Anion-doped perovskite-type mixed conductor hydrogen permeable membrane material and its preparation method and application

A perovskite-type, mixed-conductor technology, applied in separation methods, chemical instruments and methods, membrane technology, etc., can solve the problem of reduced hydrogen flux in the total conductivity of zirconates, reduced material conductivity, high grain boundary resistance, etc. problems, to achieve the effect of increasing hydrogen permeation, increasing oxygen hole concentration, and low cost

Active Publication Date: 2019-11-15
SOUTH CHINA UNIV OF TECH
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  • Abstract
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  • Claims
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Problems solved by technology

However, cerate is very easy to react in carbon-containing or sulfur-containing acid gases to form carbonates or sulfur-containing compounds. These heterogeneous substances will reduce the conductivity of the material and reduce the mechanical properties and separation efficiency of the membrane. ; while zirconates have relatively good stability and are suitable for such conditions, but due to their high grain boundary resistance, the overall conductivity of zirconates and their hydrogen flux are greatly reduced compared with cerates
[0004] In the field of hydrogen separation membrane research, mixed conductor hydrogen permeable membranes have obvious advantages and are widely used. However, the hydrogen separation efficiency and chemical stability of mixed conductor hydrogen permeable membranes are generally not high at present, and it is difficult to achieve large-scale production and industrial application.

Method used

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  • Anion-doped perovskite-type mixed conductor hydrogen permeable membrane material and its preparation method and application
  • Anion-doped perovskite-type mixed conductor hydrogen permeable membrane material and its preparation method and application
  • Anion-doped perovskite-type mixed conductor hydrogen permeable membrane material and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A perovskite-type mixed conductor hydrogen permeable film material BaCe doped with fluorine ions in this embodiment 0.9 Fe 0.1 o 2.75-δ f 0.5 (BCFF 0.5 ) and perovskite-type hydrogen permeable membrane material BaCe without doped fluoride ions 0.9 Fe 0.1 o 3-δ The preparation method of (BCF9010), wherein δ=0~1, specifically comprises the following steps:

[0040] (1) Synthetic BCFF 0.5 : Weigh 25.65g BaCO respectively 3 , 16.41 g CeO 2 , 1.038g Fe 2 o 3 , 4.271gCeF 3 , add 20ml of ethanol after preliminary mixing, ball mill at a speed of 300r / min, take out and dry naturally after 5h;

[0041] (2) Synthesis of BCF9010: Weigh 25.65g BaCO respectively 3 , 20.14 g CeO 2 , 1.038g Fe 2 o 3 , add 20ml of ethanol after preliminary mixing, ball mill at a speed of 300r / min, take out and dry naturally after 5h;

[0042] (3) BCFF after ball milling 0.5 The raw material powder mixed evenly with BCF9010 was placed in a high-temperature muffle furnace and raised to 105...

Embodiment 2

[0046] A perovskite-type mixed conductor hydrogen-permeable membrane material SrCe not doped with anions in this embodiment 0.1 Zr 0.9 o 3-δ (SCZ) preparation method, wherein δ=0~1, specifically comprises the following steps:

[0047] (1) Weigh 8.858g SrCO respectively 3 , 1.033g CeO 2 , 6.654g ZrO 2 , add 10ml of ethanol after preliminary mixing, ball mill at a speed of 300r / min, take it out and dry it naturally after 30h; then put it in a high-temperature muffle furnace to raise the temperature to 900°C at a heating rate of 1°C / min, keep it warm for 10h, and then The rate of 1°C / min was lowered to room temperature to obtain a phase-formed powder. The obtained SCZ powder is subjected to phase analysis, and the results are as follows: figure 1 shown.

[0048] (2) After a little grinding of the SCZ phase-formed powder, weigh 1g of the powder, place it in a stainless steel abrasive tool with an inner diameter of 16mm, and keep it under a pressure of 22.5MPa for 5min to ob...

Embodiment 3

[0050] A perovskite-type mixed conductor hydrogen permeable film material BaCe doped with fluorine ions in this embodiment 0.5 Ni 0.5 o 2.5-δ f 1.0 (BCFF 1.0 ) preparation method, wherein δ=0~1, specifically comprises the following steps:

[0051] (1) Weigh and weigh 29.60g BaCO respectively 3 , 8.606 g CeO 2 , 5.603g NiO 2 , 9.856g CeF 3 After preliminary mixing, 30ml of ethanol was added, ball milled at a speed of 300r / min, taken out and dried naturally after 17.5h; then placed in a high-temperature muffle furnace to raise the temperature to 1200°C at a heating rate of 2°C / min, and keep it warm for 10h, then Decrease to room temperature at a rate of 1°C / min to obtain a phase-formed powder. The obtained SCZ powder is subjected to phase analysis, and the results are as follows: figure 1 shown.

[0052] (2) BCFF 1.0 After a little grinding of the phase-formed powder, weigh 2g of the powder, put it in a stainless steel grinding tool with an inner diameter of 16mm, and...

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Abstract

The invention discloses an anion-doped perovskite mixed conductor hydrogen permeation membrane material and a preparation method and application thereof, and belongs to the field of mixed conductor membrane materials. A chemical general formula of the material is ACe(1-b)BO<3-delta-c / 2>X<c>, wherein A is at least one of Ca, Sr and Ba; B is at least one of Fe, Co, Ni, Nd, Tm, Y, Yb an Zr; X is one of F, Cl, Br and I; delta is the non-stoichiometric ratio; b is smaller than or equal to 0.9 and greater than or equal to 0.1; and c is smaller than or equal to 1 and greater than or equal to 0. The material can be prepared by adopting a solid-phase reaction method and an EDTA-citric acid mixed complex method. According to the anion-doped perovskite mixed conductor hydrogen permeation membrane material, the oxygen hole concentration of the membrane material is improved by anion doping, the hydrogen permeability of the membrane material is greatly improved, and the anion-doped perovskite mixed conductor hydrogen permeation membrane material can be used for selectively separating hydrogen from a hydrogen-containing mixed gas, and can be coupled to hydrogen-related reaction to build a membrane reactor.

Description

technical field [0001] The invention belongs to the field of mixed conductor membrane materials, in particular to an anion-doped perovskite-type mixed conductor hydrogen permeable membrane material and its preparation method and application. Background technique [0002] Hybrid proton-electron conductor hydrogen permeable membrane is a kind of dense inorganic ceramic membrane material with both proton conductivity and electron conductivity at high temperature. Since the mixed conductor hydrogen permeable membrane not only has the function of hydrogen separation, but also has catalytic performance, it can be used not only for pure hydrogen production, but also for coupling with many hydrogen-related reactions, reducing process flow, reducing investment costs, and improving reaction conversion efficiency. Therefore, it has become a research hotspot in the field of inorganic membrane separation, chemical reaction and catalysis. [0003] The research on perovskite-type mixed co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/02B01D67/00B01D53/22C01B3/50
CPCB01D53/228B01D67/0044B01D71/024C01B3/503C01B2203/0405
Inventor 王海辉陈莉薛健
Owner SOUTH CHINA UNIV OF TECH
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