CN103601496A - Diphase mixed conductor oxygen permeation membrane material and preparation method thereof - Google Patents
Diphase mixed conductor oxygen permeation membrane material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a diphase mixed conductor oxygen permeation membrane material and a preparation method thereof, belonging to the technical field of comprehensive utilization of metallurgy resource and ceramic manufacture. The oxygen permeation membrane material structurally comprises two phases fluorite and similar perovskite, and is prepared through steps of respectively preparing fluorite Ce0.8Gd0.2O2-detal powder and similar perovskite PrBaCoxFe[2-x]O[5+y] powder through a sol-gel method, mixing the two phases of powder according to certain weight percentage, grinding, and molding under certain pressure, thereby obtaining a green body, roasting for 5-8 hours at 1130-1180 DEG C, so as to obtain the diphase mixed conductor oxygen permeation membrane. The two phases of the membrane prepared by the method are distributed uniformly, and the membrane has a compact structure, has no mixed phase and has good chemical compatibility. Under the condition that the temperature is 925 DEG C, the air mass flow is 300mlmin<-1>, and helium mass flow is 100mlmin<-1>, high oxygen permeation flux of 2.81.1*10<-7>mols<-1>cm<-2> is obtained, and therefore, the oxygen permeation membrane material has application potential.
Description
Technical field
The present invention relates to a kind of biphase mixed conducting oxygen-permeable membrane material and preparation method thereof, belong to Metallurgical resources comprehensive utilization and ceramic fabrication technique field.
Background technology
China has one of coal reserves ，Shi world coal resource big country of flood tide, and in Energy Mix, coal accounts for more than 60%, has 80% raw coal as fuel in produced raw coal.Coal produces a large amount of CO when promoting Economic development
2.By inference, China will replace the U.S. and becomes CO in the world in the near future
2the country of quantity discharged maximum.CO
2global climatologic change and economic impact are caused to the concern of Chinese Government just gradually, and take the measure of some to reduce discharge.Want to reduce the discharge of greenhouse gases and dusty gas, the means of generally taking have: (1) reduces the usage quantity of the energy, particularly fossil energy; (2) use the fuel of low carbon content, effectively utilize Sweet natural gas (especially coke-oven gas), avoid directly discharging or burning; (3) adopt oxygen-rich air or pure oxygen to replace air as combustion oxidant; (4) CO is caught and stores in development
2technology; (5) use nuclear energy and tap a new source of energy, progressively replacing fossil energy; (6) other means (comprise afforestation, advocate the non-energy field means such as energy-conserving and environment-protective prevailing custom).
In view of current energy structure, fossil oil remains the primary energy derive in the whole world, and it is afterwards in the quite a long time, also will be the main energy.Therefore, the way of reality is to improve the service efficiency of fossil energy, to reduce unit energy, produces the CO being discharged
2amount.However, use fossil oil still inevitably can discharge a large amount of greenhouse gases.Settle the matter once and for all, only way is the CO that combustion of fossil fuel is produced
2collection is caught, and stores, rather than leaves that it is discharged in the middle of atmosphere.Because the exploitation of fossil oil has formed a large amount of holes, stratum, the CO that marine bottom also has large quantity space storage to catch
2, estimate the CO of over one hundred year from now on
2discharge can be held wherein, and this measure is expected to significantly solve existing greenhouse gas emission problem.One step of the enforcement most critical of this scheme is high concentration CO
2catch.
