Molecular sieve nanotube aerogel and preparation method thereof

A molecular sieve and airgel technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of long molecular diffusion path, uncontrollable mesopore and macropore diameter, and numerous steps , to achieve the effect of shortening the molecular diffusion path, facilitating the catalysis of macromolecules, and reducing production costs

Inactive Publication Date: 2014-08-13
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has many steps, the pore size of mesopores and macropores cannot be adjusted, and the molecular diffusion path is long.

Method used

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  • Molecular sieve nanotube aerogel and preparation method thereof
  • Molecular sieve nanotube aerogel and preparation method thereof
  • Molecular sieve nanotube aerogel and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Example 1: Preparation of Silicalite-1 molecular sieve nanotube airgel

[0067] (1) Preparation of precursor: Add 0.01g of cetylmethylammonium bromide (CTAB) to 10ml of ethanol solution, stir to dissolve at room temperature, add 1ml of tetraethyl orthosilicate and stir to dissolve, then add cellulose Airgel 0.01g, stir at room temperature to make the airgel fully swell and become translucent, add 1ml of ammonia water, stir at room temperature for 2 hours, at this time the soft translucent massive airgel turns into hard and slightly elastic white gas Gel blocks. After being taken out by filtration, it was washed three times with ethanol and dried in an oven at 30°C. Scanning electron microscope image of nanocellulose airgel figure 1 As shown, the cellulose filaments with a diameter of about 20 nm are cross-linked to form a network-like structure. The scanning electron microscope image of the precursor is shown in figure 2 As shown, amorphous silicon dioxide is evenl...

Embodiment 2

[0071] Example 2: Preparation of Silicalite-1 molecular sieve nanotube airgel

[0072] (1) Preparation of precursor: Add 0.2g CTAB to 10ml tert-butanol solution, stir to dissolve with slight heat, add 2.5ml of ammonia water and stir to dissolve, add 0.03g of cellulose airgel, stir at room temperature to make the air coagulate The gel is fully swollen and becomes translucent. Add 5ml of tetraethyl orthosilicate and stir at room temperature for 6 hours. At this time, the soft and translucent block-shaped airgel becomes a hard and slightly elastic white airgel block. After being taken out by filtration, it was washed five times with ethanol, and dried in an oven at 100°C. The scanning electron microscope of the precursor as Figure 10 As shown, the amorphous silica is evenly coated on the outer layer of the cross-linked cellulose filaments to form nanotubes with a wall thickness of about 80 nm, and the nanotubes are cross-linked to form a network skeleton.

[0073] (2) Preparat...

Embodiment 3

[0076] Embodiment 3: Preparation of Silicalite-1 molecular sieve nanotube airgel

[0077] (1) Preparation of precursor: Add 1g CTAB to 10ml ethanol solution, stir to dissolve with slight heat, add 7ml of propyl orthosilicate and stir to dissolve, add 0.05g of cellulose airgel, stir at room temperature to make the air coagulate The glue is fully swollen and becomes translucent. Add 5ml of ammonia water and stir at room temperature for 24 hours. The subsequent operation steps are the same as in Example 2 (1).

[0078] (2) Preparation of Silicalite-1 seed liquid: Add 16g of ethyl orthosilicate to 27ml of tetrapropylammonium hydroxide solution, stir at room temperature for 24h, then put the above mixed solution into a flask, and reflux at 90°C After heating for 96 hours, the obtained seed crystal solution was ultracentrifuged at 12000 rpm for 20 minutes, the supernatant liquid was discarded to take the lower solid seed crystal, and then dispersed into distilled water to form a col...

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Abstract

The invention relates to a molecular sieve nanotube aerogel as well as a preparation method thereof and belongs to the technical field of the preparation of a molecular sieve. The inner diameter of the molecular sieve nanotubes is adjustable within a range of 50nm to 100nm and the outer diameter of the molecular sieve nanotubes is adjustable within the range of 170nm to 400nm. The molecular sieve nanotubes are symbiotically built of molecular sieve nanocrystals and have firm and stable structure; and the nanotubes are crosslinked and communicated to form a network skeleton. A macropore of which the diameter is 1-20mu m is defined by the crosslinked molecular sieve nanotubes, the molecular sieve nanotubes have the same structural characteristics as micropore-mesopore-macropore-nanotubes. The different macroscopical morphologies of the molecular sieve nanotubes, such as zero dimensional particle, two-dimensional films, and three-dimensional block can be self-formed and have a very low density of 0.15-0.25g / cm3 and a high porosity of 85-95%. The preparation method disclosed by the invention is applied to silica-alumina and heteroatom silica-alumina molecular sieves, such as Silicalite-1, ZSM-5, TS-1, X, Y and A.

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 inorganic silicon salt with regular micropore structure (2.0nm), which has good thermal stability and high specific surface area, and is widely used in important industrial fields such as ion exchange, petroleum cracking, adsorption separation, and biomedicine [Chem . Rev. 1997, 97, 2373-2419.]. While the micropores of molecular sieves provide reactive active sites, their pore size also limits the diffusion of macromolecules in the pores. Molecules with a kinetic diameter greater than 2.0nm cannot diffuse into the micropores, which greatly reduces the number of effective active sites. , reducing the use efficiency of molecular sieve catalysts. At the same time, becaus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02B82Y30/00B82Y40/00
Inventor 徐雁李冠楠黄海波李守贵
Owner JILIN UNIV
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