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Micropore-mesopore grading structural material and preparation method thereof

A technology with hierarchical structure and mesoporous structure, applied in chemical instruments and methods, molecular sieve catalysts, crystalline aluminosilicate zeolites, etc., to achieve good hydrothermal performance, short cycle time, and good hydrothermal stability

Active Publication Date: 2010-01-06
中国科学院上海硅酸盐研究所苏州研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, the steam-assisted method has been successfully applied to the preparation of microporous zeolite molecular sieves. The zeolite molecular sieves prepared by this method have uniform particles and good crystallization. The method of crystallization treatment to prepare microporous-mesoporous hierarchical structure materials with pore wall crystallization has not been reported yet.

Method used

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  • Micropore-mesopore grading structural material and preparation method thereof
  • Micropore-mesopore grading structural material and preparation method thereof
  • Micropore-mesopore grading structural material and preparation method thereof

Examples

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Embodiment 1

[0044] Take 0.66 grams of aluminum isopropoxide, 20.8 grams of ethyl orthosilicate, 1.49 grams of triethanolamine and 19.8 grams of deionized water, mix them vigorously for 1 hour, and then add 82 grams of tetrapropyl hydroxide with a mass fraction of 25%. Ammonium solution, continue stirring until a solid gel is formed. The molar ratio of various precursors in the raw material is: aluminum isopropoxide: ethyl orthosilicate: triethanolamine: tetrapropyl ammonium hydroxide: deionized water = 1:30:3:30:330. After aging the prepared gel at room temperature for 24 hours, it was heated at 98° C. for 12 hours. The resulting product after heating is then transferred to a polytetrafluoroethylene container, which is then placed into a larger polytetrafluoroethylene hydrothermal kettle (such as figure 1 ), and drop 1 gram of deionized water between the periphery of the container and the hydrothermal kettle, seal the hydrothermal kettle, and heat at 160° C. for 24 hours. After the stea...

Embodiment 2

[0046] According to the method of Example 1, but the molar ratio of various precursors in the raw material is adjusted to: aluminum isopropoxide: ethyl orthosilicate: triethanolamine: tetrapropyl ammonium hydroxide: deionized water=1: 200 : 20: 200: 2200 to obtain a sample with a silicon-aluminum ratio of 200: 1. Then some of the samples prepared in Example 2 were taken for hydrothermal stability test, specifically hydrothermal treatment at 100°C for 50 hours.

Embodiment 3

[0048] According to the method of Example 1, but the molar ratio of various precursors in the raw material is adjusted to: tetrabutyl titanate: ethyl orthosilicate: triethanolamine: tetrapropyl ammonium hydroxide: deionized water=1: 50:5:50:550. A sample with a silicon to titanium ratio of 50:1 was obtained. Then some of the samples prepared in Example 3 were taken for hydrothermal stability test, specifically hydrothermal treatment at 100° C. for 50 hours.

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Abstract

The invention belongs to the field of inorganic materials, in particular to a micropore-mesopore grading structural material and a preparation method thereof. A microscopic particle of the micropore-mesopore grading structural material has a three-dimensional penetrated mesopore structure, and the pore wall of the mesopore structure is in a crystallized zeolite structure. The micropore-mesopore grading structural material has favorable hydrothermal stability; because the pore wall of the micropore-mesopore grading structural material is in the crystallized zeolite structure, the micropore-mesopore grading structural material can be applied to the field of catalyst; and the preparation method of the micropore-mesopore grading structural material has the characteristics of simple condition and easy operation and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of inorganic materials, and in particular relates to a microporous-mesoporous hierarchical structure material and a preparation method thereof. Background technique [0002] As a traditional solid acid catalyst, microporous zeolite molecular sieve materials have been widely used in industry. The outstanding feature of zeolite molecular sieve is that it can adjust the acidity, and at the same time, it can provide pores and holes of different sizes to play a shape-selective effect, so it is different Molecular sieves with different pore sizes have different shape-selective effects. However, due to its small pore size (<1.5nm), the difficulty of diffusion of reactants and products in the pores seriously affects the catalytic efficiency. For example, heavy oil macromolecules with a diameter greater than 1nm in the reaction raw material are difficult to diffuse into the pores of the molecular sieve, and its narrow pore...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02C01B39/04B01J29/06B01J29/89B01J29/88B01J32/00
Inventor 周健华子乐施剑林
Owner 中国科学院上海硅酸盐研究所苏州研究院