Verified, oxygen-enriched combusting is considered to very promising method, has received lasting concern.The source that needs a large amount of oxygen in order to solve oxygen-enriched combusting, a kind of based on (generally at 800～900 ° of C) under middle high temperature, from air, the mixed conductor ceramic oxygen-permeable membrane reactor of oxygen separation is sent to great expectations.The oxygen sepn process of mixed conductor ceramic oxygen-permeable membrane and combustion processes coupling, not only can be reduced by least 35% oxygen loss, and simplification of flowsheet, avoids the problem of reactor local superheating.Oxygen-enriched burning process based on mixed conductor ceramic oxygen-permeable membrane is that wide prospect has been opened up in the application of oxygen permeable film, also gives the new problem of having researched and proposed of oxygen permeable film material simultaneously, finds, develops resisting high-concentration CO
2oxygen permeable film material.Document [catalysis journal, 2009,30:801-816] has disclosed Ce
0.8gd
0.2o
2-
δ -Gd
0.2sr
0.8feO
3-
δ two-phase mixed conductor, and find to use mixed conductor Gd
0.2sr
0.8feO
3-
δ inhibition as the relative oxonium ion transmission of electronics is less, and oxygen transmission rate is higher, and 950
ounder C, thickness 0.5 mm condition, the oxygen transmission rate of phase membrane is single-phase mixed conductor Gd
0.2sr
0.8feO
3-
δ 2 times.Document [Angewandte Chemie International Edition, 2011,50:759-763] is used one-step synthesis to prepare fluorite type-spinel type Ce
0.9gd
0.1o
2-
δ -NiFe
2o
4two-phase mixed conductor film, and prove by situ X-ray diffraction diffraction and stability experiment, this two-phase oxygen permeable film at high temperature has fabulous resistance to CO
2corrodibility.
Summary of the invention
The defect existing for prior art, the object of this invention is to provide a kind of biphase mixed conducting oxygen-permeable membrane material and preparation method thereof.
For achieving the above object, the present invention adopts following technical scheme:
A biphase mixed conducting oxygen-permeable membrane material, has following composition and weight percent:
Ce
0.8gd
0.2o
2-
δ oxide compound 60%
PrBaCo
x fe
2-
x o
5+
y oxide compound 40%
Described
xvalue be 0,0.5,1.0,1.5 and 2.0;
δfor Ce
0.8gd
0.2o
2-
δ oxygen room in oxide compound,
δvalue between 0 to 0.1;
yfor PrBaCo
x fe
2-
x o
5+
y oxygen room in oxide compound,
yvalue between 0 to 0.5.
A preparation method for biphase mixed conducting oxygen-permeable membrane material, has following technological process and step:
(a) according to Ce
0.8gd
0.2o
2-
δ stoichiometric ratio by a certain amount of cerium salt and Gd
2o
3join in nitre aqueous acid, heat and stir until dissolve completely; In metal ion: ethylenediamine tetraacetic acid (EDTA): the amount of substance of citric acid is than being the ratio of 1:1:1.5, and the quality of accurate weighing ethylenediamine tetraacetic acid (EDTA) and citric acid, is added in distilled water, heats and stirs, until organism dissolves;
(b) two kinds of solution that step (a) obtained mix, and 90～100
oc stirs, and by dripping ammoniacal liquor, makes the pH value of solution between 7～8, and continuous heated and stirred, until solution becomes colloidal sol shape; By the molten gelatinoid of gained 130～150
oc is dry, until it takes out after being expanded to spongy porosu solid, 350～450
oc roasting 12～24 hours; Gained solid is milled evenly, 650～750
oc roasting 5～8 hours, obtains Ce
0.8gd
0.2o
2-
δ powder;
(c) according to PrBaCo
x fe
2-
x o
5+
y stoichiometric ratio by a certain amount of Pr
2o
3, barium salt, cobalt salt and molysite join in nitre aqueous acid, heat and stir until dissolve completely; In metal ion: ethylenediamine tetraacetic acid (EDTA): the amount of substance of citric acid is than being the ratio of 1:1:1.5, and the quality of accurate weighing ethylenediamine tetraacetic acid (EDTA) and citric acid, is joined in distilled water, heats and stirs, until organism dissolves;
(d) two kinds of solution that step (c) obtained mix, and 90～100
oc stirs, and by dripping ammoniacal liquor, makes the pH value of solution between 7～8, and continuous heated and stirred, until solution becomes colloidal sol shape; By the molten gelatinoid of gained 130～150
oc is dry, until it takes out after being expanded to spongy porosu solid, 350～450
oc roasting 12～24 hours; Gained solid is milled evenly, 800～950
oc roasting 2～5 hours, obtains PrBaCo
x fe
2-
x o
5+
y powder;
(e) in mass ratio for 6:4 weighs two kinds of powders that step (b) and step (d) obtain, and in mortar, grind 3～4 hours, it is mixed, in gained powder, add appropriate oleic acid, and at 100～150MPa forming under the pressure, gained flake shaped base substrate is 1130～1180
oc roasting 5～8 hours, obtains biphase mixed conducting oxygen-permeable membrane.
