CN102489175A - Preparation method of ceramic/molten salt double-phase composite gas separating film - Google Patents
Preparation method of ceramic/molten salt double-phase composite gas separating film Download PDFInfo
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- CN102489175A CN102489175A CN2011104283379A CN201110428337A CN102489175A CN 102489175 A CN102489175 A CN 102489175A CN 2011104283379 A CN2011104283379 A CN 2011104283379A CN 201110428337 A CN201110428337 A CN 201110428337A CN 102489175 A CN102489175 A CN 102489175A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
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- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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Abstract
The invention discloses a preparation method of a ceramic/molten salt double-phase composite gas separating film, belonging to the technical field of preparation of functional materials. The preparation method comprises the following steps of: 1, synthesizing ceramic powder with high ion-electron conducting performance; 2, preparing a porous ceramic substrate by taking the ceramic powder, a pore forming agent and a bonding agent as raw materials; and 3, soaking the porous ceramic substrate into a molten salt bath to prepare the ceramic/molten salt double-phase composite gas separating film. The preparation method disclosed by the invention has the advantages of simple process, convenience for operating, capability of obtaining the ceramic/molten salt double-phase composite gas separating film with a CO2 separating function, suitability for separating high-temperature CO2 gas, particular suitability for separating CO2 gas exhausted from power plant flues, reduction in emission into the atmospheric air, avoidance of environmental pollution and reduction in the greenhouse effect.
Description
Technical field
The invention belongs to the functional material preparing technical field, particularly a kind of high temperature CO that can be used for
2The preparation method of the pottery/fused salt two-phase composite gas diffusion barrier that separates.
Background technology
In recent years, along with China's rapid economic development, China demonstrates the trend of accelerated growth to the demands for energy amount.According to prediction in many ways, in the following quite a long time, China still will continue rapid growth to the demands for energy amount.Huge energy resource consumption; Energy demand to China has proposed great challenge on the one hand; On the other hand; The a large amount of gas that produces also can bring certain influence to China and even Global Climate variation, wherein then is the generation of greenhouse effects to global implication, and it is becoming one of people's environmental problem of greatest concern.
Research shows, greenhouse effects be because greenhouse gases (Greenhouse Gases, a large amount of dischargings GHG) produce, GHG mainly comprises 6 kinds of gases, removes CO
2Also comprise methane (CH outward,
4), nitrogen oxide (N
2O), hydrogen fluorine carbide (HFCs), perfluorinated hydrocarbon (PFCs) and sulfur hexafluoride (SF
6), CO wherein
2Maximum to the global warming contribution.The harm that greenhouse effects bring to the mankind is comprehensive, and is multi-level, multiple dimensioned, melts or the like like unusual weather conditions, sea-level rise, glacial recession, frozen soil.
Combustion of fossil fuel is main CO
2Emission source, China is coal-fired big country, according to DOE/EIAInternational Energy Outlook (2005), the CO of China's coal combustion discharging
2Amount accounts for fossil fuel CO
278% of discharge capacity.Therefore, reduce atmosphere percent of greenhouse gases content, the control flue tail gas CO of coal-burning power plant
2Discharging is very important link.
Development and utilization based on current new forms of energy is in the starting stage, so also exist very big problem at technology and economic aspect, under these circumstances, to catch, seals up for safekeeping and the CO that technological means is correlated with such as separates
2Reduce discharging and just becoming the focus that the whole world is paid close attention to.Generally speaking, CO
2Seizure and seal up for safekeeping and all will relate to very big energy loss and energy consumption, CO simultaneously
2Separation have very strong operability and specific aim, therefore become the focus of current research.
CO
2Gas separates and comprises absorption and separation method, adsorption method of separation and membrane separation process etc.The absorption and separation method generally uses organic amine compound as absorbent, and CO is emitted in the desorb of low temperature absorption high temperature
2Thereby, accomplish CO
2Separation.U.S. Pat 2886405A utilizes the chemosorbent (K of heat
2CO
3) separation of C O
2And H
2The admixture of gas of S can be through boiling and remove the method regeneration of steam, but great energy consumption is arranged in the regenerative process.Therefore, in the current society that is the theme with environmental protection and sustainable development, the method is not widely used.
Adsorption method of separation is based on that intermolecular force between gas and the adsorbent surface realizes; Different according to action type; Can be divided into pressure swing adsorption method (PSA), transformation vacuum suction (VSA) and alternating temperature and press absorption (TSA); But their adsorption capacities and selectivity are low, and energy consumption is higher, so be not widely used.
It then is according to the selectivity different separation processes carried out of every kind of gas of mist through film that film separates, and is a kind of continous-stable, the process of easy operating.Partial pressure gradient is CO
2The motive force of film separation process, according to the difference of material, can be with being used for CO
2The film that separates is divided into organic film (polyimides, polysulfones, ethyl cellulose etc.) and inoranic membrane (γ-Al
2O
3, zeolite, carbon molecular sieve etc.).For the gas CO that discharges in the flue
2, temperature is than higher, and hundreds of even thousands of degree centigrade, organic film is used limited in this temperature range usually.And be used for CO more at present
2The inoranic membrane that separates, or need the supply of oxygen in the separation process, or the stability of high temperature membrane is affected.Therefore, we are devoted to study a kind of CO that is used for of novelty
2Pottery/fused salt two-phase the composite membrane that separates, it has very high oxygen-ion conductive simultaneously, stability that has improved high temperature two-phase composite membrane simultaneously and the demand that reduces in the air-flow oxygen.
Summary of the invention
To existing CO
2The deficiency of diffusion barrier separation aspect, the particularly improvement aspect the separation of two-phase composite membrane, the technical problem that quasi-solution of the present invention is determined is to design a kind of high temperature CO that is used for
2The preparation method of the pottery/fused salt two-phase composite gas diffusion barrier that separates.This product has the CO under effective separating high-temp
2Gas, and nontoxic pollution-free; The preparation method of this product has controllability well, and technology is simple, does not produce characteristics such as pollution.
