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Method for synthesizing ultra-stable ordered mesoporous Si-Al molecular sieve

A technology of mesoporous molecular sieve and mesoporous silica-alumina, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problem that the hydrothermal stability of molecular sieve is not as good as that of microporous zeolite, and achieve the effect of high condensation degree and strong hydrothermal stability

Inactive Publication Date: 2008-06-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The synthesis method described in the above background technology is only to modify the hydrothermal stability of the ordered mesoporous molecular sieve from a single aspect such as increasing the thickness of the pore wall, increasing the condensation degree of the silicon species in the framework, or introducing the microstructure unit of the microporous zeolite in the pore wall. , the hydrothermal stability of the obtained molecular sieve is still not as good as that of microporous zeolite, so it cannot meet the needs of practical industrial applications.

Method used

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  • Method for synthesizing ultra-stable ordered mesoporous Si-Al molecular sieve
  • Method for synthesizing ultra-stable ordered mesoporous Si-Al molecular sieve
  • Method for synthesizing ultra-stable ordered mesoporous Si-Al molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0026] Add 1.44 g of tetrapropylammonium bromide into deionized water at room temperature. After it is completely dissolved, add tetraethyl orthosilicate, sodium aluminate and deionized water to the solution, so that the moles of each reactant Ratio: TPA + / Al 2 o 3 / SiO 2 / Na 2 O / H 2 O=1:0.055:2.58:0.057:316.5. The above solution was stirred at 25° C. for 24 hours to obtain a ZSM-5 type precursor. Add 90 ml of deionized water to the prepared ZSM-5 precursor, and stir at 25° C. for 2 hours to obtain a dilution of the ZSM-5 precursor. Next, 3 grams of calcined SBA-15 was added to the diluted solution of the precursor, and stirred at 25° C. for 1 hour, and then the reaction mixture was placed at 130° C. for constant temperature crystallization for 24 hours. After the product obtained from the first crystallization was filtered, washed and dried for 24 hours, it was suspended in 10.0 ml of glycerin and crystallized at a constant temperature of 130° C. for 48 hours. Finall...

Embodiment 2

[0030] Add 1.14 g of tetraethylammonium bromide into deionized water at room temperature. After it is completely dissolved, add tetraethylorthosilicate, sodium aluminate and deionized water to the solution, so that the moles of each reactant Ratio: TEA + / Al 2 o 3 / SiO 2 / Na 2 O / H 2 O=1:0.055:2.58:0.057:316.5. The above solution was stirred at 25° C. for 24 hours to obtain a Beta type precursor. Add 90 ml of deionized water to the prepared Beta precursor, and stir at 25° C. for 2 hours to obtain a dilution of the Beta precursor. Next, 3 grams of calcined SBA-15 was added to the diluted solution of the precursor, and stirred at 25° C. for 1 hour, and then the reaction mixture was placed at 130° C. for constant temperature crystallization for 24 hours. After the product obtained from the first crystallization was filtered, washed and dried for 24 hours, it was suspended in 10.0 ml of glycerin and crystallized at a constant temperature of 130° C. for 48 hours. Finally, th...

Embodiment 3

[0034] Add 1.44 g of tetrapropylammonium bromide into deionized water at room temperature. After it is completely dissolved, add tetraethyl orthosilicate, sodium aluminate and deionized water to the solution, so that the moles of each reactant Ratio: TPA + / Al 2 o 3 / SiO 2 / Na 2 O / H 2 O=1:0.275:2.58:0.285:316.5. The above solution was stirred at 25° C. for 24 hours to obtain a ZSM-5 type precursor. Add 90 ml of deionized water to the prepared ZSM-5 precursor, and stir at 25° C. for 1 hour to obtain a dilution of the ZSM-5 precursor. Next, 3 grams of calcined SBA-15 was added to the diluted solution of the precursor, and stirred at 25° C. for 1 hour, and then the reaction mixture was placed at 130° C. for constant temperature crystallization for 36 hours. After the first crystallization product was filtered, washed and dried for 24 hours, it was suspended in 7.5 ml of glycerin and crystallized at a constant temperature of 130°C for 48 hours. Finally, the product obtaine...

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Abstract

The invention discloses a siallite molecular sieve synthesizing method of super-stable sequent dielectric hole, which is characterized by the following: adopting sintered dielectric hole SBA-15 molecular sieve as hard mould; placing the hard mould in the diluent of micro-hole zeolitic priority mould agent; suspending in the glycerin to proceed second crystallizing synthesis to obtain dielectric hole molecular sieve with thick hole wall; possessing high-condensed silicon material and little hydroxyl group on the surface or in the inner part of hole wall. The hole wall contains five-ring micro-structure unit with micro-hole zeolite, which possesses super-strong water-heat stability.

Description

technical field [0001] The invention belongs to the technical field of inorganic nanometer materials, and in particular relates to the preparation technology of ordered mesoporous silicon-aluminum molecular sieves with super-strong hydrothermal stability. Background technique [0002] Ordered mesoporous molecular sieves have high specific surface area, regularly arranged and adjustable pores (2-50nm), which makes them have broad application prospects in many fields such as catalysis, adsorption and assembly of macromolecules. It has attracted widespread attention since its publication. However, compared with microporous zeolites, the condensation of silicon species in the mesoporous molecular sieve framework is not complete, and there are a large number of hydroxyl groups on the surface and inside of the pore walls, so their hydrothermal stability is low. In addition, the acidity of pure silica-based mesoporous molecular sieves is very weak. These shortcomings seriously re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02
Inventor 罗永明候昭胤郑小明
Owner ZHEJIANG UNIV