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Preparation method of metal palladium loaded type SiO2 composite membrane

A supported, composite membrane technology, applied in chemical instruments and methods, membranes, membrane technologies, etc., can solve the problems of difficulty in increasing gas permeation rate and separation factor at the same time, so as to improve water vapor stability, improve separation selectivity, The effect of increasing the penetration rate

Inactive Publication Date: 2016-04-20
XI'AN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of metal palladium loading type SiO 2 The preparation method of the composite film solves the problem of existing common SiO 2 It is difficult to improve the gas permeation rate and separation factor of the membrane at the same time

Method used

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  • Preparation method of metal palladium loaded type SiO2 composite membrane
  • Preparation method of metal palladium loaded type SiO2 composite membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Step 1, fully mix ethyl orthosilicate, methyltriethoxysilane and absolute ethanol to form a homogeneous solution, place it in an ice-water mixture, add water and HCl with a concentration of 1.0mol / L while stirring The mixture was stirred and refluxed at 60 °C for 3 h and then cooled to obtain methylated SiO 2 Sol; wherein the molar ratio of ethyl orthosilicate (TEOS), methyltriethoxysilane (MTES), absolute ethanol (EtOH), water, and HCl is 1:0.81:7.7:7.3:0.086;

[0031] Step 2, to the methylation modified SiO obtained in step 1 2 Add N,N-dimethylformamide (the addition amount of N,N-dimethylformamide is methylated modified SiO 2 30% of the volume of the sol), stirred vigorously for 45min, and then pressed PdCl 2 The molar ratio to tetraethyl orthosilicate is 0.08:1, while stirring, add PdCl with a concentration of 0.14mol / L 2 solution and a mixture of absolute ethanol (N,N-dimethylformamide, PdCl 2 The sum of the volumes of the solution and absolute ethanol is methy...

Embodiment 2

[0035] Step 1, thoroughly mix ethyl orthosilicate, methyltriethoxysilane and absolute ethanol to form a homogeneous solution, place it in an ice-water mixture, add water and HCl with a concentration of 1.5mol / L while stirring The mixture was stirred and refluxed at 65 °C for 2.5 h and then cooled to obtain methylated SiO 2 Sol; wherein the molar ratio of ethyl orthosilicate (TEOS), methyltriethoxysilane (MTES), absolute ethanol (EtOH), water, and HCl is 1:0.9:8.3:7.6:0.10;

[0036] Step 2, to the methylation modified SiO obtained in step 1 2 Add N,N-dimethylformamide (the addition amount of N,N-dimethylformamide is methylated modified SiO 2 35% of the volume of the sol), stirred vigorously for 50min, and then pressed PdCl 2 The molar ratio to tetraethyl orthosilicate is 0.065:1, while stirring, add PdCl with a concentration of 0.14mol / L 2 solution and a mixture of absolute ethanol (N,N-dimethylformamide, PdCl 2 The sum of the volumes of the solution and absolute ethanol is...

Embodiment 3

[0040] Step 1, thoroughly mix ethyl orthosilicate, methyltriethoxysilane and absolute ethanol to form a homogeneous solution, place it in an ice-water mixture, add water and HCl with a concentration of 2.0mol / L while stirring The mixture was stirred and refluxed at 70 °C for 2 h and then cooled to obtain methylated SiO 2 Sol; wherein the molar ratio of ethyl orthosilicate (TEOS), methyltriethoxysilane (MTES), absolute ethanol (EtOH), water, and HCl is 1:1.0:9.0:8.0:0.12;

[0041] Step 2, to the methylation modified SiO obtained in step 1 2 Add N,N-dimethylformamide (the addition amount of N,N-dimethylformamide is methylated modified SiO 2 40% of the volume of the sol), stirred vigorously for 60min, and then pressed PdCl 2 The molar ratio to tetraethyl orthosilicate is 0.05:1, while stirring, add PdCl with a concentration of 0.14mol / L 2 solution and a mixture of absolute ethanol (N,N-dimethylformamide, PdCl 2 The sum of the volumes of the solution and absolute ethanol is me...

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Abstract

The invention provides a preparation method of a metal palladium loaded type SiO2 composite membrane. The method comprises the steps that tetraethoxysilane, methyl triethoxysilane and absolute ethyl alcohol are sufficiently mixed to be a homogeneous solution, the homogeneous solution is put into an ice-water mixture, water and HCl are added when stirring is conducted, cooling is conducted after stirring and refluxing are conducted, and methylation modified SiO2 sol is obtained; N,N-dimethyl formamide is added, stirring is conducted, a PdCl2 solution and absolute ethyl alcohol are added when stirring is conducted, stirring is conducted continuously, and Pd / SiO2 sol is obtained; porous alpha-Al2O3 ceramic serves as a supporting body, the surface of the supporting body is coated with the Pd / SiO2 sol through an impregnation method, and drying and calcining are conducted; the third step is repeated, and the metal palladium loaded type SiO2 composite membrane is obtained. According to the prepared metal palladium loaded type SiO2 composite membrane, high permeation flux of a traditional porous membrane can be reserved, the separation selectivity of H2 can be improved, and the purpose of increasing the permeation rate of H2 and the H2 / CO2 separation factor on the basis of improving the water vapor stability of the SiO2 membrane is achieved.

Description

technical field [0001] The invention belongs to the technical field of gas separation, in particular to a metal palladium-loaded SiO 2 Preparation method of composite membrane. Background technique [0002] As we all know, 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. while H 2 It is a clean energy with great development prospects. 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 high-concentration CO 2 Transported to designated locations for storage to reduce greenhouse gas CO 2 emissions. In the process of coal gasification hydrogen production, coal is generally converted into coal gas (H 2 +CO), however, in order to facilitate more separation of C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D69/12B01D67/00B01D71/02
CPCB01D67/0039B01D69/12B01D71/027B01D2323/46
Inventor 杨靖李淋钰同帜侯海云郭雅妮赵亚梅
Owner XI'AN POLYTECHNIC UNIVERSITY
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