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Preparation method of metal doped organic-inorganic composite SiO2 film

A metal doping, inorganic composite technology, applied in separation methods, chemical instruments and methods, membrane technology, etc., can solve the problem of insignificant separation effect, and achieve the effect of excellent separation performance and excellent water vapor stability.

Active Publication Date: 2010-10-13
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

where H 2 / CO 2 The separation factor is only 5.5, which is slightly higher than the ideal separation factor (4.7) of Knudsen diffusion, and the separation effect is not obvious

Method used

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  • Preparation method of metal doped organic-inorganic composite SiO2 film
  • Preparation method of metal doped organic-inorganic composite SiO2 film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1, with BTESE and Nb (OC 4 h 9 ) 5 Nb-doped organic-inorganic composite SiO as precursor 2 Preparation of Membrane Nb-BTESE

[0020] Mix 5ml of BTESE and 30ml of absolute ethanol and place in an ice bath at 0°C, add 0.6ml, 1mol / l HCl solution to it under stirring conditions, stir and mix evenly, and place in a constant temperature water bath at 60°C, After reacting for 1.5 hours, take it out and place it in an ice bath at 0°C, add 7ml of Nb(OC 4 h 9 ) 5 and 35ml of absolute ethanol, after mixing evenly, continue to add 0.6ml of 1mol / l HCl solution, and then react in a constant temperature water bath at 60°C for 1.5 hours. After the reaction, a transparent Nb-doped organic-inorganic composite SiO was obtained 2 Sol. Store it at -20°C until use. Mix the sol and absolute ethanol at a volume ratio of 1:8 to obtain a film-forming solution, and place the film-forming solution in a sheet-shaped γ-Al 2 o 3 Membrane surface coating, natural dried flake Nb-d...

Embodiment 2

[0023] Embodiment 2, with tetraethyl orthosilicate (TEOS) and tetraethyl titanate (Ti(OC 2 h 5 ) 4 ) as the precursor of Ti-doped organic-inorganic composite SiO 2 Preparation of Membrane Ti-TEOS

[0024] Mix 10ml TEOS and 20ml butanol in an ice bath at -10°C, add 1.8ml, 1.5mol / l HNO3 solution to it under stirring, stir and mix evenly, then place in a constant temperature water bath at 70°C , after reacting for 2 hours, take it out and place it in an ice bath at -10°C, add 2ml Ti(OC 2 h 5 ) 4 and 20ml of ethanol, after mixing evenly, continue to add 1.8ml, 1.5mol / l of HNO 3 solution, and then reacted in a constant temperature water bath at 70°C for 2 hours. After the reaction, a transparent Ti-doped organic-inorganic composite SiO was obtained. 2 Sol. Store it at -20°C until use. The sol and butanol were mixed at a volume ratio of 1:10 to obtain a film-forming solution, and the film-forming solution was placed in the flake TiO 2 Membrane surface coating, naturally d...

Embodiment 3

[0025] Example 3, using 1,2-bis(triethoxysilyl)methane (BTESM) as a precursor to incorporate Co(NO 3 )·6H 2 Preparation of Co-doped organic-inorganic composite SiO by O 2 Membrane Co-BTESM

[0026] Mix 5ml of BTESM and 45ml of methanol in an ice bath at -20°C, and add 6ml of 0.5mol / l H 2 SO 4 solution, stirred and mixed evenly, placed in a constant temperature water bath at 55°C, reacted for 1 hour, took it out and placed it in an ice bath at -20°C, added 15.7g Co(NO 3 )·6H 2 O and 60ml of ethanol, after mixing evenly, continue to add 6ml, 0.5mol / l of H 2 SO 4 solution, and then reacted in a constant temperature water bath at 55°C for 1 hour. After the reaction, a Co-doped organic-inorganic composite SiO with a transparent appearance was obtained. 2 Sol. Store it at -20°C until use. The sol and methanol were mixed at a volume ratio of 1:3 to obtain a film-forming solution, and the film-forming solution was placed in a sheet of ZrO 2 Membrane surface coating, natural...

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Abstract

The invention relates to a preparation method of a metal doped organic-inorganic composite SiO2 film, which is characterized by using siloxane as a precursor, carrying out hydrolysis under acid catalysis, adding ethanol solution of salt (alkoxide or nitrate) containing metal M into ice bath to synthesize metal doped organic-inorganic composite SiO2 sol, after film coating and drying, obtaining the metal doped organic-inorganic composite SiO2 film through firing under inert atmosphere. The composite SiO2 film effectively solves the problem of efficient separation of H2(He) / CO2 in the industrial gases (H2, CO2, O2, N2, CH4 and CO) and obviously improves the separation effect of H2(He) / CO2 through double effects of molecular sieving mechanism and adsorption. The composite SiO2 film has good application prospects in such environments containing water vapor and various mixed gases (H2, CO2, CO and CH4) as water gas shift reaction, methane steam reforming reaction and the like.

Description

Technical field: [0001] The invention relates to a metal-doped organic-inorganic composite SiO 2 Membrane preparation method, especially related to the H 2 (He) / CO 2 Metal-doped modified organic-inorganic composite SiO in the field of gas separation 2 Membrane preparation method. The composite SiO 2 Membranes will have broad application prospects in large-scale industrial applications, such as methane steam reforming reaction, water gas shift reaction and so on. Background technique: [0002] At present, due to the pressure of global warming, the international 2 More and more attention has been paid to the issue of emissions. While saving energy and reducing emissions, how to deal with the emitted CO 2 Capture and storage is one of the hotspots in the current chemical industry. Currently commonly used CO 2 Capture technologies include chemical absorption, physical adsorption, etc., but all of them have some shortcomings. Membrane separation is a very promising gas s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D69/12B01D71/02B01D71/06B01D53/22
Inventor 漆虹韩静邢卫红范益群徐南平
Owner NANJING UNIV OF TECH
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