Compared with prior art, the present invention has following outstanding substantive distinguishing features and advantage significantly:
Two-phase oxygen flow diaphragm two-phase prepared by the present invention is evenly distributed, and compact structure generates without dephasign, has good chemical compatibility; And there is high oxygen penetrating power, containing CO
2under atmosphere, there is good stability.
Accompanying drawing explanation
Fig. 1 is Ce prepared by the method for the invention
0.8gd
0.2o
2-
δ -PrBaCo
2o
5+
y (CG-PBC
2) X-ray diffraction (XRD) figure of each single-phase oxygen permeable film and two-phase oxygen permeable film.
Fig. 2 is Ce prepared by the method for the invention
0.8gd
0.2o
2-
δ -PrBaCo
2o
5+
y (CG-PBC
2) back scattering surface sweeping electronics (BSEM) photo of two-phase oxygen flow membrane surface.
Fig. 3 is Ce prepared by the method for the invention
0.8gd
0.2o
2-
δ -PrBaCo
2o
5+
y (CG-PBC
2) the oxygen permeating amount variation with temperature figure of two-phase oxygen permeable film.
Fig. 4 is Ce prepared by the method for the invention
0.8gd
0.2o
2-
δ -PrBaCo
2o
5+
y (CG-PBC
2) two-phase oxygen permeable film is at different CO
2oxygen permeating amount in concentration atmosphere.
Embodiment
After now specific embodiments of the invention being described in.
embodiment 1
By 39.566 g Ce (NO
3)
36H
2o and 4.129 g Gd
2o
3join in nitre aqueous acid, heat and stir until dissolve completely; In metal ion: ethylenediamine tetraacetic acid (EDTA): citric acid amount of substance is than being the ratio of 1:1:1.5, and the quality of accurate weighing ethylenediamine tetraacetic acid (EDTA) and citric acid, is added in distilled water, heats and stirs, until organism dissolves; Above-mentioned two kinds of solution are mixed, and 95
oc stirs, and by dripping ammoniacal liquor, the pH value that makes solution is 7, and continuous heated and stirred, until solution becomes colloidal sol shape; By the molten gelatinoid of gained 150
oc is dry, until it takes out after being expanded to spongy porosu solid, 400
oc roasting 18 hours; Gained solid is milled evenly, 650
oc roasting 5 hours, obtains Ce
0.8gd
0.2o
2-
δ (CG) powder;
By 18.266 g Pr (NO
3)
36H
2o, 10.976 g Ba (NO
3)
2with 24.447 g Co (NO
3)
26H
2o is dissolved in deionized water, gets 49.096 g ethylenediamine tetraacetic acid (EDTA)s and 48.419 g citric acids and is dissolved in another beaker that a certain amount of deionized water is housed, and above-mentioned two solution is mixed, and be heated to 95
oc, by dropping ammoniacal liquor, making the pH value of solution is 7, continues heating until obtain molten gelatinoid.By the molten jelly of gained 150
oc is dry, until it takes out after being expanded to spongy porosu solid, 350
oc roasting 10 hours, subsequently 850
oc roasting 5 hours, obtains PrBaCo
2o
5+
y (PBC
2) powder.According to Ce
0.8gd
0.2o
2-
δ : PrBaCo
2o
5+
y for the mass ratio of 6:4 takes corresponding powder, and in mortar, grind 3 hours, it is mixed, in gained powder, add appropriate oleic acid, and at 120MPa forming under the pressure, gained flake shaped base substrate is 1150
oc roasting 6 hours, obtains Ce
0.8gd
0.2o
2-
δ -PrBaCo
2o
5+
y (CG-PBC
2) biphase mixed conducting oxygen-permeable membrane.
embodiment 2
By the identical method of above-described embodiment 1, prepare Ce
0.8gd
0.2o
2-
δ (CG) powder.
