US5057296A — Method for synthesizing mesoporous crystalline ma…

Claim 1

Independent Claim 353 words

A method for synthesizing a composition of matter comprising an inorganic, non-layered, porous crystalline phase material having, after calcination, an arrangement of uniformly-sized pores having diameters of at least about 13 Angstrom Units, exhibiting an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing and exhibiting a benzene adsorption capacity of greater than about 15 grams benzene per 100 grams at 50 torr and 25° C., which comprises (i) preparing a reaction mixture capable of forming said composition, said mixture comprising one or a combination of oxides selected from the group consisting of divalent element, trivalent element, tetravalent element and pentavalent element, organic directing agent and solvent or solvent mixture, said organic directing agent comprising an ion of the formula R 1 R 2 R 3 R 4 Q 30 , wherein Q is nitrogen or phosphorus and wherein at least one of R 1 , R 2 , R 3 and R 4 is selected from the group consisting of aryl of from 6 to about 36 carbon atoms, alkyl of from 6 to about 36 carbon atoms and combinations thereof, the remainder of R 1 , R 2 , R 3 and R 4 being selected from the group consisting of hydrogen, alkyl of from 1 to 5 carbon atoms and combinations thereof, (ii) maintaining said mixture under sufficient conditions of pH, temperature and time for formation of said composition of matter and (iii) recovering said composition of matter, wherein added to said reaction mixture is an auxiliary organic selected from the group consisting of (1) aromatic hydrocarbons and amines of from 5 to 20 carbons and halogen- and C 1 -C 14 alkyl-substituted derivatives thereof, (2) cyclic aliphatic hydrocarbons and amines of from 5 to 20 carbons and halogen- and C 1 -C 14 alkyl-substituted derivatives thereof, (3) polycyclic aliphatic hydrocarbons and amines of from 6 to 20 carbons and halogen- and C 1 -C 14 alkyl-substituted derivatives thereof, (4) straight and branched aliphatic hydrocarbons and amines of from 3 to 16 carbons and halogen-substituted derivatives thereof, and (5) combinations thereof.

Claim 2

Independent Claim 353 words

A method for synthesizing a composition of matter comprising an inorganic, non-layered, porous crystalline phase material having, after calcination, an arrangement of uniformly-sized pores having diameters of at least about 13 Angstrom Units, exhibiting an X-ray diffraction pattern with at least one peak at a position greater than about 18 Angstrom Units d-spacing and exhibiting a benzene adsorption capacity of greater than about 15 grams benzene per 100 grams at 50 torr and 25° C., which comprises (i) preparing a reaction mixture capable of forming said composition, said mixture comprising one or a combination of oxides selected from the group consisting of divalent element, trivalent element, tetravalent element and pentavalent element, organic directing agent and solvent or solvent mixture, said organic directing agent comprising an ion of the formula R 1 R 2 R 3 R 4 Q 30 , wherein Q is nitrogen or phosphorus and wherein at least one of R 1 , R 2 , R 3 and R 4 is selected from the group consisting of aryl of from 6 to about 36 carbon atoms, alkyl of from 6 to about 36 carbon atoms and combinations thereof, the remainder of R 1 , R 2 , R 3 and R 4 being selected from the group consisting of hydrogen, alkyl of from 1 to 5 carbon atoms and combinations thereof, (ii) maintaining said mixture under sufficient conditions of pH, temperature and time for formation of said composition of matter and (iii) recovering said composition of matter, wherein added to said reaction mixture is an auxiliary organic selected from the group consisting of (1) aromatic hydrocarbons and amines of from 5 to 20 carbons and halogen- and C 1 -C 14 alkyl-substituted derivatives thereof, (2) cyclic aliphatic hydrocarbons and amines of from 5 to 20 carbons and halogen- and C 1 -C 14 alkyl-substituted derivatives thereof, (3) polycyclic aliphatic hydrocarbons and amines of from 6 to 20 carbons and halogen- and C 1 -C 14 alkyl-substituted derivatives thereof, (4) straight and branched aliphatic hydrocarbons and amines of from 3 to 16 carbons and halogen-substituted derivatives thereof, and (5) combinations thereof.

Claim 3

Dependent Claim 32 words

The method of claim 1 wherein said auxiliary organic is present in said reaction mixture such that the mole ratio of auxiliary organic/tetravalent element oxide is from about 0.05 to about 20.

