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US4410501A Expired / Lapsed US ⏱️ 0.0 years remaining

Preparation of porous crystalline synthetic material comprised of silicon and titanium oxides

Assignee: SnamProgetti SpA
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Filing: 1982-06-29
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Granted: 1983-10-18
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Expires: 2002-06-29
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Abstract

Abstract This invention relates to a porous crystalline synthetic material constituted by silicon and titanium oxides, a method for synthesizing said material, and the use thereof as a catalyst. Said material is given the name titanium silicalite or TS-1, and corresponds to the following formula: xTiO2.(1-x)SiO2 where x lies between 0.0005 and 0.04, preferably between 0.01 and 0.025. The material is prepared starting from a mixture constituted by a source of silicon oxide and a source of titanium oxide. The reaction takes place in the aqueous phase at a temperature of 130 DEG to 200 DEG C., and the solid product obtained is calcined in air at 550 DEG C. The TS-1 can be used for alkylation of toluene with methanol, or benzene with ethylene or ethanol, disproportioning of toluene to produce paraxylol, for cracking, hydrocracking, isomerization of n-paraffins and naphthenes, reforming, isomerization of substituted polyalkyl aromatics, disproportioning of aromatics, conversion of dimethylether and/or methanol or other alcohols to hydrocarbons, polymerization of compounds containing olefine or acetylene bonds, conversion of aliphatic carbonyl compounds into at least partly aromatic hydrocarbons, separation of ethyl benzene from other C8 aromatic hydrocarbons, hydrogenation and dehydrogenation of hydrocarbons, methanation, oxidation, dehydration of aliphatic compounds containing oxygen, and conversion of olefines into compounds of high octane number.

Inventors

  • 👤 Marco Taramasso
  • 👤 Giovanni Perego
  • 👤 Bruno Notari

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 13:59
CPC Classifications
C; C01; C01B; C01B37/00; C01B37/005; B; B01; B01J; B01J29/00; B01J29/89; C01B39/00; C01B39/02; C01B39/06; C01B39/12; Y; Y10; Y10S; Y10S423/00; Y10S423/22

Claims Analysis

Total Claims: 8
Claim 1
Independent Claim 221 words
The method of preparing a porous, crystalline material comprised of silicon oxide and titanium oxide wherein the ratio of said oxides is represented by the formula xTiO.sub.2.(1-x)SiO.sub.2 in which x is a number between 0.0005 and 0.04, which comprises the steps of: (1) preparing an aqueous mixture of starting reagents free from alkali- and alkaline-earth metals including a source of silicon oxide selected from the group consisting of silica gel and tetraalkylorthosilicates, a source of titanium oxide consisting of a hydrolysable titanium compound, and a nitrogenated organic base, and wherein the starting reagents have the following molar ratios: SiO 2 /TiO 2 from 5 to 200, OH - /SiO 2 from 0.1 to 1.0, H 2 O/SiO 2 from 20 to 200, RN + /SiO 2 from 0.1 to 2.0 wherein RN + is the cation of the nitrogenated organic base, (2) subjecting said mixture to hydrothermal treatment in an autoclave at a temperature in the range of 130° to 200° centrigrade under its own pressure for a period of 6 to 30 days to obtain crystals and a mother liquor, (3) separating said crystals from the mother liquor, (4) washing the separated crystals with water and then drying the same, and (5) heating the dried crystals in air so as to calcine the same and eliminate said nitrogenated base therefrom.
Claim 2
Independent Claim 221 words
The method of preparing a porous, crystalline material comprised of silicon oxide and titanium oxide wherein the ratio of said oxides is represented by the formula xTiO.sub.2.(1-x)SiO.sub.2 in which x is a number between 0.0005 and 0.04, which comprises the steps of: (1) preparing an aqueous mixture of starting reagents free from alkali- and alkaline-earth metals including a source of silicon oxide selected from the group consisting of silica gel and tetraalkylorthosilicates, a source of titanium oxide consisting of a hydrolysable titanium compound, and a nitrogenated organic base, and wherein the starting reagents have the following molar ratios: SiO 2 /TiO 2 from 5 to 200, OH - /SiO 2 from 0.1 to 1.0, H 2 O/SiO 2 from 20 to 200, RN + /SiO 2 from 0.1 to 2.0 wherein RN + is the cation of the nitrogenated organic base, (2) subjecting said mixture to hydrothermal treatment in an autoclave at a temperature in the range of 130° to 200° centrigrade under its own pressure for a period of 6 to 30 days to obtain crystals and a mother liquor, (3) separating said crystals from the mother liquor, (4) washing the separated crystals with water and then drying the same, and (5) heating the dried crystals in air so as to calcine the same and eliminate said nitrogenated base therefrom.
Claim 3
Dependent Claim 29 words
A method as claimed in claim 1, wherein the hydrolysable titanium compound is a member of the group consisting of TiCl 4 , TiOCl 2 and Ti(alkoxy) 4 .
Claim 4
Dependent Claim 18 words
A method as claimed in claim 2, wherein Ti(alkoxy) 4 is Ti(OC 2 H 5 ) 4 .
Claim 5
Dependent Claim 15 words
A method as claimed in claim 1, wherein the nitrogenated organic base is tetraalkylammonium hydroxide.
Claim 6
Dependent Claim 16 words
A method as claimed in claim 1, wherein x is a number between 0.01 and 0.025.
Claim 7
Dependent Claim 15 words
A method as claimed in claim 4, wherein the nitrogenated organic base is tetrapropylammonium hydroxide.
Claim 8
Dependent Claim 48 words
A method as claimed in claim 1, wherein the molar ratios of the starting reagents are: SiO 2 /TiO 2 from 35 to 65, OH - /SiO 2 from 0.03 to 0.6, H 2 O/SiO 2 from 60 to 100, RN + /SiO 2 from 0.4 to 1.0.

References Cited (Backward Citations)

US3329482A Cited
US3941871A Cited
US3972983A Cited
US4061724A Cited
US4208305A Cited
US4104294A Cited
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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1986-10-17 1987-04-18 1987-10-18 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1990-10-17 1991-04-18 1991-10-18 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1994-10-17 1995-04-18 1995-10-18 $7700.00 Window Closed / Lapsed

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