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A non-metal ion-doped perovskite-type mixed conductor hydrogen permeable film and its preparation method and application

A perovskite-type, mixed-conductor technology, which is applied in separation methods, non-metallic elements, chemical instruments and methods, etc., can solve the problems that the permeability and stability cannot be taken into account at the same time, and limit the input of membrane materials, so as to achieve the improvement of hydrogen gas permeability , small particle diameter, low powder phase formation temperature and low film sintering densification temperature

Active Publication Date: 2021-05-14
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The hydrogen permeability of the hydrogen permeable membrane can be increased by doping metal ions at the B site, but the metal ions will be reduced to a certain extent in the hydrogen atmosphere, which limits the investment of membrane materials in practical applications.
[0004] At present, the permeability and stability of hydrogen permeable membranes are two major problems that limit the practical industrial application of membrane materials. Existing materials cannot give consideration to both permeability and stability at the same time.

Method used

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  • A non-metal ion-doped perovskite-type mixed conductor hydrogen permeable film and its preparation method and application
  • A non-metal ion-doped perovskite-type mixed conductor hydrogen permeable film and its preparation method and application
  • A non-metal ion-doped perovskite-type mixed conductor hydrogen permeable film and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A phosphorus ion-doped perovskite-type hybrid hydrogen permeable material BaCe of the present embodiment 0.8 P 0.2 o 3-δ (δ = 0.2) (BCP20) and undoped perovskite-type hybrid hydrogen permeable material BaCeO 3-δ (δ = 0) (BCO), the preparation method comprises the following steps:

[0034] (1) Weigh BCP20 raw material: 12.91g Ba (NO 3 ) 2 , 9.33g Ce (NO 3 ) 4 ·6H 2 O, 1.14g NH 4 h 2 PO 4 Dissolve in deionized water, add 8.89g glycine to the mixture;

[0035] (2) Weigh BCO raw material: 12.91g Ba (NO 3 ) 2 , 11.66g Ce (NO 3 ) 4 ·6H 2 O was dissolved in deionized water, and 9.88g glycine was added to the mixture;

[0036] (3) Heat the nitrate mixture obtained in steps (1) and (2) to 100°C and stir for 40 hours until the solution becomes gelatinous, then put the gel in an electric furnace, heat to 350°C and roast to obtain The precursor of the powder; the powder is placed in a muffle furnace, and the temperature is kept at a rate of 2.5 ° C to 850 ° C per...

Embodiment 2

[0043] A kind of phosphorus ion-doped perovskite type mixed conductor hydrogen permeable film material Ba of the present embodiment 5.3 Zr 0.7 P 0.3 o 3-δ (δ = 0.3) (BZP30) preparation method includes the following steps:

[0044] (1) Weigh BZP30 raw material: 10.11g Ba (NO 3 ) 2 , 11.63g Zr (NO 3 ) 4 ·5H 2 O, 1.33g NH 4 h 2 PO 4 Dissolve in deionized water, add 6.72g glycine to the mixture;

[0045] (2) Heat the nitrate mixture obtained in step (1) to 250°C and stir for 32 hours until the solution takes on the form of a gel, then put the gel into an electric furnace, heat to 200°C and bake to obtain the precursor of the powder ; Put the powder in a muffle furnace, keep the temperature at a rate of 5° C. to 950° C. per minute for 12 hours, and obtain the powder BZP30.

[0046] (3) Weigh 2g of powder BZP30 and put it into a cast iron mold, keep it under a pressure of 15MPa for 5 minutes to obtain a green body; put the green body into a high-temperature muffle furna...

Embodiment 3

[0049] A kind of sulfide-doped perovskite type mixed conductor hydrogen permeable membrane material SrCe of the present embodiment 0.5 S 0.5 o 3-δ (δ =0.5) (SCS50) preparation method comprises the following steps:

[0050] (1) Weigh SCS50 raw material: 12.79g Sr (NO 3 ) 2 4H 2 O, 5.32g Ce (NO 3 ) 4 ·6H 2 O, 2.62gNH 4 h 2 SO 4 Dissolve in deionized water, add 8.05g glycine to the mixture;

[0051] (2) Heat the nitrate mixture obtained in step (1) to 350°C and stir for 25 hours until the solution becomes gel-like, then put the gel into an electric furnace, heat to 500°C and bake to obtain the precursor of the powder ; Put the powder in a muffle furnace, keep the temperature at a rate of 1° C. to 750° C. per minute for 5 hours, and obtain the powder SCS50.

[0052] (3) Weigh 0.5g of phase-forming powder SCS50 and put it into a cast iron mold, keep it under 10MPa pressure for 10 minutes to obtain a green body; put the green body into a high-temperature muffle furnace ...

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Abstract

The invention discloses a perovskite-type mixed conductor hydrogen permeable membrane doped with non-metal ions, a preparation method and application thereof. The general chemical formula of the perovskite mixed conductor hydrogen permeable film is AB 1‑ X m X o 3‑δ , where A is one of Sr, Ba, Ca; B is one of Ce, Zr; M is one of non-metallic elements P, S; δ is a non-stoichiometric ratio; 0≤δ≤0.5, 0≤ x≤0.5. The material of the present invention can be prepared by glycine-nitrate combustion method. In the material of the present invention, the electronic conductivity of the membrane material is improved by the doping of non-metal ions, thereby increasing the hydrogen permeability of the membrane material. The material has excellent separation performance in a hydrogen-containing atmosphere and can be used for hydrogen-containing The hydrogen in the gas mixture is separated.

Description

technical field [0001] The invention belongs to the technical field of application of energy separation materials, and in particular relates to a perovskite-type mixed conductor hydrogen permeable membrane doped with non-metal ions and its preparation method and application. Background technique [0002] Mixed conductor hydrogen permeable membrane can occupy a certain position in the field of hydrogen separation because it can conduct protons and electrons at the same time. Among the many types of mixed conductor hydrogen permeable membranes, perovskite-type inorganic metal oxides are the most common and studied. [0003] The general structural formula of perovskite inorganic metal oxides is ABO3, and most hydrogen permeable materials are based on BaCeO 3-δ and SrCeO 3-δ system, the conductivity of the perovskite-type mixed conductor hydrogen permeable film can reach 10 -2 ~10 -3 S cm -1 . Although BaCeO 3-δ and SrCeO 3-δ Compared with the proton conductivity, the e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/02B01D67/00B01D53/22C01B3/50
CPCB01D53/228B01D67/0039B01D71/024B01D2256/16C01B3/503C01B2203/0405
Inventor 王海辉庄丽彬薛健李家祺
Owner SOUTH CHINA UNIV OF TECH
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