Claim 4

Dependent Claim 45 words

The method of claim 1 wherein said auxiliary organic is selected from the group consisting of an aromatic hydrocarbon of 6 to 20 carbons; a cyclic aliphatic hydrocarbon of 5 to 20 carbons; a polycyclic aliphatic hydrocarbon of 6 to 20 carbons; and combinations thereof.

Claim 5

Dependent Claim 46 words

The method of claim 1 wherein said auxiliary organic is selected from the group consisting of a straight chain aliphatic hydrocarbon of from about 3 to about 16 carbon atoms, branched chain aliphatic hydrocarbon of from about 3 to about 16 carbon atoms and combinations thereof.

Claim 6

Dependent Claim 34 words

The method of claim 3 wherein said auxiliary organic is selected from the group consisting of benzene, alkyl-substituted benzene, alkyl-substituted adamantane and combinations thereof, alkyl being of from 1 to about 14 carbon atoms.

Claim 7

Dependent Claim 23 words

The method of claim 5 wherein said auxiliary organic is selected from the group consisting of p-xylene, trimethylbenzene, triethylbenzene, dimethyladamantane and combinations thereof.

Claim 8

Dependent Claim 27 words

The method of claim 1 wherein said auxiliary organic is selected from the group consisting of pentane, hexane, heptane, octane, nonane, decane, dodecane, dihalooctane and combinations thereof.

Claim 9

Dependent Claim 32 words

The method of claim 3 wherein said auxiliary organic is present in said reaction mixture such that the mole ratio of auxiliary organic/tetravalent element oxide is from about 0.1 to about 10.

Claim 10

Dependent Claim 32 words

The method of claim 4 wherein said auxiliary organic is present in said reaction mixture such that the mole ratio of auxiliary organic/tetravalent element oxide is from about 0.1 to about 10.

Claim 11

Dependent Claim 179 words

The method of claim 1 wherein said reaction mixture has a composition, in terms of mole ratios, within the following ranges: ______________________________________ X.sub.2 O.sub.3 /YO.sub.2 0 to 0.5 Al.sub.2 O.sub.3 /SiO.sub.2 0 to 0.01 X.sub.2 O.sub.3 /(YO.sub.2 + Z.sub.2 O.sub.5) 0.1 to 100 X.sub.2 O.sub.3 /(YO.sub.2 + W'O + Z.sub.2 O.sub.5) 0.1 to 100 Solvent/ 1 to 1500 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) OH.sup.- /YO.sub.2 0 to 10 (M.sub.2/e O + R.sub.2/f O)/ 0.01 to 20 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) M.sub.2/e O/ 0 to 10 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) R.sub.2/f O/ 0.01 to 2.0 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) Auxiliary Organic/YO.sub.2 0.05 to 20 Auxiliary Organic/R.sub.2/f O 0.02 to 100 ______________________________________ wherein M is said alkali or alkaline earth metal cation, W' is said divalent element, X is said trivalent element, Y is said tetravalent element, Z is said pentavalent element, R is said organic directing agent, and e and f are the weighted average valences of M and R, respectively.

Claim 12

Dependent Claim 44 words

The method of claim 10 wherein said auxiliary organic is selected from the group consisting of an aromatic hydrocarbon of 6 to 20 carbons; a cyclic aliphatic hydrocarbon of 5 to 20 carbons; a polycyclic aliphatic of 6 to 20 carbons; and combinations thereof.

Claim 13

Dependent Claim 46 words

The method of claim 10 wherein said auxiliary organic is selected from the group consisting of a straight chain aliphatic hydrocarbon of from about 3 to about 16 carbon atoms, branched chain aliphatic hydrocarbon of from about 3 to about 16 carbon atoms and combinations thereof.

Claim 14

Dependent Claim 23 words

The method of claim 10 wherein R is selected from the group consisting of cetyltrimethylammonium, octadecyltrimethylammonium, benzyltrimethylammonium, cetylpryidinium, myristyltrimethylammonium, decyltrimethylammonium, dodecyltrimethylammonium and dimethyldidodecylammonium.

