Method of preparing ordered mesoporous molecular sieve with high hydrothermal stability

A technology of mesoporous molecular sieve and thermal stability, which is applied in the direction of molecular sieve compounds, molecular sieves and base exchange compounds, chemical instruments and methods, etc., to achieve good hydrothermal stability and avoid toxicity

Inactive Publication Date: 2009-09-30
JILIN UNIV
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Problems solved by technology

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

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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

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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 suction filtered 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. Afte...

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] Figure 5 Among them, A is JLU-20-TPA obtained after calcination, and B is 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 JLU-20-TPA powder ( Figure 6 ), the degree of condensation of silicon species even exceeds that of JLU-20-TEA, and the Q obtained by fitting 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 t...

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 preparation method of the ordered mesoporous molecular sieve with high hydrothermal stability belongs to the technical field of inorganic chemistry and catalytic chemistry. The process includes preparing template agent, making raw powder and removing template agent. The templating agent is prepared by using a mixture of small molecule quaternary ammonium salts and hydrocarbon surfactants as the templating agent, and the aqueous solution of the templating agent is adjusted to a pH value less than 1 with HCl; the original powder is prepared by adding the silicon source to the templating agent solution and stirring To form a gel, carry out hydrothermal crystallization at 100-220°C for 24-120 hours, and hydrothermal crystallization can also be carried out in two steps; removing the template agent can be performed by calcining the original powder at a temperature of 400-700°C. The present invention replaces the fluorocarbon surfactant as a mixed template with a small molecule quaternary ammonium salt, avoids the toxicity of the fluorine-containing surfactant, and synthesizes an ordered mesoporous molecular sieve under high-temperature hydrothermal conditions. The skeleton of the product is The silicon species in are highly condensed and have very good hydrothermal stability.

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 Patents(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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