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Preparation method of nano hierarchical pore Beta molecular sieve

A molecular sieve, multi-level pore technology, applied in molecular sieve catalyst, nanotechnology, nanotechnology and other directions, can solve problems such as ineffective utilization, and achieve the effect of simplifying synthesis steps and reducing costs

Active Publication Date: 2021-04-09
JILIN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, the product is in an aggregated state due to the condensation of solid raw materials, which makes the micropores of Beta molecular sieves unable to be effectively utilized in catalytic applications.

Method used

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  • Preparation method of nano hierarchical pore Beta molecular sieve
  • Preparation method of nano hierarchical pore Beta molecular sieve
  • Preparation method of nano hierarchical pore Beta molecular sieve

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preparation example Construction

[0040] The invention provides a kind of preparation method of nanometer hierarchical porous Beta molecular sieve, comprises the following steps:

[0041] (1) Silicon source, aluminum source, inorganic base, templating agent, Beta crystal seed and water are carried out ball milling and mixing, obtain solid-phase reaction mixture; The consumption of described silicon source, aluminum source and inorganic base is represented by SiO 2 、Al 2 o 3 and Na 2 O content meter, the SiO 2 、Al 2 o 3 、Na 2 O, the molar ratio of template agent and water is 1: (0.0083~0.05): (0.113~0.168): (0.28~0.40): (1.5~3);

[0042] (2) The solid-phase reaction mixture and water are separated and placed in a reaction kettle, and a steam-assisted crystallization reaction is performed to obtain a molecular sieve precursor; the temperature of the steam-assisted crystallization reaction is 140°C, and the time is 24-72h ;

[0043] (3) Calcining the molecular sieve precursor to obtain a nano-hierarchical...

Embodiment 1

[0060] Weigh 0.5g of solid silica gel, 0.495g of tetraethylammonium bromide, 0.068g of sodium hydroxide, 0.052g of sodium aluminate, 0.05g of seed crystals and 0.45g of deionized water as solid-phase raw materials, and add them to ball mills for 5 hours Finally, the solid-phase reaction mixture was obtained; 0.5g of the solid-phase reaction mixture was weighed and packed into a 5mL polytetrafluoroethylene liner, and then embedded in a 50mL reactor with 1g of deionized water at the bottom, at 140°C Steam assisted crystallization for 72 hours. After the crystallization was completed, the product was centrifugally washed with deionized water until neutral, then dried at 60°C for 12 hours, and finally calcined at 550°C under air conditions for 6 hours to obtain a Beta molecular sieve, which was designated as sample Beta -1.

[0061] The solid silica gel is purchased from Qingdao Ocean Chemical Co., Ltd., and the molar ratio of each raw material in the solid-phase reaction mixture ...

Embodiment 2

[0063] Weigh 0.5g of solid silica gel, 0.495g of tetraethylammonium bromide, 0.068g of sodium hydroxide, 0.052g of sodium aluminate, 0.05g of seed crystals and 0.225g of deionized water as solid-phase raw materials, and add them to ball mills for 5 hours Finally, the solid-phase reaction mixture was obtained; 0.5g of the solid-phase reaction mixture was weighed and packed into a 5mL polytetrafluoroethylene liner, and then embedded in a 50mL reactor with 2g of deionized water at the bottom, at 140°C Steam assisted crystallization for 72 hours. After the crystallization was completed, the product was centrifugally washed with deionized water until neutral, then dried at 60°C for 12 hours, and finally calcined at 550°C under air conditions for 6 hours to obtain a Beta molecular sieve, which was designated as sample Beta -2.

[0064] The solid silica gel is purchased from Qingdao Ocean Chemical Co., Ltd., and the molar ratio of each raw material in the solid-phase reaction mixture...

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Abstract

The invention provides a preparation method of a nano hierarchical pore Beta molecular sieve, and belongs to the technical field of preparation of Beta molecular sieves. Compared with an existing steam-assisted xerogel conversion method for preparing the Beta molecular sieve, the method has the advantages that the process of obtaining xerogel through evaporation of synthetic gel is avoided, a solid-phase reaction mixture obtained after raw materials such as tetraethylammonium bromide and solid silica gel are subjected to ball milling is directly used for steam-assisted conversion, the synthesis steps are simplified, and the synthesis cost is reduced; meanwhile, due to the existence of the steam, the migration and dispersion of the solid-phase raw material are promoted, so that the nano hierarchical pore Beta molecular sieve with relatively small and dispersed nano particles and rich intracrystalline mesopores is prepared.

Description

technical field [0001] The invention relates to the technical field of preparation of Beta molecular sieves, in particular to a preparation method of nanometer hierarchically porous Beta molecular sieves. Background technique [0002] Beta molecular sieves are widely used in industrial catalysis, adsorption separation and biomass conversion due to their unique pore structure, high specific surface area, good thermal stability and hydrothermal stability. The traditional method of synthesizing Beta molecular sieve is hydrothermal synthesis (hydrothermal synthesis). This method needs to use a large amount of water as a solvent. The reaction process will generate high pressure and produce a large amount of strong alkali waste liquid, polluting the environment. In 1996, M.Matsukata applied the dry gel conversion technology (dry gel conversion) to the synthesis of Beta molecular sieves for the first time. The method is characterized by evaporating the water in the synthetic hydrog...

Claims

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Application Information

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IPC IPC(8): C01B39/04B01J29/70B82Y30/00B82Y40/00
CPCC01B39/04B82Y30/00B82Y40/00B01J29/7007C01P2002/72C01P2004/04C01P2004/03C01P2004/50C01P2004/62C01P2004/64C01P2006/12C01P2006/14
Inventor 于吉红马哲张强闫文付
Owner JILIN UNIV
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