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A kind of molecular sieve nanotube airgel and preparation method thereof

A molecular sieve and aerogel technology, applied in the field of molecular sieve nanotube aerogel and its preparation, can solve the problems of uncontrollable mesopore and macropore pore size, long molecular diffusion path, etc. Molecular diffusion path, the effect of prolonging the service life

Active Publication Date: 2016-06-08
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the pore size of mesopores and macropores cannot be adjusted and the molecular diffusion path is long.

Method used

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  • A kind of molecular sieve nanotube airgel and preparation method thereof
  • A kind of molecular sieve nanotube airgel and preparation method thereof
  • A kind of molecular sieve nanotube airgel and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] Example 1: Preparation of Silicalite-1 molecular sieve nanotube airgel

[0070] Step 1: Add 0.01g CTAB to 50mL of absolute ethanol, stir magnetically at room temperature to dissolve, add 1mL tetraethyl silicate and stir to dissolve, then add 0.01g cellulose airgel, stir at room temperature to fully swell the airgel It is translucent, add 1mL of ammonia water, and stir at room temperature for 2h, at this time the soft translucent airgel turns into a hard and slightly elastic white block. After being taken out by filtration, it was washed three times with ethanol, and dried in an oven at 30°C to obtain a cellulose / silicon dioxide precursor, which was used as a silicon source for crystallized molecular sieves. Scanning electron microscope image of cellulose airgel figure 1 As shown, the cellulose nanofibers with an average diameter of about 32 nm were cross-linked to form a three-dimensional network structure. SEM image of cellulose / silica precursor as shown in figure ...

Embodiment 2

[0075] Example 2: Preparation of Silicalite-1 molecular sieve nanotube airgel

[0076] Step 1: Add 0.2g CTAB to 50mL tert-butanol, stir to dissolve with slight heat, add 5mL tetraethyl silicate and stir evenly, add 0.03g cellulose airgel, stir at room temperature to make the airgel fully swell In the translucent state, add 2.5mL of ammonia water and stir at room temperature for 6h. At this time, the soft and translucent airgel becomes hard and slightly elastic white aerogel. After being taken out by filtration, it was washed five times with ethanol, and dried in an oven at 100°C to obtain a cellulose / silicon dioxide precursor, which was used as a silicon source for crystallized molecular sieves.

[0077]Step 2: Add 18g of tetraethyl silicate to 28mL of tetrapropylammonium hydroxide solution, stir at room temperature for 24h, then put the above mixed solution into a flask, heat at reflux at 80°C for 96h, and dilute the obtained seed liquid Ultracentrifuge at 12000rpm for 20min...

Embodiment 3

[0081] Embodiment 3: Preparation of Silicalite-1 molecular sieve nanotube airgel

[0082] Step 1: Add 1g of CTAB to 50mL of absolute ethanol, stir to dissolve with slight heat, add 7mL of tetrapropyl silicate and stir to dissolve, then add 0.05g of cellulose airgel, stir at room temperature to fully swell the airgel to half In a transparent state, add 5.0 mL of ammonia water and stir at room temperature for 24 hours. The subsequent operation steps are the same as step 1 of Example 2 to obtain a cellulose / silicon dioxide precursor as a silicon source for crystallized molecular sieves.

[0083] Step 2: Add 16g of tetraethyl silicate to 27mL of tetrapropylammonium hydroxide solution, stir at room temperature for 24h, then put the above mixed solution into a flask, heat at reflux at 90°C for 96h, and dissolve the obtained seed liquid Ultracentrifuge at 12000rpm for 20min, discard the supernatant to take the lower layer of solid seed, and then disperse it into distilled water to fo...

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Abstract

The invention relates to molecular-sieve nanotube aerogel and a preparation method thereof, and belongs to the technical field of molecular sieve preparation. The molecular-sieve nanotube has the tube internal diameter adjustable in the scope of 50-100 nm and has the tube wall thickness adjustable in the scope of 60-120 nm. The molecular-sieve nanotube is formed by intergrowth construction of molecular sieve nanometer crystal grains and is firm and stable in structure. The meso pore is formed by accumulation of molecular sieve nanometer crystal grains, and a network framework is formed by crosslinking of nanotubes. A macropore of 0.5-20 mu m is enclosed through crosslinking of molecular sieve nanotubes, the molecular-sieve nanotube aerogel has the structure characteristic of macropore-nanotube-mesopore-micropore communication, can form a sphere, a membrane, a block and other space forms, has the extremely low density of 0.15-0.25 g / cm<3> and the high porosity of 85-95%, is applicable to silicon-aluminium molecular sieve and heteroatom-silicon-aluminium molecular sieves, such as Silicalite-1, ZSM-5, TS-1, Y, A molecular sieve and the like.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve preparation, and in particular relates to a molecular sieve nanotube aerogel formed by cross-linking molecular sieve nanotubes and a preparation method thereof. Background technique [0002] Molecular sieve is a crystalline aluminosilicate with regular microporous structure (pore diameter is usually 0.5-1.2nm), which has excellent acidity, thermal stability, hydrothermal stability and high specific surface area, and is widely used in petroleum refining , fine chemical industry, ion exchange, adsorption separation and biomedicine and other important industrial fields [Chem.Rev.1997,97,2373-2419.]. The microporous structure of the molecular sieve not only endows it with shape-selective catalytic performance, but also limits the entry and diffusion of molecules with a kinetic diameter greater than 1.0 nm, reducing the use efficiency of the molecular sieve catalyst. Due to the slow diffusion ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
CPCC01B39/02C01P2004/03C01P2004/04C01P2004/13
Inventor 徐雁李冠楠黄海波李守贵
Owner JILIN UNIV
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