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Mesoporous titanium-silicon material preparation method

A titanium-silicon and mesoporous technology, which is applied in the field of preparing mesoporous titanium-silicon materials, achieves the effects of high selectivity of target products, improved synthesis efficiency, and high catalytic oxidation activity

Active Publication Date: 2015-04-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the yield, mesoporous order (relative crystallinity) and catalytic performance of Ti-MCM-41 prepared by the existing method need to be further improved.

Method used

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  • Mesoporous titanium-silicon material preparation method
  • Mesoporous titanium-silicon material preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] First, add 50 grams of tetraethyl orthosilicate and cetyltrimethylammonium bromide to the aqueous solution of tetrapropylammonium hydroxide dispersed in tetrabutyl titanate in advance and stir and mix, wherein tetraethyl orthosilicate The molar ratio of ester, tetrabutyl titanate, tetrapropylammonium hydroxide, cetyltrimethylammonium bromide and water is 1:0.02:0.45:0.15:85, and the organosilicate is SiO 2 Meter, titanium source as TiO 2 Alkali source templating agent is measured by OH- or N. After the silicon ester is hydrolyzed, transfer the mixture into a sealed reaction kettle for hydrothermal crystallization at 110°C for 12 hours. After cooling, add silica gel to the crystallization system and mix well. The molar ratio of the silica gel to the organic silicon source is 1:0.2, and then the mixture is crystallized in a sealed reaction vessel at a temperature of 150°C and an autogenous pressure for 18h, and the resulting crystallized product is filtered, washed, and d...

Embodiment 2

[0028] First, 50 grams of tetramethyl orthosilicate and tetradecyltrimethylammonium bromide, a surfactant, were added to the aqueous solution of tetrapropylammonium hydroxide in which tetraethyl titanate was dispersed in advance and stirred and mixed, wherein orthosilicate The molar ratio of tetramethyl titanate, tetraethyl titanate, tetrapropylammonium hydroxide, surfactant and water is 1:0.008:0.15:0.05:25, wherein the organosilicate is SiO 2 Meter, titanium source as TiO 2 Alkaline source template agent is calculated by OH- or N. After the silicon ester is hydrolyzed, the mixture is transferred to a sealed reaction kettle for hydrothermal crystallization at 120°C for 12 hours. After cooling, silica gel is added to the crystallization system and mixed evenly. The molar ratio of the silica gel to the organic silicon source is 1:0.1, and then the mixture is continued to be crystallized in a sealed reaction vessel at a temperature of 170°C and an autogenous pressure for 12 hour...

Embodiment 3

[0030] First, 50 grams of tetraethyl orthosilicate and cetyltrimethylammonium bromide were added to the ethylamine aqueous solution in which tetrabutyl titanate was dispersed in advance and stirred and mixed, wherein tetraethyl orthosilicate, tetrabutyl titanate The molar ratio of butyl ester, ethylamine, surfactant and water is 1:0.4:0.35:0.25:150, wherein the organosilicate is SiO 2 Meter, titanium source as TiO 2 Alkaline source templating agent is measured by OH- or N. After the silicon ester is hydrolyzed, transfer the mixture into a sealed reaction kettle for hydrothermal crystallization at 100°C for 12 hours. After cooling, add silica gel to the crystallization system and mix well. The molar ratio of the silica gel to the organic silicon source is 1:0.5, and then the mixture is continued to be crystallized in a sealed reaction vessel at a temperature of 140°C and an autogenous pressure for 12h, and the obtained crystallized product is filtered, washed with water, and he...

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Abstract

The present invention provides a mesoporous titanium-silicon material preparation method, which is characterized by comprising: adding an organic silicon source and a surfactant to a titanium source-containing alkali source aqueous solution to obtain a mixture A, transferring the mixture A into a sealed reaction kettle after the organic silicon source is hydrolyzed, carrying out hydrothermal crystallization for 1-12 h at a temperature of 100-180 DEG C, contacting a silica gel or silica sol after the crystallization, uniformly mixing to obtain a mixture B, carrying out hydrothermal crystallization on the mixture B in the sealed reaction kettle for 6-36 h at a temperature of 120-200 DEG C, and recovering to obtain the mesoporous titanium-silicon material, wherein the molar ratio of the organic silicon source to the titanium source to the alkali source (calculated as OH<-> or N) to the surfactant to the water is 1:0.001-0.5:0.05-0.8:0.01-0.5:5-250, the molar ratio of the silica gel or silica sol in the mixture B to the organic silicon source in the mixture A is 1:0.05-0.5, the organic silicon source is calculated as SiO2, the titanium source is calculated as TiO2, and the alkali source templating agent is calculated as OH<-> or N. The mesoporous titanium-silicon material prepared by the preparation method of the present invention has characteristics of yield increasing, relative crystallinity increasing, and excellent catalysis performance on macromolecule oxidation reactions.

Description

technical field [0001] The present invention relates to a method for synthesizing inorganic materials, and more specifically to a method for preparing mesoporous titanium-silicon materials. Background technique [0002] Titanium-silicon molecular sieve is a new molecular sieve containing heteroatom titanium, which was developed in the early 1980s. Among them, TS-1 molecular sieve is a new type of titanium-silicon molecular sieve with excellent directional oxidation catalytic performance formed by introducing transition metal element titanium into the molecular sieve framework with ZSM-5 structure. However, TS-1 only has a microporous (about 0.55 nanometer) structure, and it is difficult for large organic molecules to diffuse and be catalyzed and oxidized in it, making it difficult to exert its excellent catalytic oxidation performance in a wider field, especially in the field of biological and pharmaceutical macromolecules Come out, which in turn prompts people to develop a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04C01B39/08
CPCC01B39/085
Inventor 史春风朱斌林民
Owner CHINA PETROLEUM & CHEM CORP
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