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Multi-stage porous titanium-silicon zeolite preparation method and its uses in catalytic oxidation

A titanium silicalite, catalytic oxidation technology, applied in the direction of crystalline aluminosilicate zeolite, molecular sieve catalyst, chemical equipment and methods, etc., can solve the problems of difficult control, wide distribution of titanium silicalite mesopore size, etc., and achieve good catalytic performance Effect

Inactive Publication Date: 2006-07-26
DALIAN UNIV OF TECH
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Scientists at Haldor Topsoe used mesoporous carbon black to prepare titanium silicalite (TS-1), which improved the catalytic performance of titanium silicalite in ethylene epoxidation (Schmidt et.al, Chem.Comm, 2000, 2157-2158 ), but the obtained titanium silicalite has a wide pore size distribution and is difficult to control

Method used

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  • Multi-stage porous titanium-silicon zeolite preparation method and its uses in catalytic oxidation
  • Multi-stage porous titanium-silicon zeolite preparation method and its uses in catalytic oxidation
  • Multi-stage porous titanium-silicon zeolite preparation method and its uses in catalytic oxidation

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Preparation of powdery ordered mesoporous carbon material: take 5g powder Al / SBA-15 with a silicon-aluminum ratio of 20 (using P123 as a template), add furan methanol according to the equal volume impregnation method, and polymerize in an oven at 90°C After 12 hours, the obtained polymer was carbonized under the protection of high-purity nitrogen. The carbonization program was from room temperature to 150°C at a heating rate of 1°C / min; Let cool to room temperature. The resulting product was refluxed overnight in 5% HF acid to remove the templated SBA-15.

Embodiment 2

[0027] Preparation of bulk ordered mesoporous carbon material: the powdered Al / SBA-15 in Example 1 was replaced with bulk Al / SBA-15, and other methods were similar to Example 1.

Embodiment 3

[0029] Synthesis of mesoporous TS-1: take 4 g of the ordered mesoporous carbon material synthesized in Example 1, add a pre-mixed solution containing tetrapropylammonium hydroxide, ethanol, and water according to the equal volume impregnation method, and let the ethanol Volatile, then press C / SiO 2 The mass ratio of 2:1 was added dropwise to the mixed solution of ethyl orthosilicate and butyl titanate. The material ratio of each raw material is SiO 2 / TiO 2 / TPAOH / H 2 O 1:0.0125:0.2:2, aging at room temperature for 3h, and then crystallized in a Teflon-lined autoclave at 170°C for 48h, the resulting solid was washed with water, filtered, dried at 120°C for 4h, and calcined at 550°C for 4h to obtain a white Mesoporous TS-1 powder. The obtained product was characterized by X-ray diffraction, Fourier transform infrared spectroscopy, ultraviolet-visible spectroscopy, nitrogen adsorption, transmission electron microscopy, etc., which proved that the product contained a signific...

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Abstract

The preparation method for titanium-silicon zeolite with multilevel holes comprises: 1) preparing the ordered meso-hole carbon material template agent; 2) leading all the silicon source, titanium source and said template agent into the hole channel in template agent with stage dipping; 3) taking water-thermal crystallization treatment to the obtained mixture; 4) removing the carbon material and agent. This invention has better catalysis performance than traditional molecular sieve, and fits to oil and fine chemical industry.

Description

technical field [0001] The invention belongs to the technical field of preparation and application of zeolite. Specifically, it relates to a method for preparing a multi-level porous titanium silicalite by using an ordered mesoporous carbon material as a template. Background technique [0002] As a new type of catalytic material, titanium-silicon molecular sieve shows excellent performance in the field of catalytic oxidation. The earliest studied titanium-silicon molecular sieves are TS-1 with MFI topology (Taramasso et.al, U.S.Pat.4,410,501) and TS-2 with MEL topology (Reddy et.al, Appl.Catal., 1990, 58( 2): L1-L4). In the 20 years since its first synthesis, it has been widely used in the oxidation of many organic compounds (Sheldon et.al., Appl.Catal.A, 1999, 189:163-183), such as the epoxidation of alkenes , Hydroxylation of aromatics, ammoxidation of ketones, oxidation of alkanes, and oxidation of alcohols and amines. Titanium silicate molecular sieve TS-1 (TS-2) exh...

Claims

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Application Information

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IPC IPC(8): C01B39/08B01J29/89
Inventor 胡浩权方云明
Owner DALIAN UNIV OF TECH
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