Method of preparing ordered mesoporous molecular sieve with high hydrothermal stability

A mesoporous molecular sieve, thermal stability technology, applied in molecular sieve compounds, molecular sieve and alkali exchange compounds, chemical instruments and methods, etc., to achieve good hydrothermal stability and avoid toxicity.

Inactive Publication Date: 2007-10-17
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to disclose a synthesis method of mesoporous molecular sieve material, which uses small molecule quaternary ammonium salt to replace the fluorocarbon surfactant in the background technology, mixes it with hydrocarbon surfactant as template agent, and passes through high temperature water Thermal synthesis to prepare mesoporous molecular sieve materials with highly condensed silicon species in the product skeleton, good hydrothermal stability and high catalytic activity

Method used

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  • Method of preparing ordered mesoporous molecular sieve with high hydrothermal stability
  • Method of preparing ordered mesoporous molecular sieve with high hydrothermal stability
  • Method of preparing ordered mesoporous molecular sieve with high hydrothermal stability

Examples

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Embodiment 1

[0026] Example 1: High temperature synthesis of hydrothermally stable ordered mesoporous molecular sieve JLU-20-TEA.

[0027] Dissolve 0.4g of triblock copolymer (P123) and 0.8g of tetraethylammonium bromide in 25mL of deionized water, stir well, add 3mL of hydrochloric acid, stir until clarified, then add silicon source tetraethyl orthosilicate (TEOS) 2.08g. The above solution was stirred at 40° C. for 20 hours, then transferred to a reaction kettle, and left at 120° C. for 48 hours. The product was extracted and dried at room temperature to obtain the original powder. Raise the temperature of the original powder to 450°C in the air and keep it for 5 hours to remove the surfactant and obtain open channels.

[0028] It is also possible to carry out two crystallizations after the surfactant and the silicon source solution are transferred into the reactor, that is, standing at 100° C. for 24 hours. Then the temperature was raised to 180° C. and left for 48 hours. After calci...

Embodiment 2

[0030] Example 2: High temperature synthesis of hydrothermally stable ordered mesoporous molecular sieve JLU-20-TPA.

[0031] Weigh 0.8g tetrapropylammonium bromide (TPABr) instead of tetraethylammonium bromide, other feeding steps and treatment methods are the same as in Example 1, and the obtained product is designated as JLU-20-TPA.

[0032] In Figure 5, A is the JLU-20-TPA obtained after calcination, and B is the JLU-20-TPA after calcination and treated with steam at 800°C for two hours. The results show that, similar to JLU-20-TEA, JLU-20-TPA is also a highly ordered mesoporous molecular sieve, and also has high hydrothermal stability. 29 Si NMR results show that in the original powder of JLU-20-TPA (Figure 6), the degree of condensation of silicon species even exceeds that of JLU-20-TEA, and the Q 4 / Q 3 The value of 4.9. These results indicate that tetrapropylammonium bromide can obtain ordered and hydrothermally stable mesoporous molecular sieves at high temperature...

Embodiment 3

[0033] Example 3: High temperature synthesis of hydrothermally stable ordered mesoporous molecular sieve JLU-20-TBA.

[0034] Using 0.8g of tetrabutylammonium bromide and hydrocarbon surfactant (P123) as a mixed template, other feeding steps and treatment methods are the same as in Example 1, and the obtained product is designated as JLU-20-TBA. The structure and performance of the product obtained are substantially the same as the JLU-20-TPA obtained in Example 2.

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Abstract

The invention relates to a method for preparing ordered media-hole molecular screen with high hydro-thermal stability, which belongs to the technical field of inorganic chemistry and catalysis chemistry. And the processing contains preparing template agent and raw powder and removing template agent. During the template agent preparation, the mixture of small molecular quaternary ammonium salt and the carbon and hydrogen surface active agent is used as the template agent and the template agent solution is adjusted to PH<1 with HCl. During the raw powder preparation process, silica source is added in the template agent solution, stirred to produce sol and hydro-thermal crystallization for 24-120 hours at the temperature 100-220 degree which can be carried out in two steps. And during the template agent removal process, the raw powder is calcined in 400-700 degree. The invention uses the small molecular quaternary ammonium salt instead of F/C surface active agent as the mixed template agent, which avoids the toxicity of F-contained surface active agent and produces ordered media-hole molecular screen. The product has good hydro-thermal stability because the silica-contained substances in the skeleton of the product are highly condensed.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemistry and catalytic chemistry, and particularly relates to a method for synthesizing ordered mesoporous molecular sieves by using small molecular quaternary ammonium salts as template agents. Background technique [0002] Since Mobil Corporation of the United States first synthesized highly ordered mesoporous molecular sieves in 1992, mesoporous molecular sieves have attracted increasing attention. Because it has potential uses in many fields such as separation and purification, biological materials, chemical synthesis, semiconductors, optical devices, drug delivery, etc., especially it has extremely important application value as an adsorbent, catalyst and catalyst carrier. However, unlike traditional microporous molecular sieve crystals, mesoporous molecular sieves have low hydrothermal stability due to incomplete condensation of silicon species in the framework and a large number of hydro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04C01B39/00C01B37/00
Inventor 肖丰收杜耘辰李德凤关项羽
Owner JILIN UNIV
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