Claim 15

Dependent Claim 323 words

The method of claim 1 wherein said reaction mixture has a composition, in terms of mole ratios, within the following ranges: ______________________________________ X.sub.2 O.sub.3 /YO.sub.2 0 to 0.5 X.sub.2 O.sub.3 /(YO.sub.2 + Z.sub.2 O.sub.5) 0.1 to 100 X.sub.2 O.sub.3 /(YO.sub.2 + W'O + Z.sub.2 O.sub.5) 0.1 to 100 Solvent/ 1 to 1500 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) OH.sup.- /YO.sub.2 0 to 10 (M.sub.2/e O + R.sub.2/f O)/ 0.01 to 20 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) M.sub.2/e O/ 0 to 10 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) R.sub.2/f O/ 0.01 to 2.0 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) Auxiliary Organic/YO.sub.2 0.05 to 20 Auxiliary Organic/R.sub.2/f O 0.02 to 100 ______________________________________ wherein M is said alkali or alkaline earth metal cation, W' is said divalent element, X is said trivalent element, Y is said tetravalent element, Z is said pentavalent element, R comprises a mixture of component (a) an ion of the formula R 1 R 2 R 3 R 4 Q + , wherein Q is nitrogen or phosphorus and wherein at least one of R 1 , R 2 , R 3 and R 4 is selected from the group consisting of aryl of from 6 to about 36 carbon atoms, alkyl of from 6 to about 36 carbon atoms and combinations thereof, the remainder of R 1 , R 2 , R 3 and R 4 being selected from the group consisting of hydrogen, alkyl of from 1 to 5 carbon atoms and combinations thereof, and component (b) an additional ion of the formula R 1 R 2 R 3 R 4 Q + wherein R 1 , R 2 , R 3 and R 4 are selected from the group consisting of hydrogen, alkyl of 1 to 5 carbon atoms and combinations thereof, and wherein e and f are weighted average valences of M and R, respectively.

Claim 16

Dependent Claim 44 words

The method of claim 14 wherein said auxiliary organic is selected from the group consisting of an aromatic hydrocarbon of 6 to 20 carbons; a cyclic aliphatic hydrocarbon of 5 to 20 carbons; a polycyclic aliphatic of 6 to 20 carbons; and combinations thereof.

Claim 17

Dependent Claim 46 words

The method of claim 14 wherein said auxiliary organic is selected from the group consisting of a straight chain aliphatic hydrocarbon of from about 3 to about 16 carbon atoms, branched chain aliphatic hydrocarbon of from about 3 to about 16 carbon atoms and combinations thereof.

Claim 18

Dependent Claim 23 words

The method of claim 14 wherein R is selected from the group consisting of cetyltrimethylammonium, octadecyltrimethylammonium, benzyltrimethylammonium, cetylpryidinium, myristyltrimethylammonium, decyltrimethylammonium, dodecyltrimethylammonium and dimethyldidodecylammonium.

Claim 19

Dependent Claim 108 words

The method of claim 1 wherein said reaction mixture has a composition, in terms of mole ratios, within the following ranges: ______________________________________ Al.sub.2 O.sub.3 /SiO.sub.2 0 to 0.1 Solvent/SiO.sub.2 1 to 1500 OH.sup.- /SiO.sub.2 0 to 10 (M.sub.2/e O + R.sub.2/f O)/ 0.01 to 20 (SiO.sub.2 + Al.sub.2 O.sub.3) M.sub.2/e O/ 0 to 5 (SiO.sub.2 + Al.sub.2 O.sub.3) R.sub.2/f O/ 0.01 to 2 (SiO.sub.2 + Al.sub.2 O.sub.3) Auxiliary Organic/SiO.sub.2 0.05 to 20 Auxiliary Organic/R.sub.2/f O 0.02 to 100 ______________________________________ wherein M is said alkali or alkaline earth metal cation, R is said organic direction agent, e and f are the weighted average valences of M and R, respectively.

Claim 20

Dependent Claim 44 words

The method of claim 18 wherein said auxiliary organic is selected from the group consisting of an aromatic hydrocarbon of 6 to 20 carbons; a cyclic aliphatic hydrocarbon of 5 to 20 carbons; a polycyclic aliphatic of 6 to 20 carbons; and combinations thereof.

Claim 21

Dependent Claim 46 words

The method of claim 18 wherein said auxiliary organic is selected from the group consisting of a straight chain aliphatic hydrocarbon of from about 3 to about 16 carbon atoms, branched chain aliphatic hydrocarbon of from about 3 to about 16 carbon atoms and combinations thereof.

Claim 22

Dependent Claim 23 words

The method of claim 18 wherein R is selected from the group consisting of cetyltrimethylammonium, octadecyltrimethylammonium, benzyltrimethylammonium, cetylpryidinium, myristyltrimethylammonium, decyltrimethylammonium, dodecyltrimethylammonium and dimethyldidodecylammonium.

