Catalyst – solid sorbent – or support therefor: product or process – Catalyst or precursor therefor – Organic compound containing
Patent
1998-09-24
2000-08-22
Wood, Elizabeth
Catalyst, solid sorbent, or support therefor: product or process
Catalyst or precursor therefor
Organic compound containing
502402, 521 21, 521 28, B01J 3108
Patent
active
061072338
DESCRIPTION:
BRIEF SUMMARY
BACKGROUND OF THE INVENTION
The present invention relates to a process for preparing a spherically shaped microcomposite comprising a perfluorinated ion-exchange polymer containing pendant sulfonic acid groups and/or pendant carboxylic acid groups entrapped within and highly dispersed throughout an inorganic oxide network. Due to their high surface area and acid functionality, these spherically shaped microcomposites possess wide utility as improved solid acid catalysts.
A microcomposite comprising perfluorinated ion-exchange polymers containing pendant sulfonic acid groups and/or pendant carboxylic acid groups entrapped within and highly dispersed throughout a metal oxide network and its preparation are disclosed in W095/19222. The microcomposites described therein are irregular shaped particles which can be subject to attrition. Attrition can lead to fines which can cause problems in certain filtering processes and columns, such as clogging, pressure build up and the generation of friction. Fines can also find their way into a final product in certain applications which is undesirable.
Canadian Patent Application No. 2,103,653 describes shaped organosiloxane polycondensates in the form of macroscopic spherical particles. The polycondensates described contain no perfluorinated ion exchange polymer.
It is an object of the present invention to provide a shaped microcomposite that possesses high catalytic activity, high attrition resistance, and better handling characteristics.
SUMMARY OF THE INVENTION
The present invention provides a process for the preparation of at least one spherically shaped porous microcomposite which comprises a perfluorinated ion-exchange polymer containing pendant sulfonic and/or carboxylic acid groups entrapped within and highly dispersed throughout a network of inorganic oxide, wherein the weight percentage of the perfluorinated ion-exchange polymer in the microcomposite is from about 0.1 to about 90 percent, and wherein the size of the pores in the microcomposite is about 0.5 nm to about 75 nm; said process comprising the steps of: water-miscible liquid composition comprising a perfluorinated ion-exchange polymer containing pendant sulfonic and/or carboxylic acid groups, and an organic liquid to form a two phase liquid system; dispersion of the water-miscible phase in the shape of spheres in the organic phase; of inorganic oxide to yield at least one spherically shaped porous microcomposite having the above-described properties; and
DETAILED DESCRIPTION
This invention is directed to a process for preparing at least one spherically shaped porous microcomposite having a diameter of about 0.1 to about 1.0 mm, a specific surface area of about 10 to about 800 m.sup.2 /g, and a specific pore volume of about 0.2 to about 3.0 cc/g. The at least one spherically shaped microcomposite comprises a perfluorinated ion-exchange polymer containing pendant sulfonic and/or carboxylic acid groups entrapped within and highly dispersed throughout a network of inorganic oxide, wherein the weight percentage of the perfluorinated ion-exchange polymer in the microcomposite is from about 0.1 to about 90 percent. The size of the pores in the microcomposite is about 0.5 nm to about 75 nm. Preferably, the pore size is about 0.5 to about 50 nm, most preferably about 0.5 to about 30 nm.
In step (a) of the process of the present invention, a water-miscible inorganic oxide network precursor system is combined with a water-miscible liquid composition comprising a perfluorinated ion-exchange polymer containing pendant sulfonic and/or carboxylic acid groups, and an organic liquid to form a two phase liquid system. Although the sequence of combining the components of the two phase liquid system is not critical preferably the water-miscible components are contacted with each other first followed by contact with the organic liquid.
The water-miscible inorganic oxide network precursor system comprises an inorganic oxide network precursor, water and optionally a catalyst.
The "inorganic oxide" signifies metallic,
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Harmer Mark Andrew
Sun Qun
E. I. Du Pont de Nemours and Company
Wood Elizabeth
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