# US 5,350,722 A · MTW-type zeolite and its preparation process

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- Number: US 5,350,722 A
- Document ID: US5350722A
- Status: Granted
- Kind: A
- Application number: 07/920,487
- Filed: 1992-08-20
- Granted: 1994-09-27
- Earliest claimed: 1990-12-21
- Assignees: Institut Francias du Petrole
- Inventors: Jean-Francois Joly; Philippe Caullet; Anne-Catherine Faust; Jacques Baron; Jean-Louis Guth
- Web page: https://patentgrep.com/patent/US5350722A

## CPC

- B01J 29/7034: {MTW-type, e.g. ZSM-12, NU-13, TPZ-12 or Theta-3}
- C01B 39/42: Type ZSM-12
- B01J 2229/26: to stabilize the total catalyst structure
- B01J 2229/42: Addition of matrix or binder particles
- Y10S 423/33: MTW, e.g. ZSM-12, NU-13, CZH-5, TPZ-3
- 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

The invention relates to a synthetic crystalline zeolite of the MTW type, characterized by: a) the following approximate general formula: M.sub.2/n O, Al.sub.2 O.sub.3, xSiO.sub.2 in which M represents a metal cation and/or proton, n is the valency of M and x is a number between 14 and 800, b) a X-ray diagram shown in table I of the description, c) a fluorine content between approximately 0.005 and 2% by weight, said zeolite having been synthesized in a fluoride medium and accompanied by stirring.

## Claims

### Claim 1

Synthetic crystalline zeolite of the MTW type characterized by:
a) the following approximate general formula:
M.sub.2/n O, Al.sub.2 O.sub.3, xSiO.sub.2
in which M represents a metal cation and/or a proton, n is the valency of M and x is a number between 14 and 800,
b) a X-ray diagram shown in table I of the description,
c) a fluorine content between approximately 0.005 and 2% by weight, said zeolite having been synthesized in a fluoride medium, accompanied by stirring.

### Claim 2 (depends on 1)

Zeolite according to claim 1, characterized in that x is a number between 20 and 800.

### Claim 3 (depends on 1, 2)

Zeolite according to either of the claims 1 and 2, characterized in that it has a fluorine content between approximately 0.01 and 1.5% by weight.

### Claim 4 (depends on 1)

Catalyst containing a zeolite according to claim 1 wherein said catalyst further comprises a matrix.

### Claim 5 (depends on 1)

Catalyst containing a zeolite according to claim 1 wherein said catalyst further comprises a matrix at least one metal and/or metal compound chosen from among groups IA, VIB and VIII of the periodic classification of elements.

### Claim 6 (depends on 1)

Process for the preparation of a zeolite according to claim 1, characterized in that:
a) a reaction mixture in solution is formed having a pH below approximately 9 and containing water, at least one silica source, at least one aluminium source, at least one mobilizing agent source containing fluoride ions (F.sup.-), at least one source of at least one structuring agent chosen from within the group formed by 1,4-diazabicyclo-(2,2,2)-octane and a mixture of 1,4-diazabicyclo-(2,2,2)-octane and methyl amine, said structuring agent optionally supplying organic cations, said reaction mixture having a composition, in molar ratio terms, within the following value ranges:
Si/Al: 6-300,
F.sup.- /Si: 0.1-8,
H.sub.2 O/Si: 4-50,
(R+R')/Si: 0.5-4,
R/R': 0.1-infinity, in which R is 1,4-diazabicyclo-(2,2,2)-octane and R' is methyl amine.
b) the said reaction mixture is maintained under stirring at a heating temperature between approximately 100.degree. and 250.degree. C. until a crystalline compound is obtained and
c) said compound is calcined at a temperature above approximately 350.degree. C.

### Claim 7 (depends on 6)

Process according to claim 6, wherein, in stage a), the reaction mixture has a composition, in molar ratio terms, within the following value ranges:
Si/Al:10-300,
F.sup.- /Si:0.2-6,
H.sub.2 O/Si:10-50,
(R+R')/Si:0.5-4,
R/R':0.2-infinity, in which R is 1,4-diazabicyclo-(2,2,2)-octane and R' is methyl amine.

### Claim 8 (depends on 6)

Process according to claim 6, wherein, in stage a), said reaction mixture has a composition, in molar ratio terms, within the following value ranges:
Si/Al:12-100
F.sup.- /Si:0.5-4,
H.sub.2 O/Si:20-40,
(R+R')/Si:0.9-2.1,
R/R':0.3-infinity in which R is 1,4-diazabicyclo-(2,2,2)-octane and R' is methyl amine.

### Claim 9 (depends on 6, 7, 8)

Process according to any one of the claims 6 to 8, wherein, in stage a), said reaction mixture also incorporates an alkali metal and/or alkaline earth cation source.

### Claim 10 (depends on 9)

Process according to claim 9, wherein, in stage b), said reaction mixture is maintained at a heating temperature between approximately 150.degree. and 250.degree. C., the reaction mixture being kept under stirring until a crystalline compound is obtained.