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Method for preparing nano molecular sieve by coordinating amino acid assisting and sectional crystallizing through concentrated gel system

A technology of nano-molecular sieve and segmental crystallization, which is applied in chemical instruments and methods, molecular sieves and alkali-exchange compounds, nanotechnology for materials and surface science, etc., can solve problems of low crystallinity, complex and changeable control factors, poor Dispersion and other issues, to achieve good crystallization, improve safety and reliability, and good monodispersity

Inactive Publication Date: 2017-06-30
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These controlling factors are complex and changeable, and the synthesis conditions of nano-molecular sieves with different topological structures are different, and the synthesized nano-molecular sieves have low crystallinity and poor dispersion.

Method used

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  • Method for preparing nano molecular sieve by coordinating amino acid assisting and sectional crystallizing through concentrated gel system
  • Method for preparing nano molecular sieve by coordinating amino acid assisting and sectional crystallizing through concentrated gel system
  • Method for preparing nano molecular sieve by coordinating amino acid assisting and sectional crystallizing through concentrated gel system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] This example presents nano-Silicalite-1 molecular sieves. Under the concentrated gel system, the method of synergistically preparing nano-molecular sieves through amino acid assistance and segmented crystallization is adopted:

[0037] Disperse 1.819g ethyl orthosilicate and 3.197g tetrapropylammonium hydroxide aqueous solution (the mass fraction of tetrapropylammonium hydroxide solute is 25%) in 3g deionized water, and stir evenly at room temperature for 3 hours until the orthosilicic acid Ethyl ester is completely hydrolyzed; then add 0.13g lysine, stir for 10min to disperse evenly, then follow the molar ratio of 9H 2 O: 1SiO 2 The excess water was evaporated under an infrared oven lamp to obtain a transparent initial gel of Silicalite-1, which was placed in a stainless steel reactor with a polytetrafluoroethylene liner, crystallized in an oven at 60°C for 48 hours, and then moved to Continue to crystallize in an oven at 170°C for 24 hours. After the crystallization ...

Embodiment 2

[0043] This example presents nano-Silicalite-1 molecular sieves. Under the concentrated gel system, the method of synergistically preparing nano-molecular sieves through amino acid assistance and segmented crystallization is adopted:

[0044] Disperse 1.819g tetrapropylammonium hydroxide solution and 3.197g tetrapropylammonium hydroxide solution (tetrapropylammonium hydroxide solute mass fraction is 25%) in 3g deionized water, and stir evenly at room temperature for 3 hours to reach tetrapropylammonium hydroxide solution. The ester is completely hydrolyzed; then add 0.13g of lysine, stir for 10min until the dispersion is uniform, then follow the molar ratio of 9H 2 O: 1SiO 2 The excess water was evaporated under an infrared oven lamp to obtain a transparent initial gel of Silicalite-1, which was placed in a stainless steel reactor with a polytetrafluoroethylene liner, crystallized in an oven at 80 °C for 24 hours, and then moved to The crystallization was continued in an oven...

Embodiment 3

[0049] In this example, nano-beta molecular sieves are given. Under the concentrated gel system, the method of synergistically preparing nano-molecular sieves through amino acid assistance and segmental crystallization is adopted:

[0050] Disperse 1.819g ethyl orthosilicate and 2.78g tetraethylammonium hydroxide (the mass fraction of tetraethylammonium hydroxide is 25%) in 3g of deionized, and stir uniformly at room temperature for 3 hours until the ethyl orthosilicate is completely Hydrolyze to obtain solution A; 0.1g sodium metaaluminate (wherein Al 2 o 3 The content is 0.042g) mixed with 0.01g sodium hydroxide and 1g water and ultrasonically dissolved to obtain solution B; slowly add solution B to solution A, and at the same time add 0.13g lysine to solution A, stir for 2 hours until uniform , according to the molar ratio 6H 2 O: 1SiO 2 The excess water was evaporated and removed under the infrared oven lamp to obtain the initial gel of Beta molecular sieve; it was put ...

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Abstract

The invention provides a method for a preparing nano molecular sieve by coordinating amino acid assisting and sectional crystallizing through a concentrated gel system, and belongs to the technical field of molecular sieve preparation. The method is characterized in that a traditional hydro-thermal synthesis mode is carried out; tetrapropylammonium hydroxide or tetraethylammonium hydroxide or Na<+> is used as a template; amino acid is added to control crystal nucleation and growth of the molecular sieve, and the sectional crystallizing reaction is carried out through the concentrated gel system, so that the synthesized nano molecular sieve is good in crystal, high in micropore specific surface area, high in external specific surface area and large in micropore volume; the synthesized Beta type molecular sieve is 9.5 nm in average size; an Silicalite-1 type molecular sieve is 30nm in average size; an A type molecular sieve is 50nm in average size. The nano molecular sieve is high in crystalline and monodispersity, and has a certain industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve preparation, and in particular relates to a method for synergistically preparing nanometer molecular sieves through amino acid assistance and segmented crystallization in a concentrated gel system. Background technique [0002] Since the 1950s, nano-molecular sieves have gradually attracted everyone's attention. Due to their large external specific surface area, good thermal stability, more exposed active sites, and fast diffusion and mass transfer rates, they It has shown excellent properties and applications in the fields of catalysis, ion exchange, sensors, optical devices and biomedicine. Since molecular sieve research is closely related to industrial development, the exploration of new synthetic routes of nano molecular sieves has become the focus of modern scientists. There are many factors and methods controlling the synthesis of nano-molecular sieves, such as: (1) addition of orga...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48B82Y30/00B82Y40/00C01B39/14
CPCC01B39/48C01B39/14C01P2002/01C01P2002/72C01P2004/64C01P2006/12C01P2006/14
Inventor 于吉红张强
Owner JILIN UNIV
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