Catalyst – solid sorbent – or support therefor: product or process – Catalyst or precursor therefor – Organic compound containing
Reexamination Certificate
1999-07-02
2001-06-19
Bell, Mark L. (Department: 1755)
Catalyst, solid sorbent, or support therefor: product or process
Catalyst or precursor therefor
Organic compound containing
C502S401000, C502S407000, C556S410000, C556S431000, C556S434000
Reexamination Certificate
active
06248686
ABSTRACT:
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to porous materials that can be used as adsorption materials for concentration of organic substances and/or separation of undesired substances, and as catalyst materials for selective catalytic reactions. The porous materials comprise organic groups integrated into the inorganic porous structure.
2. Description of the Related Art
Known mesoporous molecular sieves (hereinafter, referred to as mesoporous materials) consist of an inorganic oxide porous substance and have a pore diameter of 1.5 to 30 nm, which is larger than known zeolite pore diameters. The pore size distribution is generally uniform and the pores are regularly arranged. The pore structure of such mesoporous materials is large enough to absorb large molecules and the pore wall structure can be as thin as about 1 nm. Further, such mesoporous materials are known to have large specific surface areas (about 1000 m
2
/g) and large pore volumes (about 1 cc/g). For these reasons, such the mesoporous materials enable reactive catalysts, adsorbents composed of a functional organic compound and other molecules to rapidly diffuse into the pores and are therefore, advantageous over zeolites, which have smaller pore sizes. Consequently, such mesoporous materials have been used in high-speed catalytic reactions that require fast reactions and as large capacity adsorbents, which are capable of adsorbing a large amount of an adsorbing material.
Examples of such mesoporous materials are FSM-16 (T. Yanagisawa et al., Bull. Chem. Soc., Jpn., 63,988 (1990), S. Inagaki et al., J. Chem. Soc., Chem. Commun., 680 (1993)) and the M41Ss (e.g., MCM-41, MCM-48) (C. T. Kresge et al., Nature, 359,710 (1992), J. S. Beck et al., J. Am. Chem. Soc., 114, 10834 (1992)).
PCT publication No. WO9834723 describes trials that were conducted in which an organic group was attached onto the surface of an inorganic skeleton of these mesoporous materials, namely onto the inner surface of a pore, so as to impart a selective adsorption ability and specific catalyst function to the mesoporous substance. Another trial was conducted in which organic groups were introduced during the synthesis the mesoporous material. Such mesoporous materials were formed with organic groups bound as side chains to the base skeleton made of the inorganic material. Specifically, the organic groups were suspended from the surface of the base skeleton made of the inorganic material. Consequently, the pore wall was basically composed of a skeleton made of inorganic materials and the organic groups project from the surface of the pore wall to form a layer composed of the organic groups.
In such a structure, the surface characteristics of the porous material may be determined by the characteristics of the organic groups. As a result, such porous materials were restricted to adsorbing substances to which the organic groups have affinities. Further, catalytic function or adsorption function derived from the inorganic skeleton can be masked, because the catalytic active sites or adsorption sites in the inorganic skeleton are covered by the organic groups.
The thickness of the pore wall also may increase corresponding to the introduction of the organic group, and substantial decreases in pore diameter and pore volume may result. Further, such organic groups may release under high temperatures or in a catalytic reaction and adsorption reaction, thus leading to the loss of desirable surface properties and the contamination of the treated material by the released organic group.
SUMMARY OF THE INVENTION
Therefore, one object of the present teachings is to provide improved mesoporous materials that contain one or more organic groups integral to the structure of the mesoporous materials.
Preferably, complex porous materials are taught that comprise a skeleton of the porous material containing at least two metal atoms, at least one oxygen atom and at least one organic group. Naturally, the organic group contains at least one carbon atom. The metal atoms, oxygen atoms and organic groups may be bound by ionic bonds and/or covalent bonds. More preferably, the organic group is covalently bound to at least two metal atoms. Most preferably, the oxygen atom is bound to at least one metal atom.
In such a porous material, the organic group is integrated into at least a part of the porous skeleton and the base skeleton itself has a hybrid composition composed of organic and inorganic materials. As a result, a porous material can be synthesized having a novel organic/inorganic structure, because the organic group is integrally bound with in the skeleton by at least two metal atoms. Consequently, the organic group forms a part of the skeleton and porous materials are taught in which the organic group is held within the porous material in a stable manner.
One advantage of such a porous material is that the pore walls exhibit properties of the organic group without utilizing a surface organic layer. Further, the introduction of the organic group into the porous material does not substantially reduce the pore diameter and pore volume, as is the case for porous materials formed with a surface organic layer.
Preferably, 60% or more of the total pore volume in the porous material has a pore diameter in a range of ±40% of the pore diameter revealing the maximum peak in a pore size distribution curve or at least one peak is present at a diffraction angle that preferably corresponds to a d value of at least 1 nm in an x-ray diffraction pattern. When the pore volume distribution is in this range or at least one peak is present at a specific diffraction angle in the x-ray diffraction (XRD) pattern, the porous material functions as a useful molecular sieve and may be an excellent adsorbent and/or catalyst material.
Methods for producing such porous materials are also taught. Preferably, such porous materials are synthesized using a polycondensation reaction of an organometallic compound having at least one organic group bound to at least two metal atoms. Preferably, at least one hydrolysis group also is bound to the metal atom of the organometallic compound. Further, the polycondensation reaction is preferably performed in the presence of a surfactant. If such an organometallic compound is polycondensed using the surfactant as a template, a porous material can be obtained as a polycondensate having a metal atom-organic group bond in a main chain, because the organometallic compound contains the metal atom-organic group bond.
Other objects, features and advantages of the present invention will be readily understood by a person of skill in the art after reading the following detailed description together with the drawings and claims.
REFERENCES:
patent: 5599759 (1997-02-01), Inagaki et al.
patent: 5869724 (1999-02-01), Kirkland et al.
patent: WO 98/34723 (1998-08-01), None
Fukushima Yoshiaki
Guan Shiyou
Inagaki Shinji
Bell Mark L.
DiVerdi Michael J.
Kabushiki Kaisha Toyota Chuo Kenkyusho
Oblon & Spivak, McClelland, Maier & Neustadt P.C.
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