Preparation of porous crystalline synthetic material comprised of silicon and titanium oxides
First Claim
1. 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
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;
SiO2 /TiO2 from 5 to 200,OH- /SiO2 from 0.1 to 1.0,H2 O/SiO2 from 20 to 200,RN+ /SiO2 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.
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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:
xTiO.sub.2.(1-x)SiO.sub.2
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° to 200° C., and the solid product obtained is calcined in air at 550° 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.
347 Citations
7 Claims
- 1. 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
- space="preserve" listing-type="equation">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; SiO2 /TiO2 from 5 to 200, OH- /SiO2 from 0.1 to 1.0, H2 O/SiO2 from 20 to 200, RN+ /SiO2 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. - View Dependent Claims (2, 3, 4, 5, 6, 7)
Specification
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- Resources
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Current AssigneeSnamprogetti S.p.A.
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Original AssigneeSnamprogetti S.p.A.
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InventorsPerego, Giovanni, Notari, Bruno, Taramasso, Marco
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Primary Examiner(s)Meros, Edward J.
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Application NumberUS06/393,379Time in Patent Office476 DaysField of Search423/326-333, 252/431 N, 252/454, 252/455 Z, 260/429.5US Class Current423/705CPC Class CodesB01J 29/89 Silicates, aluminosilicates...C01B 37/005 Silicates, i.e. so-called m...C01B 39/12 the replacing atoms being a...Y10S 423/22 MFI, e.g. ZSM-5. silicalite...
