Method for preparing CO2 catching membrane material with high hydrothermal stability

A thermally stable and high-performance technology, applied in the field of preparation of CO2 capture membrane materials, can solve the problems of inconspicuous separation effect and achieve good separation performance

Active Publication Date: 2013-01-16
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, foreign research scholars Tsuru use ZrO 2 Ceramic membrane material prepared ZrO 2 Gas separation membrane, the membrane for H 2 The permeation flux of (He) is 3~5×10 -7 mole m -2 ·s -1 ·Pa -1 , however H 2 (He) / CO 2 The ideal separation factor is only 1.2~2.4, which is lower than the separation factor of Knudsen diffusion (4.7), and the separation effect is not obvious
There is no report on ZrO 2 water vapor treatment

Method used

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  • Method for preparing CO2 catching membrane material with high hydrothermal stability
  • Method for preparing CO2 catching membrane material with high hydrothermal stability
  • Method for preparing CO2 catching membrane material with high hydrothermal stability

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Mix 5ml (0.01mol) of zirconium n-propoxide, 35ml (0.47mol) of n-propanol and 10.3ml (0.1mol) of AcAc in an ice bath at 0°C and stir for 60 minutes, then add 3.6ml of (0.2mol) water, stirred for 20 minutes. After the reaction, ZrO with transparent appearance was obtained 2 Sol. Store it at -20°C until use. Mix the sol and absolute ethanol at a ratio of 1:3 by volume to obtain a film-forming solution, and place the film-forming solution in a sheet-shaped γ-Al 2 o 3 Membrane surface coating, naturally dried flaky ZrO 2The film was sintered at a heating rate of 2°C / min, and kept at 400°C for 8 hours before cooling down naturally to obtain ZrO 2 membrane. The gas permeability and hydrothermal stability of the membrane are as follows: figure 1 with figure 2 shown. from figure 1 It can be seen from the figure that at 200°C, the film is 2 The permeability can reach ~5×10 -8 mol.m -2 .s -1 .pa -1 , H 2 / CO 2 The selectivity exceeds the ideal separation factor o...

Embodiment 2

[0031] Mix 10ml (0.02mol) of zirconium isopropoxide, 1.2ml (0.02mol) of absolute ethanol and 0.2ml (0.002mol) of DEA in an ice bath at -10°C and stir for 1 minute, then add 10.8ml of (0.6mol) water, reacted for 60 minutes. After the reaction, ZrO with transparent appearance was obtained 2 Sol. Store it at -20°C until use. The sol and absolute ethanol were mixed with a volume ratio of 1:8 to obtain a film-making solution, and the film-making solution was placed in the flake TiO 2 Membrane surface coating, naturally dried flaky ZrO 2 The film was sintered at a heating rate of 1 °C / min, and after reaching 100 °C, it was kept for 1 hour and then cooled naturally to obtain ZrO 2 membrane. The membrane pairs H 2 The permeability reaches 4×10 -8 mol.m -2 .s -1 .pa -1 , H 2 / CO 2 The ideal separation factor is over 20, and it is stable for 125 hours at 200°C and 300kPa water vapor.

Embodiment 3

[0033] Mix 9ml (0.02mol) of zirconium n-butoxide, 40ml (0.44mol) of n-butanol and 40ml (0.39mol) of AcAc in an ice bath at -20°C. After stirring for 30 minutes, add 0.4ml of (0.022mol) water, react for 1 minute. After the reaction, ZrO with transparent appearance was obtained 2 Sol. Store it at -20°C until use. The sol and n-propanol are mixed with a volume ratio of 1:20 to obtain a film-making solution, and the film-making solution is placed in a sheet of ZrO 2 Membrane surface coating, naturally dried flaky ZrO 2 The film was sintered at a heating rate of 0.2°C / min, and after reaching 800°C, it was kept for 10 hours and then cooled naturally to obtain ZrO 2 membrane. The membrane pairs H 2 The permeability reaches 1.7×10 -8 mol.m -2 .s -1 .pa -1 , H 2 / CO 2 The ideal separation factor is over 20, and it is stable for 20 hours at 200°C and 500kPa water vapor.

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Abstract

The invention relates to a method for preparing a CO2 catching membrane material with high hydrothermal stability. The method comprises the following steps of: synthesizing ZrO2 sol through a sol-gel method by using zirconium alkoxide as a precursor, and coating on a platy carrier to obtain a ZrO2 membrane. The H2 permeability of the ZrO2 gas separation membrane prepared by the method is 5*10<-8>mol.m<-2>.s<-1>.pa<-1>, and H2/CO2 selectivity can reach 15 which is far more than an H2/CO2 ideal separation factor (4.7) based on a Knudsen diffusion mechanism; the performance of the membrane is basically unchanged after the membrane is treated at the temperature of 200 DEG C under the water vapor partial pressure of 100kPa for 400 hours; and by prolonging treatment time to 1,250 hours, the H2 permeability is reduced to a certain extent, but the H2/CO2 ideal separation factor is increased to 33, which prove that the membrane still has a separation effect, so that a foundation is laid for gas separation of the ZrO2 gas separation membrane in water vapor environment.

Description

Technical field: [0001] The present invention relates to a CO with high hydrothermal stability 2 The preparation method of trapping membrane material, especially relates to H in water vapor environment 2 / CO 2 A pure ZrO in the field of gas separation 2 Membrane preparation method. The ZrO 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] In recent years, with the rapid economic development and the acceleration of industrialization, CO 2 Emissions are increasing day by day. At the same time, the depletion of oil, coal and natural gas resources urgently requires new energy supplements. Hydrogen is a promising new energy source at present. Its main preparation method is the water-gas shift reaction, but the reaction is in the process of obtaining H 2 while producing CO 2 . More and more CO 2 Emissions will cause the gre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D67/00B01D53/22C01B31/20C01B32/50
CPCY02C10/10Y02C20/40Y02P20/151
Inventor 漆虹李丽徐南平
Owner NANJING UNIV OF TECH
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