By 18.266 g Pr (NO
3)
36H
2o, 10.976 g Ba (NO
3)
2, 18.335 g Co (NO
3)
26H
2o and 8.484 g Fe (NO
3)
39H
2o is dissolved in deionized water, gets 49.096 g ethylenediamine tetraacetic acid (EDTA)s and 48.419 g citric acids and is dissolved in another beaker that a certain amount of deionized water is housed, and above-mentioned two solution is mixed, and be heated to 95
oc, by dropping ammoniacal liquor, making the pH value of solution is 7, continues heating until obtain molten gelatinoid.By the molten jelly of gained 160
oc is dry, until it takes out after being expanded to spongy porosu solid, 400
oc roasting 12 hours, subsequently 850
oc roasting 5 hours, obtains PrBaCo
1.5fe
0.5o
5+
y (PBC
1.5f
0.5) powder.According to Ce
0.8gd
0.2o
2-
δ : PrBaCo
1.5fe
0.5o
5+
y for the mass ratio of 6:4 takes corresponding powder, and in mortar, grind 3 hours, it is mixed, in gained powder, add appropriate oleic acid, and at 120MPa forming under the pressure, gained flake shaped base substrate is 1150
oc roasting 5 hours, obtains Ce
0.8gd
0.2o
2-
δ -PrBaCo
1.5fe
0.5o
5+
y (CG-PBC
1.5f
0.5) biphase mixed conducting oxygen-permeable membrane.
embodiment 3
By the identical method of above-described embodiment 1, prepare Ce
0.8gd
0.2o
2-
δ (CG) powder.
By 18.266 g Pr (NO
3)
36H
2o, 10.976 g Ba (NO
3)
2, 12.223 g Co (NO
3)
26H
2o and 16.969 g Fe (NO
3)
39H
2o is dissolved in deionized water, gets 49.096 g ethylenediamine tetraacetic acid (EDTA)s and 48.419 g citric acids and is dissolved in another beaker that a certain amount of deionized water is housed, and above-mentioned two solution is mixed, and be heated to 95
oc, by dropping ammoniacal liquor, making the pH value of solution is 7, continues heating until obtain molten gelatinoid.By the molten jelly of gained 160
oc is dry, until it takes out after being expanded to spongy porosu solid, 400
oc roasting 12 hours, subsequently 850
oc roasting 5 hours, obtains PrBaCoFeO
5+
y (PBCF) powder.According to Ce
0.8gd
0.2o
2-
δ : PrBaCoFeO
5+
y for the mass ratio of 6:4 takes corresponding powder, and in mortar, grind 3 hours, it is mixed, in gained powder, add appropriate oleic acid, and at 120MPa forming under the pressure, gained flake shaped base substrate is 1150
oc roasting 5 hours, obtains Ce
0.8gd
0.2o
2-
δ -PrBaCoFeO
5+
y (CG-PBCF) biphase mixed conducting oxygen-permeable membrane.
embodiment 4
By the identical method of above-described embodiment 1, prepare Ce
0.8gd
0.2o
2-
δ (CG) powder.
By 18.266 g Pr (NO
3)
36H
2o, 10.976 g Ba (NO
3)
2, 6.112 g Co (NO
3)
26H
2o and 25.453 g Fe (NO
3)
39H
2o is dissolved in deionized water, gets 49.096 g ethylenediamine tetraacetic acid (EDTA)s and 48.419 g citric acids and is dissolved in another beaker that a certain amount of deionized water is housed, and above-mentioned two solution is mixed, and be heated to 95
oc, by dropping ammoniacal liquor, making the pH value of solution is 7, continues heating until obtain molten gelatinoid.By the molten jelly of gained 150
oc is dry, until it takes out after being expanded to spongy porosu solid, 400
oc roasting 15 hours, subsequently 850
oc roasting 6 hours, obtains PrBaCo
0.5fe
1.5o
5+
y (PBC
0.5f
1.5) powder.According to Ce
0.8gd
0.2o
2-
δ : PrBaCo
0.5fe
1.5o
5+
y for the mass ratio of 6:4 takes corresponding powder, and in mortar, grind 3 hours, it is mixed, in gained powder, add appropriate oleic acid, and at 120MPa forming under the pressure, gained flake shaped base substrate is 1150
oc roasting 5 hours, obtains Ce
0.8gd
0.2o
2-
δ -PrBaCo
0.5fe
1.5o
5+
y (CG-PBC
0.5f
1.5) biphase mixed conducting oxygen-permeable membrane.
embodiment 5
By the identical method of above-described embodiment 1, prepare Ce
0.8gd
0.2o
2-
δ (CG) powder.
