TS-PQ titano-silicate molecular sieves and methods for synthesis and use thereof
OwnerErnest Senderov, Richard J. Hinchey +1inventors
InventorsErnest Senderov, Richard J. Hinchey, Istvan Halasz
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Abstract
The present invention is directed towards methods for the cost-effective commercial manufacture of small crystal titanium-silicate molecular sieve products, toward a novel titano-silicate molecular sieve composition synthesized thereby, which the present inventors have termed “TS-PQ”, and toward uses of that molecular sieve composition as an oxidation catalyst.
Claims69
A method for preparing a titano-silicate molecular sieve, comprising the steps of:
- a) reacting a silica source with an aqueous, alkaline solution of an organic structure directing agent under conditions sufficient to activate the silica source forming silica species in an activated silica solution, wherein the silica species are more reactive than the silica source;
- b) combining the activated silica solution with a titanium source under conditions sufficient to form titanium-silicate oligomeric species in a titanium-silicate solution;
- c) pretreating the titanium-silicate solution by aging the titanium-silicate solution under conditions sufficient to promote formation of nuclei or nuclear precursor species;
- d) crystallizing the titanium-silicate solution under conditions sufficient to produce titanium-silicate crystals in a liquid phase;
- e) separating the titanium-silicate crystals from the liquid phase;
- f) washing the titanium-silicate crystals;
- g) drying the titanium-silicate crystals after step f);
- and
- h) calcining the titanium-silicate crystals to provide the titanium-silicate molecular sieve.
A method for preparing a titanium-silicate molecular sieve, comprising the steps of.
- a) combining a titania-silica co-gel with an aqueous, alkaline solution of an organic structure directing agent under conditions sufficient to form titanium-silicate oligomeric species in a titanium-silicate solution;
- b) pretreating the titanium-silicate solution by aging the titanium-silicate solution under conditions sufficient to promote formation of nuclei or nuclear precursor species;
- c) crystallizing the titanium-silicate solution under conditions sufficient to produce titanium-silicate crystals in a liquid phase;
- d) separating the titanium-silicate crystals from the liquid phase;
- e) washing the titanium-silicate crystals;
- f) drying the titanium-silicate crystals after step e);
- and
- g) calcining the titanium-silicate crystals to provide the titanium-silicate molecular sieve.
A method for preparing a titanium-silicate molecular sieve, comprising the steps of:
- a) combining a reactive silica source, a titanium source, and a Ti-complexing agent under conditions sufficient to form titanium-silicate oligomeric species in a titanium-silicate solution;
- b) pretreating the titanium-silicate solution by aging the titanium-silicate solution under conditions sufficient to promote formation of nuclei or nuclear precursor species;
- c) crystallizing the titanium-silicate solution under conditions sufficient to produce titanium-silicate crystals in a liquid phase;
- d) separating the titanium-silicate crystals from the liquid phase;
- e) washing the titanium-silicate crystals;
- f) drying the titanium-silicate crystals after step e);
- and
- g) calcining the titanium-silicate crystals to provide the titanium-silicate molecular sieve.
A method for preparing a titanium-silicate molecular sieve, comprising the steps of,
- a) combining a reactive silica source and a titanium source under conditions sufficient to form titanium-silicate oligomeric species in a titanium-silicate solution;
- b) pretreating the titanium-silicate solution by aging the titanium-silicate solution under conditions sufficient to promote formation of nuclei or nuclear precursor species;
- c) crystallizing the titanium-silicate solution under conditions sufficient to produce titanium-silicate crystals in a liquid phase;
- d) separating the titanium-silicate crystals from the liquid phase;
- e) washing the titanium-silicate crystals with an acidic wash solution;
- f) drying the titanium-silicate crystals after step e);
- and
- g) calcining the titanium-silicate crystals to provide the titanium-silicate molecular sieve.
A method for preparing a titanium-silicate molecular sieve, comprising the steps of,
- h) combining a reactive silica source and a titanium source under conditions sufficient to form titanium-silicate oligomeric species in a titanium-silicate solution;
- i) pretreating the titanium-silicate solution by aging the titanium-silicate solution under conditions sufficient to promote formation of nuclei or nuclear precursor species;
- j) crystallizing the titanium-silicate solution under conditions sufficient to produce titanium-silicate crystals in a liquid phase;
- k) separating the titanium-silicate crystals from the liquid phase;
- l) steaming the titanium-silicate crystals;
- m) drying the titanium-silicate crystals after step e);
- and
- n) calcining the titanium-silicate crystals to provide the titanium-silicate molecular sieve.
A method of oxyfunctionalizing an organic material comprising the steps of,
- a) contacting the organic material with an oxidizer selected from the group of molecular oxygen, aqueous H2O2, peroxides, and alkylhydroperoxides, in contact with TS-PQ titano-silicate molecular sieve, characterized by predominance of 220 nm bant on its UV-VIS DR spectra, at temperatures from about 40° C. to about 60° C., for a period of time sufficient to convert a substantial amount of the organic material into an oxyfunctionalized organic material;
- and
- b) recovering the oxyfunctionalized organic material as a product.
A titano-silicate molecular sieve characterized by strong band on UV-VIS DRV spectra at 200-210 nm and/or at 215-300 nm area with absence or less intensive band in 240-300 nm area and above 300 nm.
Dependencies are inferred from the claim text.