Claim 23

Dependent Claim 17 words

The method of claim 18 wherein said source of an oxide of silicon comprises an organic silicate.

Claim 24

Dependent Claim 14 words

The method of claim 22 wherein said organic silicate comprises a quaternary ammonium silicate.

Claim 25

Dependent Claim 11 words

The method of claim 22 wherein said organic silicate comprises tetraethylorthosilicate.

Claim 26

Dependent Claim 49 words

The method of claim 1 wherein said crystalline phase has, after calcination, a hexagonal arrangement of uniformly-sized pores having diameters of at least about 13 Angstrom Units and exhibits a hexagonal electron diffraction pattern than can be indexed with a d 100 value greater than about 18 Angstrom Units.

Claim 27

Dependent Claim 32 words

The method of claim 25 wherein said auxiliary organic is present in said reaction mixture such that the mole ratio of auxiliary organic/tetravalent element oxide is from about 0.05 to about 20.

Claim 28

Dependent Claim 44 words

The method of claim 25 wherein said auxiliary organic is selected from the group consisting of an aromatic hydrocarbon of 6 to 20 carbons; a cyclic aliphatic hydrocarbon of 5 to 20 carbons; a polycyclic aliphatic of 6 to 20 carbons; and combinations thereof.

Claim 29

Dependent Claim 45 words

The method of claim 25 wherein said auxiliary organic is selected from the group consisting of a straight chain aliphatic hydrocarbon of about 3 to about 16 carbon atoms, branched chain aliphatic hydrocarbon of from about 3 to about 16 carbon atoms and combinations thereof.

Claim 30

Dependent Claim 34 words

The method of claim 25 wherein said auxiliary organic is selected from the group consisting of benzene, alkyl-substituted benzene, alkyl-substituted adamantane and combinations thereof, alkyl being of from 1 to about 14 carbon atoms.

Claim 31

Dependent Claim 23 words

The method of claim 25 wherein said auxiliary organic is selected from the group consisting of p-xylene, trimethylbenzene, triethylbenzene, dimethyladamantane and combinations thereof.

Claim 32

Dependent Claim 28 words

The method of claim 25 wherein said auxiliary organic is selected from the group consisting of pentane, hexane, heptane, octane, nonane, decane, dodecane, octadecane, dihalooctane and combinations thereof.

Claim 33

Dependent Claim 32 words

The method of claim 27 wherein said auxiliary organic is present in said reaction mixture such that the mole ratio of auxiliary organic/tetravalent element oxide is from about 0.05 to about 20.

Claim 34

Dependent Claim 32 words

The method of claim 28 wherein said auxiliary organic is present in said reaction mixture such that the mole ratio of auxiliary organic/tetravalent element oxide is from about 0.05 to about 20.

Claim 35

Dependent Claim 179 words

The method of claim 25 wherein said reaction mixture has a composition, in terms of mole ratios, within the following ranges: ______________________________________ X.sub.2 O.sub.3 /YO.sub.2 0 to 0.5 Al.sub.2 O.sub.3 /SiO.sub.2 0 to 0.01 X.sub.2 O.sub.3 /(YO.sub.2 + Z.sub.2 O.sub.5) 0.1 to 100 X.sub.2 O.sub.3 /(YO.sub.2 + W'O + Z.sub.2 O.sub.5) 0.1 to 100 Solvent/ 1 to 1500 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) OH.sup.- /YO.sub.2 0 to 10 (M.sub.2/e O + R.sub.2/f O)/ 0.01 to 20 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) M.sub.2/e O/ 0 to 10 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) R.sub.2/f O/ 0.01 to 2.0 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) Auxiliary Organic/YO.sub.2 0.05 to 20 Auxiliary Organic/R.sub.2/f O 0.02 to 100 ______________________________________ wherein M is said alkali or alkaline earth metal cation, W' is said divalent element, X is said trivalent element, Y is said tetravalent element, Z is said pentavalent element, R is said organic directing agent, and e and f are the weighted average valences of M and R, respectively.

