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Preparation method for high stability mesoporous molecular sieve under ionothermal system

An ionic liquid and ionic technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of poor hydrothermal stability, environmental pollution, and the production of a large amount of waste acid or lye, and achieve stable performance, extended application range, and thermal stability. The effect of strong stability

Inactive Publication Date: 2013-02-20
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the problems of poor hydrothermal stability of existing mesoporous molecular sieves, a large amount of waste acid or lye produced during the preparation process, and pollution to the environment, the present invention provides a non-ionic surface with an acid-functional ionic liquid as a medium. A method for preparing mesoporous molecular sieves with high hydrothermal stability by using an active agent or an ionic surfactant as a template. The mesoporous molecular sieves prepared by this method have better hydrothermal stability than those prepared in a hydrothermal system. Functionalized ionic liquids can be reused

Method used

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  • Preparation method for high stability mesoporous molecular sieve under ionothermal system
  • Preparation method for high stability mesoporous molecular sieve under ionothermal system

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Embodiment 1

[0020] 0.3 g sodium metaaluminate, 6.69 g silica solution (30%), 0.568 g sodium silicate, 5 g acid functionalized ionic liquid 1-methyl-3-(3-sulfopropyl)imidazole hydrogen sulfate salt, mixed in a reaction kettle, and then crystallized at 140°C for 4 hours, and then added acid-functionalized ionic liquid 1-methyl-3-(3-sulfopropyl)imidazole hydrogen sulfate to the solution after crystallization 20 grams of salt and 4 grams of P123 were mixed and stirred at 40°C for 20 hours. The crystallized mixed solution was crystallized at 100°C for 24 hours. After crystallization, cool to room temperature, add deionized water to dilute and wash, filter with suction, dry the powder at 60°C for 24 hours, and roast at 550°C for 6 hours to obtain the product.

Embodiment 2

[0022] 0.3 g sodium metaaluminate, 6.69 g silica solution (30%), 0.568 g sodium silicate, 5 g acid functionalized ionic liquid 1-ethyl-3-(3-sulfopropyl)imidazole hydrogen sulfate salt, mixed in a reaction kettle, and then crystallized at 120°C for 4 hours, and then added acid-functionalized ionic liquid 1-ethyl-3-(3-sulfopropyl) imidazole sulfuric acid to the solution after crystallization 20 grams of hydrogen salt and 4 grams of P123 were mixed and stirred at 50°C for 20 hours. Crystallization at 100°C for 24 hours. After crystallization, cool to room temperature, add deionized water to dilute and wash, filter with suction, dry the powder at 60°C for 20 hours, and roast at 600°C for 7 hours to obtain the product.

Embodiment 3

[0024] 0.3 g sodium metaaluminate, 13.92 g silica solution (30%), 1.14 g sodium silicate, 10 g acid functionalized ionic liquid 1-ethyl-3-(3-sulfobutyl)imidazole hydrogen sulfate Mix the salts in a reaction kettle, then crystallize at 130°C for 5 hours, cool to room temperature, and then add acid-functionalized ionic liquid 1-ethyl-3-(3-sulfobutyl) to the solution after crystallization Mix 45 g of imidazolium bisulfate and 4 g of P123 and stir at 40°C for 20 hours. Crystallization at 100°C for 24 hours. After crystallization, cool to room temperature, add deionized water to dilute and wash, filter with suction, dry the powder at 60°C for 12 hours, and roast at 550°C for 7 hours to obtain the product.

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Abstract

The present invention discloses a method for preparing a high hydrothermal stability mesoporous molecular sieve by adopting an acid functionalized ion liquid as a medium and adopting a non-ionic surfactant or an ionic surfactant as a template agent. The preparation method comprises: sequentially adding sodium meta-aluminate, silica hydrosol (30%), sodium silicate and an acid functionalized ion liquid to a reaction kettle, uniformly mixing at a room temperature in the reaction kettle, transferring the mixed material to an autoclave, carrying out crystallization for 4-6 hours at a temperature of 120-140 DEG C, cooling to a room temperature after completing the reaction, adding an acid functionalized ion liquid and a template agent to the solution after the reaction, stirring for 20-24 hours at a temperature of 40-60 DEG to obtain a homogeneous phase gel mixture, transferring the gel mixture to the autoclave, carrying out crystallization for 24-48 hours at a temperature of 100-120 DEG C, cooling, adding deionized water to dilute and wash, carrying out suction filtration, and carrying out drying calcination to obtain the mesoporous molecular sieve product. The mesoporous molecular sieve prepared by the preparation method has good hydrothermal stability while the ion liquid can be recycled. The synthesis method has advantages of simpleness and environmental friendliness, and has important application values in the field of material science.

Description

technical field [0001] The invention relates to a synthesis method of mesoporous molecular sieves, in particular to a mesoporous compound with high hydrothermal stability prepared by using an acid-functionalized ionic liquid as a medium and a nonionic surfactant or an ionic surfactant as a template. Molecular sieve method. Background technique [0002] Since the new mesoporous molecular sieve M41S or SBA-15 was successfully developed, it has a good application prospect as a catalyst for macromolecular reactions due to its large and uniform pore structure. However, the pore wall of this type of mesoporous molecular sieve is amorphous, and the pore wall is easily penetrated by local hydrolysis or thermal action, and even the entire molecular sieve lattice collapses, resulting in poor thermal and hydrothermal stability. This restricts the industrial application of mesoporous molecular sieves. In order to improve the thermal stability and hydrothermal stability of mesoporous m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 于世涛李露刘仕伟解从霞刘福胜陈彦
Owner QINGDAO UNIV OF SCI & TECH
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