An anion-doped fluorite type tungstic acid-based mixed conductor hydrogen permeable membrane material and its preparation method and application

A mixed conductor and fluorite-type technology, which is applied in the field of fluorite-type tungstic acid-based mixed conductor hydrogen permeable membrane material and its preparation, can solve the problem of hydrogen permeable membrane material hydrogen permeability and stability. Hydrogen permeable membrane technology is difficult to achieve large-scale For industrial applications, it is difficult to meet the requirements of hydrogen flux and demanding mechanical properties, etc., to achieve the effect of increasing hydrogen permeation, high operational stability, and increasing the concentration of oxygen holes

Active Publication Date: 2019-10-18
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The inconsistency between hydrogen permeability and stability of hydrogen permeable membrane materials makes it difficult to achieve large-scale industrial application of hydrogen permeable membrane technology. Existing materials are difficult to meet the requirements of hydrogen flux, thermal stability, chemical stability, mechanical Strict requirements in terms of performance, etc.

Method used

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  • An anion-doped fluorite type tungstic acid-based mixed conductor hydrogen permeable membrane material and its preparation method and application
  • An anion-doped fluorite type tungstic acid-based mixed conductor hydrogen permeable membrane material and its preparation method and application
  • An anion-doped fluorite type tungstic acid-based mixed conductor hydrogen permeable membrane material and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0042] A fluorite-type tungstic acid-based mixed conductor hydrogen permeable membrane material La 5.2 W 0.8 Mo 0.2 o 10.3-δ F(LWMF 1.0 ) and the hydrogen permeable membrane material La without fluoride ion 5.2 W 0.8 Mo 0.2 o 11.25-δ (LWM02) preparation method, wherein δ=0~1, specifically comprises the following steps:

[0043] (1) Synthetic LWMF 1.0 : Weigh 25.84g La respectively 2 o 3 , 2.285g LaF 3 , 6.491g WO 3 , 1.007g MoO 3 , after preliminary mixing, add 30ml of ethanol, ball mill at a speed of 300r / min, take it out after 24h and dry it naturally;

[0044] (2) Synthesis of LWM02: Weigh 29.65g La 2 o 3 , 6.491g WO 3 , 1.007 g MoO 3 , after preliminary mixing, add 30ml of ethanol, ball mill at a speed of 300r / min, take it out after 24h and dry it naturally;

[0045] (3) LWMF obtained by ball milling 1.0 The raw material powder mixed evenly with LWM02 is placed in a high-temperature muffle furnace to raise the temperature to 1000°C at a heating rate of 2...

Embodiment 2

[0049] A fluorite-type tungstic acid-based mixed conductor hydrogen permeable film material Nd doped with fluorine ions in this embodiment 5.5 WO 11-δ f 0.5 (NWMF 0.5 ) preparation method, wherein δ=0~1, specifically comprises the following steps:

[0050] (1) Weigh 30.42g Nd respectively 2 o 3 , 1.174g NdF 3 , 8.114g WO 3 After preliminary mixing, 20ml of ethanol was added, ball milled at a speed of 300r / min, taken out and dried naturally after 24h; then placed in a high-temperature muffle furnace to raise the temperature to 850°C at a heating rate of 1°C / min, and kept for 10h, and then The rate of 1°C / min was lowered to room temperature to obtain a phase-formed powder. The obtained powder was subjected to phase analysis, and the results were as follows: figure 1 As shown, the material maintains the original fluorite structure after doping with F element, and no other impurity phases are formed.

[0051] (2) Weigh 1.0g of the powder after grinding the phase-formed po...

Embodiment 3

[0053] The non-doped anion-free fluorite-type tungstic acid-based mixed conductor hydrogen permeable membrane material La 5.8 W 0.6 Mo 0.4 o 11.25-δ (LWMO) preparation method, wherein δ=0~1, specifically comprises the following steps:

[0054] (1) Weigh 18.89g La respectively 2 o 3 , 2.782g WO 3 , 1.151 g MoO 3 After initial mixing, 10ml of ethanol was added, ball milled at a speed of 300r / min, taken out and dried naturally after 24h; then placed in a high-temperature muffle furnace to raise the temperature to 700°C at a heating rate of 5°C / min, and kept for 5h, and then The rate of 1°C / min was lowered to room temperature to obtain a phase-formed powder. The obtained powder was subjected to phase analysis, and the results were as follows: figure 1 As shown, the material maintains the original fluorite structure after doping with F element, and no other impurity phases are formed.

[0055] (2) Grind the phase-formed powder for a while, weigh 2.0g of the powder, place i...

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Abstract

The invention discloses an anion doped fluorite-type tungstic acid based mixed conductor hydrogen permeation membrane material and a preparation method and applications thereof. The chemical formula of the material is LnW<1-b>MO<11.25-c / 2-delta>X<c>; wherein Ln represents one of La, Pr, Nd, Sm, Gd, and Er; M represents Nb and / or Mo; X is one of F, Cl, Br, and I; delta represents a non-stoichiometric ratio; 5.2<=a<=5.8, 0<=b<=0.4, and 0<=c<=1. The material is prepared by a solid phase reaction method and an EDTA-citric acid mixing-complexing method. The oxygen vacancy concentration of the membrane material is increased by the anion doping; the hydrogen permeation quantity of the membrane material is greatly increased; the membrane material has very high operation stability in an acidic atmosphere such as sulfur dioxide, carbon dioxide, and the like, can be used to separate hydrogen gas from hydrogen-containing mixed gas, and can be used to prepare a membrane reactor by coupling the membrane material with hydrogen related reactions.

Description

technical field [0001] The invention belongs to the field of mixed conductor membrane materials, in particular to an anion-doped fluorite-type tungstic acid-based mixed conductor hydrogen permeable membrane material and its preparation method and application. Background technique [0002] Mixed conductor hydrogen permeable membrane is a kind of inorganic dense ceramic membrane material with both proton-conducting and electronic-conducting properties 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 membranes and catalysis. [0003] Fluorite structure metal oxides with CeO 2 , Y 2 o 3 , Y...

Claims

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Application Information

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