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A three-dimensional ordered pore structure zeolite molecular sieve and its preparation method

A zeolite molecular sieve, three-dimensional ordered technology, applied in the direction of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problem that cannot meet the needs of industrial catalytic reactions, materials Poor stability, low acid catalytic activity and other problems, to achieve the effect of easy large-scale popularization and application, low cost and simple preparation method

Active Publication Date: 2018-11-09
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the non-crystalline framework structure of mesoporous molecular sieves leads to poor hydrothermal stability and low acid catalytic activity, which cannot meet the needs of industrial catalytic reactions.
The diffusion problem of macromolecules can also be solved by shortening the diffusion channel by nanosizing molecular sieves, but it faces the common disadvantages of nanoparticles: poor material stability, difficult separation, low yield, etc.
So far, the preparation of three-dimensional ordered pore-structured zeolite molecular sieves with rational structures and high acid strengths remains a challenge.

Method used

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  • A three-dimensional ordered pore structure zeolite molecular sieve and its preparation method
  • A three-dimensional ordered pore structure zeolite molecular sieve and its preparation method
  • A three-dimensional ordered pore structure zeolite molecular sieve and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 8mL of styrene, 600mL of water, and 0.12g of sodium dodecylsulfonate into a 1L three-neck flask in turn, heat and stir at 60°C, and pass through N 2 Air was removed for 30 minutes, and then, 0.33 g of potassium persulfate initiator was dissolved in 10 mL of water, heated at 60°C and added to the above-mentioned round bottom flask, heated and stirred at 60°C for 18 hours. The obtained PS spheres were filtered with glass wool to remove aggregates, and then the filtered PS sphere suspension was centrifuged at 5000 rpm for 12 h, and the obtained precipitate was dried to obtain ~50 nm PS spheres.

[0028] ethanol, HNO 3 (0.3mol·L -1 ) and tetraethyl orthosilicate in a mass ratio of 20:0.2:1, stirred at room temperature to form a sol, added ~50nm PS balls, wherein the mass ratio of PS balls to tetraethyl orthosilicate was 1, fully infiltrated, suction filtered, and dried. Get SiO 2 -PS sphere composite; the SiO 2 -PS ball composite material added to 25wt% tetrapropyl...

Embodiment 2

[0031] Add 140mL styrene, 600mL water, and 0.12g sodium dodecylsulfonate into a 1L three-neck flask in turn, heat and stir at 90°C, and pass N 2 Air was removed for 30 minutes, and then, 0.33 g of potassium persulfate initiator was dissolved in 10 mL of water, heated at 90°C and added to the above-mentioned round bottom flask, heated and stirred at 90°C for 18 hours. The obtained PS spheres were filtered with glass wool to remove aggregates, and then the filtered PS sphere suspension was centrifuged at 5000 rpm for 12 h, and the obtained precipitate was dried to obtain ~700 nm PS spheres.

[0032] ethanol, HNO 3 (0.3mol·L -1 ) and tetraethyl orthosilicate at a mass ratio of 20:5:30, stirred at room temperature to form a sol, added ~700nm PS balls, wherein the mass ratio of PS balls to tetraethyl orthosilicate was 1, fully infiltrated, suction filtered, and dried. Get SiO 2 -PS sphere composite; the SiO 2 -PS ball composite material added to 40wt% tetrapropylammonium hydro...

Embodiment 3

[0035] Add 36.6mL of styrene, 600mL of water, and 0.12g of sodium dodecylsulfonate into a 1L three-necked flask in turn, heat and stir at 60°C, and pass through N 2 30min to remove the air. Then, 0.33g of potassium persulfate initiator was dissolved in 10mL of water, heated at 60°C and added to the above-mentioned round bottom flask, heated and stirred at 60°C for 18h. The obtained PS spheres were filtered with glass wool to remove aggregates, and then the filtered PS sphere suspension was centrifuged at 5000 rpm for 12 h, and the obtained precipitate was dried to obtain ~200 nm PS spheres.

[0036] ethanol, HNO 3 (0.3mol·L -1 ) and tetraethyl orthosilicate at a mass ratio of 1:5:1, stirred at room temperature to form a sol, added ~200nm PS balls, wherein the mass ratio of PS balls to tetraethyl orthosilicate was 1, fully infiltrated, suction filtered, and dried. Get SiO 2 -PS sphere composite; the SiO 2 -PS ball composite material added to 25wt% tetrapropylammonium hydrox...

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Abstract

The invention discloses a zeolite molecular sieve of a three-dimensional orderly pore structure and a preparation method thereof and belongs to the field of inorganic material synthesis and catalysis. The zeolite molecular sieve has a macroporous structure, macropores are in three-dimensional orderly arrangement, and size of the macropores is 50-700nm. The preparation method includes: mixing alcohol, HNO3 and tetraethylorthosilicate well, adding polystyrene spheres, suction-filtering, and drying to obtain a SiO2-PS sphere composite material; adding the SiO2-PS sphere composite material into a tetrapropyl ammonium hydroxide water solution, suction-filtering, drying, adding a certain amount of NaAlO2, and drying; using a steam-assisted crystallizing method to convert obtained dry glue into a molecular sieve, drying, and roasting to remove a PS sphere template to obtain the zeolite molecular sieve of three-dimensional orderly pore structure. The preparation method is suitable for preparing ZSM-5 type, beta type and Y type molecular sieves. The zeolite molecular sieve synthesized by the method has the advantages of large specific surface area, uniform macropores, high crystallinity, complete structure and acidity adjustability and can be used as a functional material for catalysis, adsorption and separation.

Description

technical field [0001] The invention belongs to the field of inorganic material synthesis and catalysis, and in particular relates to a three-dimensional ordered pore structure zeolite molecular sieve and a preparation method thereof. Background technique [0002] Zeolite molecular sieve is a porous compound composed of aluminosilicate, composed of TO 4 The tetrahedrons form a three-dimensional four-coordinated framework by sharing vertices, and the T atoms of the framework are usually Si and Al atoms. According to the different skeleton structures, it can be divided into ZSM-5, β, Y, X, SAPO and other types. Due to their large specific surface area, strong acidity, unique micropore channels, and good hydrothermal and thermal stability, molecular sieves have advantages in the effective capture of small molecules, shape-selective catalysis, and effective separation of transition state molecules and product molecules. widely used. However, conventional zeolite molecular sie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04C01B39/24C01B39/40
CPCC01B39/04C01B39/24C01B39/40C01P2002/72C01P2004/03
Inventor 骞伟中王宁侯一林魏飞
Owner TSINGHUA UNIV