By 18.266 g Pr (NO
3)
36H
2o, 10.976 g Ba (NO
3)
2with 33.938 g Fe (NO
3)
39H
2o is dissolved in deionized water, gets 49.096 g ethylenediamine tetraacetic acid (EDTA)s and 48.419 g citric acids and is dissolved in another beaker that a certain amount of deionized water is housed, and above-mentioned two solution is mixed, and be heated to 95
oc, by dropping ammoniacal liquor, making the pH value of solution is 7, continues heating until obtain molten gelatinoid.By the molten jelly of gained 160
oc is dry, until it takes out after being expanded to spongy porosu solid, 400
oc roasting 12 hours, subsequently 850
oc roasting 5 hours, obtains PrBaFe
2o
5+
y (PBF
2) powder.According to Ce
0.8gd
0.2o
2-
δ : PrBaFe
2o
5+
y for the mass ratio of 6:4 takes corresponding powder, and in mortar, grind 3 hours, it is mixed, in gained powder, add appropriate oleic acid, and at 120MPa forming under the pressure, gained flake shaped base substrate is 1150
oc roasting 5 hours, obtains Ce
0.8gd
0.2o
2-
δ -PrBaFe
2o
5+
y (CG-PBF
2) biphase mixed conducting oxygen-permeable membrane.
evaluation test
925
oc, air flow quantity are 300ml min
-1with helium gas flow be 100 ml min
-1under condition, Ce
0.8gd
0.2o
2-
δ -PrBaCo
2o
5+
y two-phase oxygen permeable film has obtained 2.81.1
10
-7mol s
-1cm
-2high oxygen permeating amount, in sweep gas, contain a small amount of CO
2time, it is comparatively slow that the penetrating quality of its oxygen reduces trend, has good stability.
Claims (2)
1. a biphase mixed conducting oxygen-permeable membrane material, is characterized in that, has following composition and weight percent:
Ce
0.8gd
0.2o
2-
δ oxide compound 60%
PrBaCo
x fe
2-
x o
5+
y oxide compound 40%
Described
xvalue be 0,0.5,1.0,1.5 and 2.0;
δfor Ce
0.8gd
0.2o
2-
δ oxygen room in oxide compound,
δvalue between 0 to 0.1;
yfor PrBaCo
x fe
2-
x o
5+
y oxygen room in oxide compound,
yvalue between 0 to 0.5.
2. a preparation method for biphase mixed conducting oxygen-permeable membrane material, is characterized in that, has following technological process and step:
(a) according to Ce
0.8gd
0.2o
2-
δ stoichiometric ratio by a certain amount of cerium salt and Gd
2o
3join in nitre aqueous acid, heat and stir until dissolve completely; In metal ion: ethylenediamine tetraacetic acid (EDTA): the amount of substance of citric acid is than being the ratio of 1:1:1.5, and the quality of accurate weighing ethylenediamine tetraacetic acid (EDTA) and citric acid, is added in distilled water, heats and stirs, until organism dissolves;
(b) two kinds of solution that step (a) obtained mix, and 90～100
oc stirs, and by dripping ammoniacal liquor, makes the pH value of solution between 7～8, and continuous heated and stirred, until solution becomes colloidal sol shape; By the molten gelatinoid of gained 130～150
oc is dry, until it takes out after being expanded to spongy porosu solid, 350～450
oc roasting 12～24 hours; Gained solid is milled evenly, 650～750
oc roasting 5～8 hours, obtains Ce
0.8gd
0.2o
2-
δ powder;
(c) according to PrBaCo
x fe
2-
x o
5+
y stoichiometric ratio by a certain amount of Pr
2o
3, barium salt, cobalt salt and molysite join in nitre aqueous acid, heat and stir until dissolve completely; In metal ion: ethylenediamine tetraacetic acid (EDTA): the amount of substance of citric acid is than being the ratio of 1:1:1.5, and the quality of accurate weighing ethylenediamine tetraacetic acid (EDTA) and citric acid, is joined in distilled water, heats and stirs, until organism dissolves;
