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CO2 tolerance multi-phase mixed conductor compact oxygen permeable film material and preparation method and use thereof

A technology of multi-phase mixing and oxygen-permeable membrane, applied in semi-permeable membrane separation, chemical instruments and methods, membrane technology, etc., to achieve the effect of improving CO2 resistance, high oxygen flux, and low thermal expansion coefficient

Inactive Publication Date: 2009-05-06
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the invention is to improve the existing oxygen permeable membrane material in CO 2 Not stable enough under the atmosphere and easy to combine with CO 2 Reaction occurs to destroy the deficiencies of the membrane material and provide a CO resistant 2 The dense oxygen-permeable membrane material of multi-phase mixed conductor in the atmosphere not only has high oxygen ion and electron conductivity, but also has high temperature and CO 2 It still has good chemical and structural stability under the atmosphere, and is suitable for long-term operation; another object of the present invention is to provide the preparation method and application of the above-mentioned materials

Method used

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  • CO2 tolerance multi-phase mixed conductor compact oxygen permeable film material and preparation method and use thereof
  • CO2 tolerance multi-phase mixed conductor compact oxygen permeable film material and preparation method and use thereof
  • CO2 tolerance multi-phase mixed conductor compact oxygen permeable film material and preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The organic acid complex method preparation and film forming examples of the material of the present invention.

[0025] Preparation of Sm by organic acid complex method 0.85 Ce 0.1 Fe 0.8 Mn 0.2 O 3-δ Take the material as an example, according to the stoichiometric ratio of the material 4.25:1:8:2, the Sm 2 O 3 (Pre-dissolved in nitric acid), Ce(NO 3 ) 3 ·6H 2 O, Fe(NO 3 ) 3 ·9H 2 O and Mn(NO 3 ) 2 Respectively dissolve in water, add appropriate amount of citric acid and ethylenediaminetetraacetic acid. The molar ratio of citric acid, ethylenediaminetetraacetic acid (ethylenediaminetetraacetic acid is first dissolved in ammonia water) and metal ions is 2:1:1, and the pH value is adjusted to 8 with ammonia water. Put the clarified precursor into an oven and heat it at 250°C for 10 hours. After spontaneous combustion occurs, the powder is heated at 2°C / min to 1000°C for 5 hours, and then cooled at 3°C / min to 20°C to obtain the material of the present invention. Powder.

[00...

Embodiment 2

[0028] The solid-phase reaction method preparation and film forming examples of the material of the present invention.

[0029] Preparation of La by solid phase reaction method 0.85 Ce 0.1 Ga 0.3 Fe 0.6 Al 0.1 O 3 -δ material as an example, according to the stoichiometric ratio of the material 4.25:1:1.5:3:0.5, the La 2 O 3 , CeO 2 , Ga 2 O 3 , Fe 2 O 3 And Al 2 O 3 After the powder is mixed, ethanol is added, placed in a ball mill for wet grinding for 24 hours, and then dried in static air. The dried powder is placed in a high-aluminum crucible, and fired in an air atmosphere at 950°C for 10 hours at a temperature rising and falling rate of 2°C / min to obtain the material powder of the present invention.

[0030] The powder is produced under a uniaxial pressure of 400 MPa to produce a green film. The green film is sintered in a high-temperature furnace at 1250 ℃ for 20 hours at a temperature rise and fall rate of 1 ℃ / min, and then cooled to room temperature. The surface microstruc...

Embodiment 3

[0032] Prepare the material Sm of the present invention according to the organic acid complexation method of Example 1 0.85 Ce 0.1 Fe 1-x Mn x O 3-δ The following table shows the configuration of various elements

[0033] sample The molar ratio of Sm, Ce, Fe and Mn x＝0.1 4.25∶1∶9∶1 x＝0.2 4.25∶1∶8∶2 x＝0.3 4.25∶1∶7∶3

[0034] The above three powder samples were subjected to X-ray diffraction test, and the results are shown in figure 2 (a). From figure 2 (a) It can be seen that the prepared Sm 0.85 Ce 0.1 Fe 1-x Mn x O 3-δ The samples all formed a complete main phase of perovskite, in addition to CeO 2 Relative to Sm 2 O 3 phase. This shows that the prepared material is a multiphase mixed conductor material.

[0035] Prepare the material La of the present invention according to the solid-phase reaction method of Example 2 0.85 Ce 0.1 Ga 0.3 Fe 0.7-y Al y O 3-δ The following table shows the configuration of various elements

[0036] sample T...

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Abstract

The invention relates to a compact oxygen-permeable membrane material of multiphase-mixed conductors that can endure CO2 atmosphere, as well as a preparation method and usage of the compact oxygen-permeable membrane material. The compact oxygen-permeable membrane material is a composite oxide with the general formula of C1-xCexFe1-y-y'DyD' y'O3-Delta; wherein, Delta is oxygen non-stoichiometric, and C is any element among La, Pr, Nd, Sm and Gd; D and D' is any element among Al, Sc, Ti, Cr, Mn, Zn, Ga, Zr, Nb and W, and D and D' can be same or different; and x and y are both larger than 0 and less than 1, y' is larger than or equal to 0 as well as less than 1 minus y. The compact oxygen-permeable membrane material further contains small amounts of other phases besides a main perovskite body. The compact oxygen-permeable membrane material has good stability at high temperature and under CO2 atmosphere, is suitable for running stably for a long time under membrane catalytic reaction conditions, and can be used in the fields of oxygen-permeable membranes and solid electrochemistry besides membrane catalytic reactors.

Description

Technical field [0001] The invention belongs to the field of design and development of dense oxygen permeable membrane materials for mixed conductors, and in particular relates to a CO resistant 2 Atmospheric multiphase mixed conductor dense oxygen permeable membrane material and its preparation method and application. Background technique [0002] Energy and environment are the two most important issues involved in the sustainable development of human society in the future. Since natural gas reserves are abundant in nature, with the increasing shortage of oil resources, how to convert natural gas into basic organic chemical products has become a problem of great concern to people. One of the important directions is the use of partial oxidation of methane (POM) to convert natural gas into synthesis gas (Ashcroft et al., Nature, 1990, 344, 319; Hickman et al., Science, 1993, 259, 343). Then, liquid fuels and chemical products are prepared through F-T reaction or other reaction pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02
Inventor 金万勤董学良张广儒徐南平
Owner NANJING UNIV OF TECH
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