 100 grams of said material at 6.7 kPa (50 torr) and 25° C., and a composition, expressed on an anhydrous basis as follows: M.sub.n/q (W.sub.a X.sub.b Y.sub.c Z.sub.d O.sub.h) wherein M is one or more ions; n is the charge of the composition excluding M expressed as oxides; q is the weighted molar average valence of M; n/q is the number of moles or mole fraction of M; W is one or more divalent elements; X is one or more trivalent elements; Y is one or more tetravalent elements; Z is one or more pentavalent elements; a, b, c, and d are mole fractions of W, X, Y, and Z, respectively; (a+b+c+d)=1; a≧ 0; b, c, and d are each >0; and h is a number of from 1 to 2.5, said method comprising: i) crystallizing a first reaction mixture having a composition in terms of mole ratios of oxides, within the following ranges: ______________________________________ WO/X.sub.2 O.sub.3 0.0 to 0.5 Z.sub.2 O.sub.5 /X.sub.2 O.sub.3 0.5 to 5 (WO + X.sub.2 O.sub.3)/Z.sub.2 O.sub.5 0.2 to 3 Solvent/ 4 to 500 (WO + X.sub.2 O.sub.3 + Z.sub.2 O.sub.5) (M.sub.2/e O + R.sub.2/f O + R'.sub.2/g O)/ 0.05 to 5 (WO + X.sub.2 O.sub.3 + Z.sub.2 O.sub.5) R'.sub.2/g O/R.sub.2/f O ≧0 ______________________________________ wherein e, f and g are the weighted average valences of M, R and R', respectively, wherein the solvent is a C 1 to C 6 alcohol or diol, or water and wherein R comprises an organic directing agent selected from the group consisting of aromatic amines, cyclic aliphatic amines and polycyclic aliphatic amines, and R' comprises an organic directing agent having the formula R 1 R 2 R 3 R 4 Q + , wherein Q is nitrogen or phosphorus and at least one of R 1 , R 2 , R 3 and R 4 is aryl or alkyl group having 6 to 36 carbon atoms and each of the remainder of R 1 , R 2 , R 3 and R 4 is selected from hydrogen and an alkyl group having 1 to 5 carbon atoms; ii) contacting the crystallized product of i) with a second reaction mixture having a composition in terms of mole ratios of oxides, within the following ranges: ______________________________________ R'.sub.2/g O/YO.sub.2 0.05 to 2 Solvent/YO.sub.2 20 to 1000 ______________________________________ wherein the product of i) is added to provide a mixture having 0.1 to 2 moles of X 2 O 3 per mole of YO 2 in the reaction mixture; and iii) maintaining the product of ii) under conditions sufficient to form said composition of matter.

Claim 2

A method for preparing a composition of matter comprising an inorganic, porous, non-layered crystalline phase material exhibiting, after calcination, an X-ray diffraction pattern with at least one peak at a d-spacing greater than 18 Angstrom Units and having a benzene adsorption capacity of greater than 15 grams benzene per 100 grams of said material at 6.7 kPa (50 torr) and 25° C., and a composition, expressed on an anhydrous basis as follows: M.sub.n/q (W.sub.a X.sub.b Y.sub.c Z.sub.d O.sub.h) wherein M is one or more ions; n is the charge of the composition excluding M expressed as oxides; q is the weighted molar average valence of M; n/q is the number of moles or mole fraction of M; W is one or more divalent elements; X is one or more trivalent elements; Y is one or more tetravalent elements; Z is one or more pentavalent elements; a, b, c, and d are mole fractions of W, X, Y, and Z, respectively; (a+b+c+d)=1; a≧ 0; b, c, and d are each >0; and h is a number of from 1 to 2.5, said method comprising: i) crystallizing a first reaction mixture having a composition in terms of mole ratios of oxides, within the following ranges: ______________________________________ WO/X.sub.2 O.sub.3 0.0 to 0.5 Z.sub.2 O.sub.5 /X.sub.2 O.sub.3 0.5 to 5 (WO + X.sub.2 O.sub.3)/Z.sub.2 O.sub.5 0.2 to 3 Solvent/ 4 to 500 (WO + X.sub.2 O.sub.3 + Z.sub.2 O.sub.5) (M.sub.2/e O + R.sub.2/f O + R'.sub.2/g O)/ 0.05 to 5 (WO + X.sub.2 O.sub.3 + Z.sub.2 O.sub.5) R'.sub.2/g O/R.sub.2/f O ≧0 ______________________________________ wherein e, f and g are the weighted average valences of M, R and R', respectively, wherein the solvent is a C 1 to C 6 alcohol or diol, or water and wherein R comprises an organic directing agent selected from the group consisting of aromatic amines, cyclic aliphatic amines and polycyclic aliphatic amines, and R' comprises an organic directing agent having the formula R 1 R 2 R 3 R 4 Q + , wherein Q is nitrogen or phosphorus and at least one of R 1 , R 2 , R 3 and R 4 is aryl or alkyl group having 6 to 36 carbon atoms and each of the remainder of R 1 , R 2 , R 3 and R 4 is selected from hydrogen and an alkyl group having 1 to 5 carbon atoms; ii) contacting the crystallized product of i) with a second reaction mixture having a composition in terms of mole ratios of oxides, within the following ranges: ______________________________________ R'.sub.2/g O/YO.sub.2 0.05 to 2 Solvent/YO.sub.2 20 to 1000 ______________________________________ wherein the product of i) is added to provide a mixture having 0.1 to 2 moles of X 2 O 3 per mole of YO 2 in the reaction mixture; and iii) maintaining the product of ii) under conditions sufficient to form said composition of matter.