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Preparation method of iron-based ceramic oxygen permeation membrane capable of improving oxygen permeation stability under CO2 (Carbon Dioxide) atmosphere

An oxygen-permeable membrane and stability technology, applied in the field of preparation of iron-based ceramic oxygen-permeable membranes, can solve problems such as insufficient stability

Active Publication Date: 2017-09-26
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For mixed-conductor oxygen-permeable membrane materials, the most important problem at present is that the membrane material is under high temperature and membrane reaction atmosphere, especially in CO 2 The atmosphere is not stable enough, therefore, improving the stability of membrane materials in acidic atmosphere and reducing atmosphere is the key to realize industrialization

Method used

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  • Preparation method of iron-based ceramic oxygen permeation membrane capable of improving oxygen permeation stability under CO2 (Carbon Dioxide) atmosphere
  • Preparation method of iron-based ceramic oxygen permeation membrane capable of improving oxygen permeation stability under CO2 (Carbon Dioxide) atmosphere
  • Preparation method of iron-based ceramic oxygen permeation membrane capable of improving oxygen permeation stability under CO2 (Carbon Dioxide) atmosphere

Examples

Experimental program
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Effect test

Embodiment 1

[0020] 23.36 g Pr(NO 3 ) 3 ·6H 2 O, 7.58 g Sr(NO 3 ) 2 , 36.16 g Fe(NO 3 ) 3 9H 2 O was dissolved in deionized water, and 52.32 g of ethylenediaminetetraacetic acid and 56.43 g of citric acid were dissolved in another beaker filled with a certain amount of deionized water. The above two solutions were mixed and heated to 95 ° C. The pH value of the solution was 7, and heating was continued until a sol-like substance was obtained. Dry the obtained sol at 150°C until it expands into a spongy porous solid, take it out, bake it at 380°C for 10 hours, and then bake it at 950°C for 5 hours to obtain Pr 0.6 Sr 0.4 FeO 3-δ The powder is ground in a mortar for 3 hours to make the particle size uniform, and an appropriate amount of oleic acid is added to the obtained powder, and it is molded under a pressure of 300 MPa. 0.6 Sr 0.4 FeO 3-δ Single-phase mixed conductor oxygen-permeable membrane, that is, iron-based ceramic oxygen-permeable membrane.

Embodiment 2

[0022] 23.08 g Pr(NO 3 ) 3 ·6H 2 O, 7.48 g Sr(NO 3 ) 2 , 33.04 g Fe(NO 3 ) 3 9H 2 O. Dissolve 3 g of niobium oxalate in deionized water, dissolve 51.67 g of ethylenediaminetetraacetic acid and 55.74 g of citric acid in another beaker filled with a certain amount of deionized water, mix the above two solutions, and heat to 95°C , by adding ammonia water dropwise to make the pH value of the solution 8, continue heating until a sol-like substance is obtained, and dry the obtained sol-like substance at 160° C. for 10 hours. Then calcined at 950°C for 8 hours to obtain Pr 0.6 Sr 0.4 Fe 0.925 Nb 0.075 o 3-δ The powder is ground in a mortar for 3 hours to make the particle size uniform. Add an appropriate amount of oleic acid to the obtained powder, and shape it under a pressure of 300 MPa. The obtained flake body is roasted at 1350 ° C for 8 hours to obtain Pr 0.6 Sr 0.4 Fe 0.925 Nb 0.075 o 3-δ Single-phase mixed conductor oxygen-permeable membrane, that is, iron-bas...

Embodiment 3

[0024] 22.98 g Pr(NO 3 ) 3 ·6H 2 O, 7.45 g Sr(NO 3 ) 2 , 32.01 g Fe(NO3 ) 3 9H 2 O, 3.98 g of niobium oxalate was dissolved in deionized water, 51.46 g of ethylenediaminetetraacetic acid and 55.51 g of citric acid were dissolved in another beaker with a certain amount of deionized water, and the above two solutions were mixed and heated to 100 °C , by adding ammonia water dropwise to make the pH value of the solution 8, continue heating until a sol-like substance is obtained, and dry the obtained sol-like substance at 160° C. for 10 hours. Then calcined at 950°C for 8 hours to obtain Pr 0.6 Sr 0.4 Fe 0.9 Nb 0.1 o 3-δ The powder was ground in a mortar for 3 hours to make the particle size uniform. Add an appropriate amount of oleic acid to the obtained powder and shape it under a pressure of 300 MPa. The obtained flake green body was roasted at 1400 ° C for 8 hours to obtain Pr 0.6 Sr 0.4 Fe 0.9 Nb 0.1 o 3-δ Single-phase mixed conductor oxygen-permeable membrane,...

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Abstract

The invention discloses a preparation method of an iron-based ceramic oxygen permeation membrane capable of improving oxygen permeation stability under a CO2 (Carbon Dioxide) atmosphere. The iron-based ceramic oxygen permeation membrane has the chemical constitution of Pr0.6Sr0.4Fe1-xXxO3-delta, wherein X is any one of Nb and Al, and the stoichiometric ratio is that x is larger than or equal to 0 and less than or equal to 0.15. According to the iron-based ceramic oxygen permeation membrane provided by the invention, with the doping of the Nb, the CO2 resistance of the material can be effectively improved; with the doping of the Al, a cubic perovskite structure material with good symmetry can be obtained. The preparation method provided by the invention comprises the steps of dissolving various metal nitrate into deionized water, mixing with edetic acid and citric acid monohydrate, using ammonium hydroxide for adjusting a PH value to 7 to 8, and after volatilizing moisture, roasting for two times, and obtaining Pr0.6Sr0.4Fe1-xXxO3-delta powder; after grinding, forming at a certain pressure, roasting at 1200 to 1400 DEG C for 8 hours, and obtaining a compact oxygen permeation membrane. The Pr0.6Sr0.4Fe1-xXxO3-delta oxygen permeation membrane keeps long-time stable at 900 DEG C under a pure CO2 atmosphere, and the stable oxygen permeation amount is around 0.11ml.min<-1>.cm<-2>.

Description

technical field [0001] The invention discloses a method that can improve CO 2 A method for preparing an iron-based ceramic oxygen-permeable membrane with oxygen-permeable stability under atmosphere. It specifically relates to a method for obtaining a new oxygen-permeable membrane material by doping a B-site element. Background technique [0002] The mixed conductor oxygen permeable membrane can be used as an oxygen permeable membrane material because it has both electronic and oxygen ion conductivity. At a certain temperature, when there is an oxygen concentration gradient on both sides of the membrane, oxygen will pass through the oxygen vacancies in the form of oxygen ions. Theoretical Above, the dense ceramic oxygen permeable membrane has 100% oxygen permeable selectivity. [0003] The mixed conductor oxygen-permeable membrane can be used in high-purity oxygen preparation, oxygen-enriched combustion, partial oxidation of natural gas to synthesis gas or selective oxidati...

Claims

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Application Information

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IPC IPC(8): B01D67/00C04B35/26
CPCB01D67/0039B01D67/0076B01D71/024C04B35/2641C04B2235/3213C04B2235/3217C04B2235/3224C04B2235/3251C04B2235/602C04B2235/656C04B2235/6567C04B2235/768
Inventor 程红伟鲁雄刚王远枝周慧婕陈沙刘超云
Owner SHANGHAI UNIV
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