Synthetic porous crystalline MCM-71, its synthesis and use

Chemistry of inorganic compounds – Zeolite – Structure defined x-ray diffraction pattern

Reexamination Certificate

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C423S705000, C208S046000

Reexamination Certificate

active

06676922

ABSTRACT:

FIELD OF THE INVENTION
This invention relates to a novel synthetic porous crystalline material, MCM-71, to a method for its preparation and to its use in catalytic conversion of organic compounds.
BACKGROUND OF THE INVENTION
Zeolitic materials, both natural and synthetic, have been demonstrated in the past to have catalytic properties for various types of hydrocarbon conversion. Certain zeolitic materials are ordered, porous crystalline aluminosilicates having a definite crystalline structure as determined by X-ray diffraction, within which there are a large number of smaller cavities which may be interconnected by a number of still smaller channels or pores. These cavities and pores are uniform in size within a specific zeolitic material. Since the dimensions of these pores are such as to accept for adsorption molecules of certain dimensions while rejecting those of larger dimensions, these materials have come to be known as “molecular sieves” and are utilized in a variety of ways to take advantage of these properties.
Such molecular sieves, both natural and synthetic, include a wide variety of positive ion-containing crystalline silicates. These silicates can be described as a rigid three-dimensional framework of SiO
4
and Periodic Table Group IIIA element oxide, e.g., AlO
4
, in which the tetrahedra are cross-linked by the sharing of oxygen atoms whereby the ratio of the total Group IIIA element, e.g., aluminum, and silicon atoms to oxygen atoms is 1:2. The electrovalence of the tetrahedra containing the Group IIIA element, e.g., aluminum, is balanced by the inclusion in the crystal of a cation, for example an alkali metal or an alkaline earth metal cation. This can be expressed wherein the ratio of the Group IIIA element, e.g., aluminum, to the number of various cations, such as Ca/2, Sr/2, Na, K or Li, is equal to unity. One type of cation may be exchanged either entirely or partially with another type of cation utilizing ion exchange techniques in a conventional manner. By means of such cation exchange, it has been possible to vary the properties of a given silicate by suitable selection of the cation. The spaces between the tetrahedra are occupied by molecules of water prior to dehydration.
Prior art techniques have resulted in the formation of a great variety of synthetic zeolites. Many of these zeolites have come to be designated by letter or other convenient symbols, as illustrated by zeolite A (U.S. Pat. No. 2,882,243); zeolite X (U.S. Pat. No. 2,882,244); zeolite Y (U.S. Pat. No. 3,130,007); zeolite ZK-5 (U.S. Pat. No. 3,247,195); zeolite ZK-4 (U.S. Pat. No. 3,314,752); zeolite ZSM-5 (U.S. Pat. No. 3,702,886); zeolite ZSM-11 (U.S. Pat. No. 3,709,979); zeolite ZSM-12 (U.S. Pat. No. 3,832,449), zeolite ZSM-20 (U.S. Pat. No. 3,972,983); ZSM-35 (U.S. Pat. No. 4,016,245); zeolite ZSM-23 (U.S. Pat. No. 4,076,842); zeolite MCM-22 (U.S. Pat. No. 4,954,325); and zeolite MCM-35 (U.S. Pat. No. 4,981,663), merely to name a few.
The SiO
2
/Al
2
O
3
ratio of a given zeolite is often variable. For example, zeolite X can be synthesized with SiO
2
/Al
2
O
3
ratios of from 2 to 3; zeolite Y, from 3 to about 6. In some zeolites, the upper limit of the SiO
2
/Al
2
O
3
ratio is unbounded. ZSM-5 is one such example wherein the SiO
2
/Al
2
O
3
ratio is at least 5 and up to the limits of present analytical measurement techniques. U.S. Pat. No. 3,941,871 (Re. 29,948) discloses a porous crystalline silicate made from a reaction mixture containing no deliberately added alumina in the starting mixture and exhibiting the X-ray diffraction pattern characteristic of ZSM-5. U.S. Pat. Nos. 4,061,724; 4,073,865 and 4,104,294 describe crystalline silicates of varying alumina and metal content.
Many zeolites are synthesized in the presence of an organic directing agent, such as an organic nitrogen compound. For example, ZSM-5 may be synthesized in the presence of tetrapropylammonium cations and zeolite MCM-22 may be synthesized in the presence of hexamethyleneimine. It is also possible to synthesize zeolites and related molecular sieves in the presence of rigid polycyclic quaternary directing agents (see, for example U.S. Pat. Nos. 5,501,848 and 5,225,179), flexible diquaternary directing agents (Zeolites, [1994], 14, 504) and rigid polycyclic diquaternary directing agents (JACS, [1992], 114, 4195).
SUMMARY OF THE INVENTION
The present invention is directed to a novel porous crystalline material, named MCM-71, a method for its preparation, and the conversion of organic compounds contacted with an active form thereof. The calcined form of the porous crystalline material of this invention possesses a very high acid activity and exhibits a high sorption capacity. MCM-71 is reproducibly synthesized by the present method in high purity.


REFERENCES:
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patent: 5013536 (1991-05-01), Vaughan et al.
patent: 5164170 (1992-11-01), Rubin
patent: 5397560 (1995-03-01), Millar et al.
patent: 5463160 (1995-10-01), Kuhlmann et al.
patent: 5510560 (1996-04-01), O'Young et al.
patent: 5882624 (1999-03-01), Kuznicki et al.
patent: 6049018 (2000-04-01), Calabro et al.
patent: WO 02/42207 (2002-05-01), None

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