# US 5,346,685 A · Synthetic porous crystalline MCM-51, its synthesis and use

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- Number: US 5,346,685 A
- Document ID: US5346685A
- Status: Granted
- Kind: A
- Application number: 08/051,714
- Filed: 1993-04-23
- Granted: 1994-09-13
- Earliest claimed: 1993-04-23
- Assignees: Mobil Oil Corporation
- Inventors: Ahmad Moini
- Web page: https://patentgrep.com/patent/US5346685A

## CPC

- B01J 29/03: not having base-exchange properties {(B01J29/005 takes precedence)}
- C01B 37/002: {Metallophosphates not containing aluminium, e.g. gallophosphates or silicogallophosphates}
- Y10S 423/30: Alpo and sapo
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- Y10S: TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS

## Abstract

This invention relates to a new synthetic porous crystalline titanium phosphate material, a method for its preparation and use thereof in catalytic conversion of organic compounds. The new crystalline material exhibits a distinctive X-ray diffraction pattern.

## Claims

### Claim 1

A synthetic porous crystalline material characterized by an X-ray diffraction pattern including values substantially as set forth in Table I of the specification and having a composition in terms of TiO.sub.2 and P.sub.2 O.sub.5 comprising the molar relationship:
TiO.sub.2 :(0.5.+-.0.1)P.sub.2 O.sub.5.

### Claim 2 (depends on 1)

The crystalline material of claim 1 having a composition expressed by the molar relationship:
TiO.sub.2 :(0.5.+-.0.1)P.sub.2 O.sub.5 :xH.sub.2 O:yR,
wherein x is from 0 to about 0.1, y is from 0 to about 0.1, and R is an organic moiety.

### Claim 3 (depends on 2)

The crystalline material of claim 2 wherein said R is selected from the group consisting of quaternary alkylammonium ions, alkyl comprising from 2 to 4 carbon atoms, and mixtures thereof.

### Claim 4 (depends on 1)

The crystalline material of claim 1 which has a surface area of greater than about 50 m.sup.2 /g.

### Claim 5 (depends on 1)

The crystalline material of claim 1 which exhibits Equilibrium Adsorption values of greater than about 4.0 wt. % for water vapor, greater than about 3.5 wt. % for cyclohexane vapor, and greater than about 3.5 wt. % for n-hexane vapor.

### Claim 6 (depends on 1)

A composition comprising the crystalline material of claim 1 and a matrix.

### Claim 7 (depends on 6)

The composition of claim 6 wherein said matrix comprises alumina, silica, zirconia, titania, magnesia, beryllia or a combination thereof.

### Claim 8

A synthetic porous crystalline material having an X-ray diffraction pattern substantially as shown in FIG. 1 and having a composition in terms of TiO.sub.2 and P.sub.2 O.sub.5 comprising the molar relationship
TiO.sub.2 :(0.5.+-.0.1)P.sub.2 O.sub.5.

### Claim 9 (depends on 1)

A mixture capable of forming the synthetic porous crystalline material of claim 1 upon crystallization, said mixture comprising sources of titanium, phosphorus, directing agent R and solvent, and having a composition, in terms of mole ratios, within the following ranges:
______________________________________ P/Ti 2 to 30 solvent/Ti 20 to 150 R/Ti 0.2 to 10 ______________________________________
wherein R is an organic moiety selected from the group consisting of quaternary alkylammonium ions, alkyl comprising from 2 to 4 carbon atoms, and mixtures thereof.

### Claim 10 (depends on 9)

The mixture of claim 9 wherein solvent is selected from the group consisting of C.sub.1 -C.sub.6 alcohols, C.sub.1 -C.sub.6 diols, water and mixtures thereof.

### Claim 11 (depends on 1)

A method for synthesizing the porous crystalline material of claim 1 which comprises (1) mixing a source of titanium with solvent; (2) hydrolyzing the mixture of step (1) to form titanium oxide gel; (3) mixing the titanium oxide gel product of step (2) with sources of phosphorus and directing agent R to form a mixture having a composition, in terms of mole ratios, within the following ranges:
______________________________________ P/Ti 2 to 30 solvent/Ti 20 to 150 R/Ti 0.2 to 10 ______________________________________
wherein R is an organic moiety selected from the group consisting of quaternary alkylammonium ions, alkyl comprising from 2 to 4 carbon atoms, and mixtures thereof; (4) maintaining said mixture under sufficient conditions until crystals of said material are formed; and (5) recovering said crystalline material from step (4).

### Claim 12 (depends on 11)

The method of claim 11 wherein said mixture has the following composition ranges:
______________________________________ P/Ti 10 to 20 solvent/Ti 70 to 110 R/Ti 3.0 to 7.0. ______________________________________

### Claim 13 (depends on 11)

The method of claim 11 wherein said source of titanium is selected from the group consisting of titanium oxide, titanium ethoxide, titanium isopropoxide, titanium propoxide, titanium diisopropoxide bis (2,4-pentanedionate), and combinations thereof.

### Claim 14 (depends on 11)

The method of claim 11 wherein said source of phosphorus is selected from the group consisting of phosphoric acid, triethylphosphate, and combination thereof.

### Claim 15 (depends on 11)

The method of claim 11 wherein said solvent is selected from the group consisting of C.sub.1 -C.sub.6 alcohols, C.sub.1 -C.sub.6 diols, water, and mixtures thereof.

### Claim 16 (depends on 11)

The method of claim 11 wherein the concentration of R in the mixture of step (3) is within the range of from about 0.2M to about 2.0M.

### Claim 17 (depends on 12)

The method of claim 12 wherein the concentration of R in the mixture of step (3) is within the range of from about 0.2M to about 2.0M.