(d) two kinds of solution that step (c) obtained mix, and 90～100
oc stirs, and by dripping ammoniacal liquor, makes the pH value of solution between 7～8, and continuous heated and stirred, until solution becomes colloidal sol shape; By the molten gelatinoid of gained 130～150
oc is dry, until it takes out after being expanded to spongy porosu solid, 350～450
oc roasting 12～24 hours; Gained solid is milled evenly, 800～950
oc roasting 2～5 hours, obtains PrBaCo
x fe
2-
x o
5+
y powder;
(e) in mass ratio for 6:4 weighs two kinds of powders that step (b) and step (d) obtain, and in mortar, grind 3～4 hours, it is mixed, in gained powder, add appropriate oleic acid, and at 100～150MPa forming under the pressure, gained flake shaped base substrate is 1130～1180
oc roasting 5～8 hours, obtains biphase mixed conducting oxygen-permeable membrane.
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Cited By (7)
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|---|---|---|---|---|
| CN104624063A (en) * | 2014-12-12 | 2015-05-20 | 南京工业大学 | Method for improving oxygen flux of fluorite type ion conductor membrane material |
| CN104829231A (en) * | 2015-04-14 | 2015-08-12 | 上海大学 | Fluorite-perovskite type double-phase mixing conductor oxygen-permeation membrane material and preparation method thereof |
| CN104923083A (en) * | 2015-06-04 | 2015-09-23 | 上海穗杉实业有限公司 | Stainless steel doped perovskite ceramic two-phase composite hollow fiber oxygen-permeating membrane and preparation method thereof |
| CN106083045A (en) * | 2016-06-12 | 2016-11-09 | 上海大学 | A kind of anti-CO2biphase mixed conducting oxygen-permeable membrane material of corrosion and preparation method thereof |
| CN109351134A (en) * | 2018-09-07 | 2019-02-19 | 上海大学 | Single phase mixed conductor asymmetric oxygen-permeable membrane and preparation method thereof |
| CN111389242A (en) * | 2020-03-19 | 2020-07-10 | 上海大学 | Cobalt-free anti-CO2Poisoned high oxygen-permeable biphase oxygen-permeable membrane material, its preparation method and application |
| CN113332863A (en) * | 2021-07-09 | 2021-09-03 | 辽宁石油化工大学 | Preparation method of biphase oxygen permeable membrane with high surface catalytic activity |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104624063A (en) * | 2014-12-12 | 2015-05-20 | 南京工业大学 | Method for improving oxygen flux of fluorite type ion conductor membrane material |
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| CN104829231A (en) * | 2015-04-14 | 2015-08-12 | 上海大学 | Fluorite-perovskite type double-phase mixing conductor oxygen-permeation membrane material and preparation method thereof |
| CN104923083A (en) * | 2015-06-04 | 2015-09-23 | 上海穗杉实业有限公司 | Stainless steel doped perovskite ceramic two-phase composite hollow fiber oxygen-permeating membrane and preparation method thereof |
| CN106083045A (en) * | 2016-06-12 | 2016-11-09 | 上海大学 | A kind of anti-CO2biphase mixed conducting oxygen-permeable membrane material of corrosion and preparation method thereof |
| CN109351134A (en) * | 2018-09-07 | 2019-02-19 | 上海大学 | Single phase mixed conductor asymmetric oxygen-permeable membrane and preparation method thereof |
| CN111389242A (en) * | 2020-03-19 | 2020-07-10 | 上海大学 | Cobalt-free anti-CO2Poisoned high oxygen-permeable biphase oxygen-permeable membrane material, its preparation method and application |
| CN113332863A (en) * | 2021-07-09 | 2021-09-03 | 辽宁石油化工大学 | Preparation method of biphase oxygen permeable membrane with high surface catalytic activity |
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