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Melt flow index (MFI) structure titanium silicalite molecular sieve with small crystal particle and preparation method thereof

A technology of titanium-silicon molecular sieve and small crystal grains, which is applied in the direction of crystalline aluminosilicate zeolite, etc., and can solve the problems of small molecular sieve grains and large grains of MFI structure titanium-silicon molecular sieves, etc.

Inactive Publication Date: 2012-05-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] One of the technical problems to be solved by the present invention is the problem that the crystal grains of the MFI structure titanium-silicon molecular sieves obtained in the prior art are relatively large, and a new MFI structure titanium-silicon molecular sieve is provided, which has the advantage of small crystal grains

Method used

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  • Melt flow index (MFI) structure titanium silicalite molecular sieve with small crystal particle and preparation method thereof
  • Melt flow index (MFI) structure titanium silicalite molecular sieve with small crystal particle and preparation method thereof

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Effect test

Embodiment 1

[0010] Silica sol (40%, by weight), bis(triethoxysilyl)methane, TiCl 4 , Tetrapropylammonium hydroxide, ammonia water and water are mixed evenly according to the stoichiometric ratio, wherein the molar ratio of each component of the raw material is: 1:0.01:0.01:0.03:0.4:20. Crystallize at 160° C. for 1 day, and the product is filtered, washed with water, and dried to obtain MFI titanium-silicon molecular sieves containing skeleton organic groups. The sample after drying is determined, and its infrared spectrum data is at 1223cm -1 There is a corresponding infrared absorption peak of organic silicon, and the average grain length is 9 microns.

Embodiment 2

[0012] Solid silica (2000 mesh), bis(triethoxysilyl)methane, TiCl 3 , Tetrapropylammonium bromide, ethylamine and water are mixed uniformly in a stoichiometric ratio, wherein the molar ratio of each component of the raw material is: 1:0.05:0.03:0.15:2.0:100. Crystallize at 170° C. for 5 days, and the product is filtered, washed with water, and dried to obtain an MFI titanium-silicon molecular sieve containing a skeleton organic group. The sample after drying is determined, and its infrared spectrum data is at 1223cm -1 There is a corresponding infrared absorption peak of organic silicon, and the average grain length is 10 microns.

Embodiment 3

[0014] Tetraethyl orthosilicate, bis(triethoxysilyl)methane, TiOCl 2 , Tetrabutylammonium hydroxide, n-propylamine and water are mixed uniformly in a stoichiometric ratio, wherein the molar ratio of each component of the raw material is: 1:0.03:0.02:0.09:1.2:60. Crystallize at 180° C. for 10 days, and the product is filtered, washed with water, and dried to obtain an MFI titanium-silicon molecular sieve containing a skeleton organic group. The sample after drying is determined, and its infrared spectrum data is at 1223cm -1 There is a corresponding infrared absorption peak of organic silicon, and the average grain length is 11 microns.

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Abstract

The invention relates to a melt flow index (MFI) structure titanium silicalite molecular sieve with a small crystal particle and a preparation method thereof, which mainly solve the problem of big crystal particle of the MFI structure titanium silicalite molecular sieve in the prior art. The MFI structure titanium silicalite molecular sieve with the small crystal particle is prepared, wherein infrared spectrum data is provided with a corresponding organic silicon infrared absorption peak within the range of 1213-1278cm<-1>. The problem is better solved by the technical scheme of the preparation method. The preparation method can be used for preparing and producing the MFI structure titanium silicalite molecular sieve with the small crystal particle.

Description

technical field [0001] The invention relates to a small-grain MFI structure titanium-silicon molecular sieve and a preparation method thereof. Background technique [0002] USP 04410501 patent report Italy Eni (ENI) company successfully synthesized MFI structure titanium silicon molecular sieve TS-1, in which titanium entered the molecular sieve framework structure, opened up a new chapter for the research in this field. Using TS-1 as a catalytic oxidation catalyst not only has high catalytic activity and selectivity, but also has mild reaction conditions and the by-product is water (H 2 o 2 as an oxidant), harmless to the environment. dilute H 2 o 2 As an oxidizing agent, it can catalyze partial oxidation of alkanes, epoxidation of alkenes, hydroxylation of aromatic hydrocarbons and phenols, oxidation of primary (secondary) alcohols and ammonia of ketones under mild conditions (normal temperature, <60°C, normal pressure). oxidation. We know that the grain size of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08
Inventor 何欣高焕新刘志成
Owner CHINA PETROLEUM & CHEM CORP