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EP0311983A2 Expired / Lapsed EP ⏱️ 0.0 years remaining

Method for the preparation of titanium-silicalites

Assignee: Enichem Anic SpA
•
Filing: 1988-10-11
•
Granted: —
•
Expires: 2008-10-11
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Abstract

Abstract The invention concerns a method for the preparation of titanium-silicalites, in the presence of a templating agent, characterized in that a preformed TiO₂-SiO₂ coprecipitate is impregnated with an aqueous solution of said templating agent and in that the thus impregnated material is made to acquire the zeolitic structure of the titanium-silicalites by means of a hydrothermal synthesis.

Inventors

  • 👤 Mario Padovan
  • 👤 Guiseppe Leofanti
  • 👤 Paolo Dr. Roffia

Bibliographic Details

Application Number —
Jurisdiction EP
Data Source google_patents
Last Synchronized 2026-11-03 21:04
CPC Classifications
C; C07; C07C; C07C249/00; C07C249/04; B; B01; B01J; B01J29/00; B01J29/89; C01; C01B; C01B37/00; C01B37/005

Claims Analysis

Total Claims: 17
Claim 1
Independent Claim 68 words
A method for the preparation of titanium-­silicalites in the presence of a templating agent, characterized in that a co-precipitated TiO₂-SiO₂ material, amorphous or having a crystalline structure, containing titanium, silicon and oxygen ina combined form, is impregnated with an aqueous solution of said templating agent and in that the thus impregnated material is made to acquire the zeolitic structure of the titanium-­silicalites by means of a hydrothermal synthesis.
Claim 2
Independent Claim 68 words
A method for the preparation of titanium-­silicalites in the presence of a templating agent, characterized in that a co-precipitated TiO₂-SiO₂ material, amorphous or having a crystalline structure, containing titanium, silicon and oxygen ina combined form, is impregnated with an aqueous solution of said templating agent and in that the thus impregnated material is made to acquire the zeolitic structure of the titanium-­silicalites by means of a hydrothermal synthesis.
Claim 3
Dependent Claim 12 words
A method according to claim 1, wherein said co-­precipitated material is amorphous.
Claim 4
Dependent Claim 28 words
A method according to claim 1 or 2, wherein the pore volume of the co-precipitate is higher than 0.5 cm³/g, the surface area being higher than 200 m²/g.
Claim 5
Independent Claim 28 words
A method according to anyone of the preceding claims, wherein the SiO₂:TiO₂ molar ratio, in said co-­precipitate, ranges from 20 to 200 and preferably from 30 to 80.
Claim 6
Independent Claim 19 words
A method according to anyone of the preceding claims, wherein said co-precipitate is impregnated according to the dry-impregnation technology.
Claim 7
Independent Claim 31 words
A method according to anyone of the preceding claims, wherein the titanium-silicalite undergoes, before being used, an activating washing, based on hydrogen peroxide, optionally in the presence of an inorganic acid.
Claim 8
Independent Claim 21 words
A method according to anyone of the preceding claims, wherein said templating agent is selected from tetra­propyl-ammonium hydroxide and tetrapropylammonium bromide.
Claim 9
Dependent Claim 57 words
A method according to claim 7, characterized by the following molar ratios (in the material undergoing the hydrothermal synthesis): SiO₂/TiO₂ = from 20 to 200 OH⁻/SiO₂ = from 0.03 to 0.20 H₂O/SiO₂ = from 0.10 to 10 R₄N⁺/SiO₂ = from 0.03 to 0.20 wherein R₄N⁺ is the nitrogen containing organic cation corresponding to the templating agent used.
Claim 10
Dependent Claim 35 words
A method according to claim 8, characterized by the following ratio: SiO₂/TiO₂ = from 30 to 80 OH⁻/SiO₂ = from 0.05 to 10 H₂O/SiO₂ = from 0.50 to 4 R₄N⁺/SiO₂ = from 0.05 to 0.10
Claim 11
Dependent Claim 24 words
Use of the product prepared according to the method described in anyone of the preceding claims, for the oxidation of propylene to propylene oxide.
Claim 12
Dependent Claim 29 words
Use of the product prepared according to the method described in anyone of the claims 1 to 9 for the ammoximation in the liquid phase of a carbonylic compound.
Claim 13
Dependent Claim 11 words
Use according to claim 11, wherein said carbonylic compound is cyclohexanone.
Claim 14
Dependent Claim 25 words
Use according to claim 12, wherein said cyclohexanone is fed to the ammoximation zone in the form of a mixture with cyclohexanol and hydrogen peroxide.
Claim 15
Dependent Claim 20 words
Use according to claim 13, wherein said mixture comes from a partial oxidation in the liquid phase (autooxidation) of cyclohexanol.
Claim 16
Dependent Claim 55 words
Titanium-silicalites, obtainable according to the method described in anyone of the claims form 1 to 9, consisting of particles having an average size ranging from 0.2 to 0.5 micrometers, in which the Ti:(Ti+Si) molar ratio ranges from 0.0120 to 0.0190 and in which the volume of the intercrystalline cavities ranges from 0.170 to 0.185 cm³/g.
Claim 17
Dependent Claim 21 words
Titanium silicalites according to claim 15, showing the X ray diffractogram of figure 1 and/or the I.R. spectrum of figure 2.

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