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Preparation of titanium silicon molecular sieve having MFI structure

A technology of titanium-silicon molecular sieve and silicon source, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of complex operation process of TS-1 molecular sieve, low product crystallinity, long reaction time, etc., to shorten the synthesis time and crystallinity High, small grain effect

Active Publication Date: 2008-12-24
JIANGSU SANJILI CHEM
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0010] The TS-1 molecular sieve synthesized by the above method is either complicated in operation, long in reaction time (6-30 days), and it is difficult to avoid the hydrolysis of tetraethyl titanate and polymerization into non-bulk anatase; low degree

Method used

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Examples

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Embodiment 1

[0024] Example 1. A kind of preparation method of the titanium silicon molecular sieve with MFI structure, according to reaction mixture SiO 2 :TiO 2 :TPAOH:H 2 O=1: 0.005: 0.10: 20 molar ratio, silicon source, titanium source, tetrapropyl ammonium hydroxide and water are mixed evenly; Then put into the autoclave, feed inert gas, at a temperature of 100 ℃, Hydrothermal crystallization under a pressure of 2.0 MPa for 10 h to obtain a crude titanium-silicon molecular sieve crystallization product.

Embodiment 2

[0025] Example 2. A kind of preparation method of the titanium silicon molecular sieve with MFI structure, according to reaction mixture SiO 2 :TiO 2 :TPAOH:H 2 The molar ratio of O=1:0.1:0.35:80, the silicon source, the titanium source, tetrapropyl ammonium hydroxide and water are mixed evenly; Then put into the autoclave, feed inert gas, the temperature is 220 ℃, Hydrothermal crystallization under a pressure of 5.0 MPa for 72 hours to obtain a crude titanium-silicon molecular sieve crystallization product.

Embodiment 3

[0026] Example 3. A kind of preparation method of the titanium silicon molecular sieve with MFI structure, according to reaction mixture SiO 2 :TiO 2 :TPAOH:H 2 The molar ratio of O=1:0.01:0.20:50, the silicon source, the titanium source, tetrapropyl ammonium hydroxide and water are mixed evenly; Then put into the autoclave, feed inert gas, at a temperature of 160°C, Hydrothermal crystallization under a pressure of 3.5 MPa for 30 hours to obtain a crude titanium-silicon molecular sieve crystallization product.

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Abstract

The invention relates to a preparation method of titanium silicate molecular sieve with an MFI structure which is characterized by homogeneous mixing silicon source, titanium source, tetrapropyl ammonium hydroxide TPAOH with water according to a mol ratio of SiO2:TiO2:TPAOH:H2O=1:0.005-0.1:0.10-0.35:20-80 of the reacting mixture, then hydrothermally crystallizing the mixture for 10-72 hours at inert gas atmosphere in the high pressure reactor at 100-220 DEG C and 2.0-5.0 MPa to obtain the crystal crude product titanium silicate molecular sieve. The method of the invention can reduce the template dosage and the production cost, shorten the synthesis time of the molecular sieve, thereby shortening the product period. The prepared TS-1 molecular sieve has advantages of small crystal grain, high crystallinity basically without extra-framework titanium species and obviously improved catalyst oxidation activity.

Description

technical field [0001] The invention relates to a preparation method of a titanium-silicon molecular sieve, in particular to a preparation method of a five-membered ring titanium-silicon molecular sieve (TS-1) with an MFI structure, and belongs to the technical field of inorganic chemical synthesis. Background technique [0002] TS-1 molecular sieve, since it was first reported by Taramasso et al. (US4, 410, 501) in 1983, has attracted widespread attention due to its excellent catalytic oxidation performance. TS-1 with MFI structure, TS-2 with MEL structure, and TS-48 with larger pore structure have been synthesized so far. Using TS-1 molecular sieve as catalyst and dilute H 2 o 2 It is a mild reaction system for oxidizing agents, and exhibits high activity and selectivity in organic oxidation reactions such as olefin epoxidation, aromatic hydrocarbon hydroxylation, ketone ammonia oximation, and alkane oxidation, and the by-product is only water. Environmentally friendly g...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 杨世刚刘德标徐传春葛本爱
Owner JIANGSU SANJILI CHEM
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