Zirconium pyrophosphate-based mixed conductor hydrogen permeation membrane material with layered structure and capable of being operated at medium and low temperature as well as preparation method and application of zirconium pyrophosphate-based mixed conductor hydrogen permeation membrane material

A zirconium pyrophosphate-based, layered structure technology, applied in separation methods, semi-permeable membrane separation, chemical instruments and methods, etc., can solve problems such as chemically stable hydrogen permeable membrane materials that have not yet been developed, and achieve the benefits of sintering and densification , excellent compactness and high hydrogen permeability

Active Publication Date: 2021-11-02
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, hydrogen permeable membrane materials with both hydrogen separation efficiency and chemical stability in this temperature range have not been developed yet.

Method used

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  • Zirconium pyrophosphate-based mixed conductor hydrogen permeation membrane material with layered structure and capable of being operated at medium and low temperature as well as preparation method and application of zirconium pyrophosphate-based mixed conductor hydrogen permeation membrane material
  • Zirconium pyrophosphate-based mixed conductor hydrogen permeation membrane material with layered structure and capable of being operated at medium and low temperature as well as preparation method and application of zirconium pyrophosphate-based mixed conductor hydrogen permeation membrane material
  • Zirconium pyrophosphate-based mixed conductor hydrogen permeation membrane material with layered structure and capable of being operated at medium and low temperature as well as preparation method and application of zirconium pyrophosphate-based mixed conductor hydrogen permeation membrane material

Examples

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Effect test

Embodiment 1

[0039] A magnesium ion-doped layered zirconium pyrophosphate-based mixed conductor hydrogen permeable membrane material Zr that can be operated at medium and low temperatures in this embodiment 0.9 Mg 0.1 P 2 o 7-δ (ZMP10) preparation method, wherein δ=0~0.2, comprises the following steps:

[0040] (1) Synthesis of ZMP10: Weigh 9.854g Zr(HPO 4 ) 2 ·H 2 O, 0.146g MgO, measure 0.62ml H 3 PO 4 , add 20ml ethanol after initial mixing, carry out ball milling with the rotating speed of 500r / min, take out after 12h and dry naturally, the raw material layer structure Zr(HPO 4 ) 2 ·H 2 The scanning electron microscope image of O is shown in figure 1 shown, where the H 3 PO 4 The mass concentration is 85%.

[0041] (2) Put the ZMP10 raw material powder obtained by ball milling into a high-temperature muffle furnace to raise the temperature to 750°C at a heating rate of 2°C / min, keep it warm for 5 hours, and then lower it to room temperature at a rate of 2°C / min to obtain ZM...

Embodiment 2

[0064] A copper ion-doped zirconium pyrophosphate-based mixed conductor hydrogen permeable membrane material Zr with a layered structure that can be operated at medium and low temperatures in this embodiment 0.95 Cu 0.05 P2O 7-δ (ZCP5) preparation method, wherein δ=0~0.1, specifically comprises the following steps:

[0065] (1) Weigh 9.863g Zr(HPO 4 ) 2 ·H 2 O, 0.137g CuO, measure 0.46ml H 3 PO 4 After initial mixing, 20ml of ethanol was added, and ball milling was performed at a speed of 400r / min. After 10 hours, it was taken out and dried naturally; the dried ZCP5 powder was placed in a high-temperature muffle furnace and raised to 600°C at a heating rate of 1°C / min, and Keep it warm for 10 hours, then lower it to room temperature at a rate of 1°C / min to obtain a phase-formed powder. The obtained powder was subjected to phase analysis, and the results were as follows: figure 2 As shown, the material maintains the original cubic phase structure after doping copper, a...

Embodiment 3

[0068] A layered zirconium pyrophosphate-based mixed conductor material Zr doped with magnesium ions that can be operated at medium and low temperatures in this embodiment 0.85 Mg 0.15 P 2 o 7-δ The preparation method of (ZMP15), wherein δ=0~0.5, specifically comprises the following steps:

[0069] (1) Weigh 8.694g Zr(HPO 4 ) 2 ·H 2 O, 1.306g Mg(NO 3 ) 2 , measure 1.36ml H 3 PO 4 , add 20ml of ethanol after preliminary mixing, ball mill at a speed of 400r / min, take out and dry naturally after 12h; place the dried powder in a high-temperature muffle furnace to raise the temperature to 800°C at a heating rate of 1°C / min, and keep it warm 10h, and then lowered to room temperature at a rate of 1°C / min to obtain a phase-formed powder. The obtained powder was subjected to phase analysis, and the results were as follows: figure 2 As shown, the material maintains the original cubic phase structure after doping with magnesium, and no other impurity phases are formed. Among ...

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Abstract

The invention discloses a zirconium pyrophosphate-based mixed conductor hydrogen permeation membrane material with a layered structure and capable of being operated at medium and low temperatures as well as a preparation method and application of the zirconium pyrophosphate-based mixed conductor hydrogen permeation membrane material. The chemical general formula of the mixed conductor hydrogen permeation membrane material is Zr<1-x> MxP2O<7-delta>, wherein M is one of Mg and Cu; and delta is a non-stoichiometric ratio, x is greater than or equal to 0 and less than or equal to 0.5, and delta is greater than or equal to 0 and less than or equal to 1. As the zirconium pyrophosphate-based compound has a stable phase structure in a wide temperature range (200-600 DEG C), the mixed conductor hydrogen permeation membrane material still keeps a local layered structure after being sintered at high temperature, and a rapid proton transfer channel formed between layers further increases the hydrogen permeation amount of the membrane material. The zirconium pyrophosphate-based mixed conductor hydrogen permeation membrane material with the layered structure prepared by the preparation method disclosed by the invention shows very high hydrogen permeation quantity and good chemical stability at medium and low temperatures.

Description

technical field [0001] The invention belongs to the technical field of separation membrane materials, and in particular relates to a zirconium pyrophosphate-based mixed conductor hydrogen permeable membrane material with a layered structure that can be operated at a medium and low temperature, and a preparation method and application thereof. Background technique [0002] Energy is the cornerstone of social development. At present, 81% of primary energy supply and 66% of electricity come from fossil fuels, but fossil fuels are not renewable, and burning them will cause serious environmental pollution. Hydrogen energy has the advantages of high combustion calorific value, non-polluting products and wide source of raw materials, and is the most promising form of energy among renewable energy sources. However, the current hydrogen production methods are all hydrogen-containing mixtures. In order to improve the purity of hydrogen, hydrogen separation and recovery are the main ta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D67/00B01D53/22
CPCB01D71/02B01D67/0039B01D53/228
Inventor 薛健文思斯王海辉
Owner SOUTH CHINA UNIV OF TECH
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