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Gradient composite structure hierarchical pore thin film and preparation method thereof

A composite structure and multi-level pore technology, applied in chemical instruments and methods, silicon compounds, and other chemical processes, can solve the problems of poor crystallinity and continuity of microporous-mesoporous composite films, insufficient characterization of film pore structures, and persuasive problems. Insufficient power and other problems, to achieve the effect of low cost of goods, excellent continuity, and guaranteed continuity

Active Publication Date: 2016-12-07
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, various templating agents compete with each other, and they compete for the source of silicon and aluminum during the reaction process, which is easy to cause phase separation.
The final microporous-mesoporous composite film obtained on the substrate has poor crystallinity and continuity, and more porous defects
Moreover, the current characterization of the film pore structure is not sufficient and convincing
In addition, hierarchically porous films with microporous-macroporous and microporous-mesoporous-macroporous structures are rarely reported.

Method used

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  • Gradient composite structure hierarchical pore thin film and preparation method thereof
  • Gradient composite structure hierarchical pore thin film and preparation method thereof
  • Gradient composite structure hierarchical pore thin film and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0040] 0.0454g Al(NO 3 ) 3 9H 2 O was dissolved in 36g of water, and 3.88ml of analytically pure tetrapropylammonium hydroxide (TPAOH) and 2.7ml of analytically pure tetraethyl ammonium hydroxide (TEOS) were added successively, and stirred at room temperature for 24h to obtain a solution; the solution was transferred to In a 100ml reaction kettle, vertically immerse the aluminum substrate in the solution, react at 175°C for 4 hours, then cool to room temperature, and then take out the substrate on which the molecular sieve membrane was grown, to obtain the ZSM-5 microporous layer / aluminum substrate.

[0041] First 0.52g of analytically pure F127 (EO 106 PO 70 EO 106 ) was completely dissolved in 20ml of absolute ethanol, marked as 1# solution; 2.225ml of analytically pure TEOS (tetraethyl orthosilicate) was slowly added to 0.21g (1M) hydrochloric acid, 1.455g H 2 O and 10ml of ethanol in a mixed solution, reflux at 70°C for 1h, marked as 2# solution. Then slowly add 1# s...

Embodiment 2

[0048] 0.0454g Al(NO 3 ) 3 9H 2 O was dissolved in 36g of water, and 3.88ml of analytically pure tetrapropylammonium hydroxide (TPAOH) and 2.7ml of analytically pure tetraethyl ammonium hydroxide (TEOS) were added successively, and stirred at room temperature for 24h to obtain a solution; the solution was transferred to In a 100ml reaction kettle, vertically immerse the aluminum substrate in the solution, react at 175°C for 4 hours, then cool to room temperature, and then take out the substrate on which the molecular sieve membrane was grown, to obtain the ZSM-5 microporous layer / aluminum substrate.

[0049] First 0.52g of analytically pure F127 (EO 106 PO 70 EO 106 ) was completely dissolved in 20ml of absolute ethanol, marked as 1# solution; 2.225ml of analytically pure TEOS (tetraethyl orthosilicate) was slowly added to 0.21g (1M) hydrochloric acid, 1.455g H 2 O and 10ml of ethanol in a mixed solution, reflux at 70°C for 1h, marked as 2# solution. Then slowly add 1# s...

Embodiment 3

[0053] 0.0454g Al(NO 3 ) 3 9H 2 O was dissolved in 36g of water, and 3.88ml of analytically pure TPAOH (tetrapropylammonium hydroxide) and 2.7ml of analytically pure TEOS (tetraethylorthosilicate) were added successively, and stirred at room temperature for 24h. The solution was transferred to a 100ml reaction kettle, the aluminum substrate was vertically immersed in the solution, and reacted at 175°C for 4h. After cooling to room temperature, the substrate on which the molecular sieve membrane is grown is taken out to obtain the ZSM-5 microporous layer / aluminum substrate.

[0054] Fix the ZSM-5 microporous layer / aluminum substrate on the jig of the coating puller, assemble the PS colloidal crystal array on its surface, and the PS emulsion concentration is 5wt%. Set the coating program: the dipping / pulling speed is 50mm / min, the dipping time is 3min, and the coating is done once. The samples were dried at 30°C for 1 h.

[0055] 0.52g F127 (EO 106 PO 70 EO 106 ) was com...

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Abstract

The invention provides a gradient composite structure hierarchical pore thin film and a preparation method thereof. The thin film is a hierarchical pore thin film in a micropore / mesopore system and has the micropore / mesopore system or a micropore / macropore system or a micropore / mesopore / macropore system. The preparation method of the thin film includes the steps that a mesopore layer with a three-dimensional pore canal is deposited on the surface of a micropore layer, a sample of a micropore / macropore structure is obtained, or a macropore layer with an open pore canal is deposited on the surface of the micropore layer, and a sample of a micropore / macropore structure is obtained, or multiple mesopore layers and macropore layers are deposited on the surface of the micropore layer sequentially, and a sample of a micropore / mesopore / macropore gradient pore structure is obtained. The thin film sample of the gradient pore structure is put in an atmosphere oven, all templates are removed through one-step calcination, a metal base plate is removed through soaking of low-concentration inorganic acid, and the gradient composite structure hierarchical pore thin film is obtained. Operation is easy and convenient, the production period is short, the application range of products is wide, and the thin film is used for the field of catalytic cracking of heavy oil and residual oil and the separation field such as sea water desalination.

Description

technical field [0001] The invention belongs to the technical field of hierarchical porous films, and in particular relates to a preparation method of a hierarchically porous film with a gradient composite structure. Background technique [0002] Hierarchical porous films have multiple pore structures, and their microporous structures have more acidic sites, which can effectively carry out catalytic reactions; while their mesoporous or macroporous channels are conducive to accelerating the molecular diffusion rate. In addition, the introduction of Al atoms in the mesoporous or macroporous structure makes it surface acidic, which further improves the catalytic performance. It has strong application potential and broad application prospects in the fields of adsorption, separation and catalysis. [0003] There are very few hierarchically porous films reported so far, especially those containing microporous structures. However, since the pore size of micropores is on the order...

Claims

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Application Information

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IPC IPC(8): B01J20/16B01J20/32B01J29/40C02F1/28C10G11/05
CPCB01J20/103B01J20/16C10G11/05C02F1/281B01J20/3234B01J29/40C02F2103/08B01J35/59
Inventor 罗国强鄢凤麟张联盟黄静阳晓宇张建沈强
Owner WUHAN UNIV OF TECH
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