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A pd/ag/sio 2 Preparation method of composite membrane

A composite membrane and mixed liquid technology, applied in separation methods, chemical instruments and methods, membrane technology, etc., can solve the problems of water vapor stability, gas permeation rate and separation factor that are difficult to improve at the same time, so as to improve H2 separation selectivity, Effect of preventing hydrogen embrittlement and increasing penetration rate

Active Publication Date: 2022-04-22
XI'AN POLYTECHNIC UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of this invention is to provide a kind of Pd / Ag / SiO 2 The preparation method of the composite film solves the common SiO existing in the prior art 2 Membrane water vapor stability, gas permeation rate and separation factor are difficult to improve at the same time

Method used

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  • A pd/ag/sio <sub>2</sub> Preparation method of composite membrane
  • A pd/ag/sio <sub>2</sub> Preparation method of composite membrane
  • A pd/ag/sio <sub>2</sub> Preparation method of composite membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] A Pd / Ag / SiO 2 The preparation method of composite film is specifically implemented according to the following steps:

[0062] Step 1, to the HNO of 3mol / L 3 Pd(NO 3 ) 2 2H 2 O, stirred vigorously at 20°C for 8 hours to fully dissolve and obtain 0.6mol / L Pd(NO 3 ) 2 2H 2 O solution;

[0063] Step 2, prepare 1mol / L AgNO 3 solution;

[0064] Step 3: Thoroughly mix ethyl orthosilicate (TEOS), absolute ethanol (EtOH), and N,N-dimethylformamide (DMF) into a homogeneous solution, place it in an ice-water mixture, and add it while stirring Water and HNO at a concentration of 1.5mol / L 3 The mixture was stirred and refluxed at 50 ° C for 5 h and then cooled to obtain SiO 2 Sol; Among them, tetraethyl orthosilicate (TEOS), absolute ethanol (EtOH), water, N, N-dimethylformamide (DMF), HNO 3 The molar ratio is 1:3.5:4:1.5:0.04;

[0065] Step 4, to the SiO obtained in step 3 2 Pd(NO 3 ) 2 2H 2 O, AgNO 3 solution and ethanol mixture (Pd(NO 3 ) 2 2H 2 O, AgNO 3 Th...

Embodiment 2

[0069] A Pd / Ag / SiO 2 The preparation method of composite film is specifically implemented according to the following steps:

[0070] Step 1, to the HNO of 3.5mol / L 3 Pd(NO 3 ) 2 2H 2 O, stirred vigorously at 40°C for 5h to fully dissolve and obtain 0.75mol / L of Pd(NO 3 ) 2 2H 2 O solution;

[0071] Step 2, prepare 1.3mol / L AgNO 3 solution;

[0072] Step 3: Thoroughly mix tetraethyl orthosilicate (TEOS), absolute ethanol (EtOH), and N,N-dimethylformamide (DMF) into a homogeneous solution, place it in an ice-water mixture, and add it while stirring Water and HNO at a concentration of 2.0mol / L 3 The mixture was stirred and refluxed at 65 ° C for 3 h and then cooled to obtain SiO 2 Sol; Among them, tetraethyl orthosilicate (TEOS), absolute ethanol (EtOH), water, N, N-dimethylformamide (DMF), HNO 3 The molar ratio is 1:7:6:2.25:0.07;

[0073] Step 4, to the SiO obtained in step 3 2 Pd(NO 3 ) 2 2H 2 O, AgNO 3 solution and ethanol mixture (Pd(NO 3 ) 2 2H 2 O, AgN...

Embodiment 3

[0077] A kind of Pd / Ag / SiO The preparation method of composite membrane, specifically implement according to the following steps:

[0078] Step 1, to the HNO of 3.8mol / L 3 Pd(NO 3 ) 2 2H 2 O, stirred vigorously at 60°C for 2h to fully dissolve to obtain 0.9mol / L Pd(NO 3 ) 2 2H 2 O solution;

[0079] Step 2, prepare 1.5mol / L AgNO 3 solution;

[0080] Step 3: Thoroughly mix tetraethyl orthosilicate (TEOS), absolute ethanol (EtOH), and N,N-dimethylformamide (DMF) into a homogeneous solution, place it in an ice-water mixture, and add it while stirring Water and HNO at a concentration of 2.0mol / L 3 The mixture was stirred and refluxed at 75°C for 2h and then cooled to obtain SiO 2 Sol; Among them, tetraethyl orthosilicate (TEOS), absolute ethanol (EtOH), water, N, N-dimethylformamide (DMF), HNO 3 The molar ratio is 1:10:8.0:3:0.10;

[0081] Step 4, to the SiO obtained in step 3 2 Pd(NO 3 ) 2 2H 2 O, AgNO 3 solution and ethanol mixture (Pd(NO 3 ) 2 2H 2 O, AgNO ...

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Abstract

The invention discloses a Pd / Ag / SiO 2 The preparation method of the composite membrane is specifically implemented according to the following steps: 1. Prepare 0.6-0.9mol / L of Pd(NO 3 ) 2 2H 2 O solution; 2. Prepare 1‑1.5mol / L AgNO 3 solution; 3. Preparation of SiO 2 sol; 4, Pd(NO 3 ) 2 2H 2 O solution, AgNO 3 Solution and absolute ethanol are mixed to obtain mixed solution 1, which is to methylate modified SiO 2 Add mixed solution 1 to the sol, stir for 40‑60min, and obtain Pd / Ag / SiO 2 sol; 5. With porous ceramics as the support body, the Pd / Ag / SiO 2 The sol is coated on the surface of the support, dipped for 4-10s, dried at room temperature for 3-6 hours, and then roasted; 6. Repeat 1-5 times to obtain Pd / Ag / SiO 2 Composite film.

Description

technical field [0001] The invention belongs to the technical field of gas separation and relates to a Pd / Ag / SiO 2 Preparation method of composite membrane. Background technique [0002] Hydrogen is an efficient and pollution-free clean energy, which is an important direction of future energy development. But hydrogen is not a primary energy source and must be produced in other ways. CO 2 It is the largest greenhouse gas emission, and it is the focus of greenhouse gas reduction and control. CO 2 The main source of emissions is the use of fossil fuels, especially the burning of coal. At present, it has even been proposed in the world to efficiently and intensively convert heavily polluted coal into clean hydrogen for combustion, that is, coal gasification to produce hydrogen, and the separated H 2 for utilization, while the high concentration of CO 2 Transported to designated locations for storage to reduce greenhouse gas CO 2 emissions. In the process of coal gasifi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D69/12B01D67/00B01D71/02B01D53/22C01B3/56
CPCB01D69/12B01D67/0039B01D71/027B01D53/228C01B3/56C01B3/503
Inventor 杨靖袁傲赵亚梅穆瑞花
Owner XI'AN POLYTECHNIC UNIVERSITY
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