Claim 36

Dependent Claim 323 words

The method of claim 25 wherein said reaction mixture has a composition, in terms of mole ratios, within the following ranges: ______________________________________ X.sub.2 O.sub.3 /YO.sub.2 0 to 0.5 X.sub.2 O.sub.3 /(YO.sub.2 + Z.sub.2 O.sub.5) 0.1 to 100 X.sub.2 O.sub.3 /(YO.sub.2 + W'O + Z.sub.2 O.sub.5) 0.1 to 100 Solvent/ 1 to 1500 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) OH.sup.- /YO.sub.2 0 to 10 (M.sub.2/e O + R.sub.2/f O)/ 0.01 to 20 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) M.sub.2/e O/ 0 to 10 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) R.sub.2/f O/ 0.01 to 2.0 (YO.sub.2 + W'O + Z.sub.2 O.sub.5 + X.sub.2 O.sub.3) Auxiliary Organic/YO.sub.2 0.05 to 20 Auxiliary Organic/R.sub.2/f O 0.02 to 100 ______________________________________ wherein M is said alkali or alkaline earth metal cation, W' is said divalent element, X is said trivalent element, Y is said tetravalent element, Z is said pentavalent element, R comprises a mixture of component (a) an ion of the formula R 1 R 2 R 3 R 4 Q + , wherein Q is nitrogen or phosphorus and wherein at least one of R 1 , R 2 , R 3 and R 4 is selected from the group consisting of aryl of from 6 to about 36 carbon atoms, alkyl of from 6 to about 36 carbon atoms and combinations thereof, the remainder of R 1 , R 2 , R 3 and R 4 being selected from the group consisting of hydrogen, alkyl of from 1 to 5 carbon atoms and combinations thereof, and component (b) an additional ion of the formula R 1 R 2 R 3 R 4 Q + wherein R 1 , R 2 , R 3 and R 4 are selected from the group consisting of hydrogen, alkyl of 1 to 5 carbon atoms and combinations thereof, and wherein e and f are weighted average valences of M and R, respectively.

Claim 37

Dependent Claim 108 words

The method of claim 25 wherein said reaction mixture has a composition, in terms of mole ratios, within the following ranges: ______________________________________ Al.sub.2 O.sub.3 /SiO.sub.2 0 to 0.1 Solvent/SiO.sub.2 1 to 1500 OH.sup.- /SiO.sub.2 0 to 10 (M.sub.2/e O + R.sub.2/f O)/ 0.01 to 20 (SiO.sub.2 + Al.sub.2 O.sub.3) M.sub.2/e O/ 0 to 5 (SiO.sub.2 + Al.sub.2 O.sub.3) R.sub.2/f O/ 0.01 to 2 (SiO.sub.2 + Al.sub.2 O.sub.3) Auxiliary Organic/SiO.sub.2 0.05 to 20 Auxiliary Organic/R.sub.2/f O 0.02 to 100 ______________________________________ wherein M is said alkali or alkaline earth metal cation, R is said organic directing agent, e and f are the weighted average valences of M and R, respectively.

Claim 38

Independent Claim 369 words

A method for synthesizing a composition of matter comprising an inorganic, non-layered, porous crystalline phase material having, after calcination, an arrangement of uniformly-sized pores having diameters of at least about 13 Angstrom Units, exhibiting an X-ray diffraction pattern with at least two peaks at positions greater than about 10 Angstrom Units d-spacing, at least one of which is at a position greater than about 18 Angstrom Units d-spacing, and no peaks at positions less than about 10 Angstrom Units d-spacing with relative intensity greater than about 20% of the strongest peak, which comprises (i) preparing a reaction mixture capable of forming said composition, said mixture comprising one or a combination of oxides selected from the group consisting of divalent element, trivalent element, tetravalent element and pentavalent element, organic directing agent and solvent or solvent mixture, said organic directing agent comprising an ion of the formula R 1 R 2 R 3 R 4 Q 30 , wherein Q is nitrogen or phosphorus and wherein at least one of R 1 , R 2 , R 3 and R 4 is selected from the group consisting of aryl of from 6 to about 36 carbon atoms, alkyl of from 6 to about 36 carbon atoms and combinations thereof, the remainder of R 1 , R 2 , R 3 and R 4 being selected from the group consisting of hydrogen, alkyl of from 1 to 5 carbon atoms and combinations thereof, (ii) maintaining said mixture under sufficient conditions of pH, temperature and time for formation of said composition of matter and (iii) recovering said composition of matter, wherein added to said reaction mixture is an auxiliary organic selected from the group consisting of (1) aromatic hydrocarbons and amines of from 5 to 20 carbons and halogen- and C 1 -C 14 alkyl-substituted derivatives thereof, (2) cyclic aliphatic hydrocarbons and amines of from 5 to 20 carbons and halogen- and C 1 -C 14 alkyl-substituted derivatives thereof, (3) polycyclic aliphatic hydrocarbons and amines of from 6 to 20 carbons and halogen- and C 1 -C 14 alkyl-substituted derivatives thereof, (4) straight and branched aliphatic hydrocarbons and amines of from 3 to 16 carbons and halogen-substituted derivatives thereof, and (5) combinations thereof.

Claim 39

Independent Claim 369 words

A method for synthesizing a composition of matter comprising an inorganic, non-layered, porous crystalline phase material having, after calcination, an arrangement of uniformly-sized pores having diameters of at least about 13 Angstrom Units, exhibiting an X-ray diffraction pattern with at least two peaks at positions greater than about 10 Angstrom Units d-spacing, at least one of which is at a position greater than about 18 Angstrom Units d-spacing, and no peaks at positions less than about 10 Angstrom Units d-spacing with relative intensity greater than about 20% of the strongest peak, which comprises (i) preparing a reaction mixture capable of forming said composition, said mixture comprising one or a combination of oxides selected from the group consisting of divalent element, trivalent element, tetravalent element and pentavalent element, organic directing agent and solvent or solvent mixture, said organic directing agent comprising an ion of the formula R 1 R 2 R 3 R 4 Q 30 , wherein Q is nitrogen or phosphorus and wherein at least one of R 1 , R 2 , R 3 and R 4 is selected from the group consisting of aryl of from 6 to about 36 carbon atoms, alkyl of from 6 to about 36 carbon atoms and combinations thereof, the remainder of R 1 , R 2 , R 3 and R 4 being selected from the group consisting of hydrogen, alkyl of from 1 to 5 carbon atoms and combinations thereof, (ii) maintaining said mixture under sufficient conditions of pH, temperature and time for formation of said composition of matter and (iii) recovering said composition of matter, wherein added to said reaction mixture is an auxiliary organic selected from the group consisting of (1) aromatic hydrocarbons and amines of from 5 to 20 carbons and halogen- and C 1 -C 14 alkyl-substituted derivatives thereof, (2) cyclic aliphatic hydrocarbons and amines of from 5 to 20 carbons and halogen- and C 1 -C 14 alkyl-substituted derivatives thereof, (3) polycyclic aliphatic hydrocarbons and amines of from 6 to 20 carbons and halogen- and C 1 -C 14 alkyl-substituted derivatives thereof, (4) straight and branched aliphatic hydrocarbons and amines of from 3 to 16 carbons and halogen-substituted derivatives thereof, and (5) combinations thereof.

Claim 40

Dependent Claim 49 words

The method of claim 37 wherein said crystalline phase has, after calcination, a hexagonal arrangement of uniformly-sized pores having diameters of at least about 13 Angstrom Units and exhibits a hexagonal electron diffraction pattern than can be indexed with a d 100 value greater than about 18 Angstroms Units.

Claim 41

Dependent Claim 32 words

The method of claim 38 wherein said auxiliary organic is present in said reaction mixture such that the mole ratio of auxiliary organic/tetravalent element oxide is from about 0.05 to about 20.

Claim 42

Dependent Claim 44 words

The method of claim 38 wherein said auxiliary organic is selected form the group consisting of an aromatic hydrocarbon of 6 to 20 carbons; a cyclic aliphatic hydrocarbon of 5 to 20 carbons; a polycyclic aliphatic of 6 to 20 carbons; and combinations, thereof.

Claim 43

Dependent Claim 46 words

The method of claim 38 wherein said auxiliary organic is selected from the group consisting of a straight chain aliphatic hydrocarbon of from about 3 to about 16 carbon atoms, branched chain aliphatic hydrocarbon of from about 3 to about 16 carbon atoms and combinations thereof.

Claim 44

Dependent Claim 34 words

The method of claim 38 wherein said auxiliary organic is selected from the group consisting of benzene, alkyl-substituted benzene, alkyl-substituted adamantane and combinations thereof, alkyl being of from 1 to about 14 carbon atoms.

Claim 45

Dependent Claim 23 words

The method of claim 38 wherein said auxiliary organic is selected from the group consisting of p-xylene, trimethylbenzene, triethylbenzene, dimethyladamantane and combinations thereof.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1994-10-14	1995-04-15	1995-10-15	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1998-10-14	1999-04-15	1999-10-15	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	2002-10-14	2003-04-15	2003-10-15	$7700.00	Window Closed / Lapsed

Method for synthesizing mesoporous crystalline material

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