The preparation method of a kind of pottery provided by the invention/fused salt two-phase composite gas diffusion barrier comprises the steps:
(1) synthetic a kind of LSCF ceramic powder with good ion-electron conductive performance;
Said LSCF is La
1-xSr
xCo
1-yFeyO
3-δAbbreviation, wherein x is 0.1～0.9, y is 0.1～0.9; Take by weighing raw material, adopt citric acid method, take by weighing analytically pure lanthanum nitrate, strontium nitrate, cobalt nitrate, ferric nitrate respectively according to stoichiometric proportion; After adding deionized water dissolving, add a certain amount of citric acid, mix heating and be condensed into the brown viscous fluid; Oxygen blast makes its spontaneous combustion then, obtains LSCF precursor powder, and 500～800 ℃ of following sintering promptly can obtain the LSCF powder.
(2) preparation porous ceramic matrices suitable;
1. take by weighing raw material, the raw materials by weight of preparation porous ceramic matrices suitable is the LSCF ceramic powder: 60～80%, pore creating material graphite powder: 5～20%, binding agent PVA solution: 5～25%.
2. raw material is placed in the sintering furnace in 130～250MPa compression molding drying through 1～2h ball mill mixing, is warming up to 1000～1200 ℃; Wherein between 200～500 ℃ and 600～900 ℃, heating rate is 1～2 ℃/min, and all the other heating rates with 3～5 ℃/min heat up; After being warming up to 1000～1200 ℃; Heat preservation sintering 18～24h cools to room temperature with the rate of temperature fall of 3～5 ℃/min, promptly gets porous ceramic matrices suitable.
(3) pottery/fused salt two-phase composite membrane preparation
The porous ceramic matrices suitable that (2) are obtained; Preheating 20～40min above the Muffle furnace that the fused carbonate crucible is housed; Be impregnated into 10～30min in the mixed carbonate salt bath of fusion subsequently,, obtain pottery/fused salt two-phase composite membrane after the cooling subsequently with its slow taking-up.
Adopt citric acid method to prepare the LSCF powder, the mol ratio of citric acid and metal ion sum is 1: 1～4: 1.
Said pore creating material graphite particle diameter is 0.05～0.08 μ m.
The concentration of said PVA solution is 2～4wt%, and the PVA degree of polymerization is 1000～2000.
Said mixed carbonate is Li
2CO
3, Na
2CO
3, K
2CO
3In at least two kinds, preferred following situation: Li
2CO
3, Na
2CO
3, K
2CO
3Mole percent be respectively 0～45%, 20～40%, 20～80%.
The said Muffle furnace top that the fused carbonate crucible is housed has the circular hole of diameter 60～80mm, and temperature remains on 400～500 ℃ always in the stove.
The present invention solves said a kind of high temperature CO that can be used for
2The technical scheme of the preparation method's of the pottery/fused salt two-phase composite gas diffusion barrier that separates technical problem is: design a kind of high temperature CO that can be used for
2Pottery/fused salt two-phase composite gas the diffusion barrier that separates, this two-phase composite film material can be used for CO under the high temperature by of the present invention
2Pottery/fused salt two-phase composite gas separation membrane material the preparation method who separates makes.
Beneficial effect of the present invention is:
(1) because the synthetic a kind of ceramic powder with good ion-electron conductive performance of this experiment has good oxygen-ion conductive, to CO
2Separation played good facilitation.(have good oxygen-ion conductive, through
Reaction promotes CO
2Separate).
(2) because the pore creating material that adopts is the graphite powder of sub-micron,, can form the pore of ceramic matrix, in moulding, also have the effect of lubricant, help the demoulding except in sintering process, removing.
(3) because the binding agent that adopts is PVA, except at room temperature playing the effect that improves green strength, in sintering process, between 200～500 ℃, volatilize, can also play the effect of low temperature pore-creating.
(4) porosity of porous ceramic matrices suitable can be regulated through the content of adding pore creating material graphite and the content of binding agent.
(5) carbonate content can be regulated through the length of the porous ceramic matrices suitable porosity, dip time in the two-phase composite membrane.
(6) this preparation method is simple, and is easy to operate, and the porous ceramic matrices suitable and the pottery/fused salt two-phase composite membrane of this method preparation have higher electrical conductivity and higher CO respectively
2Permeability.
Description of drawings
Fig. 1 is that the pottery/fused salt two-phase composite membrane of embodiment 2 preparations separates 900 ℃ of CO
2Air inlet face amplify 3000 times SEM (SEM) picture;
Fig. 2 is that the pottery/fused salt two-phase composite membrane of embodiment 2 preparations separates 900 ℃ of CO
2The purging face amplify 3000 times SEM (SEM) picture.
The specific embodiment
Adopting citric acid method, is a kind of ceramic powder with good ion-electron conductive performance of feedstock production with lanthanum nitrate, strontium nitrate, cobalt nitrate, ferric nitrate, glycine.Ceramic powder, pore creating material graphite, binding agent PVA with good ion-electron mixing conductivity with synthetic are the feedstock production porous ceramic matrices suitable.Porous ceramic matrices suitable with preheating is immersed in the fusion compound carbonate salt bath then, takes out cooling and obtains pottery/fused salt two-phase composite membrane.
Below in conjunction with accompanying drawing and embodiment the present invention is described further:
Embodiment 1
A kind of high temperature CO that can be used for
2The preparation method of pottery/fused salt two-phase composite membrane that gas separates, this method step is following:
(1) synthesizing ceramic powder;
Ceramic powder La among this embodiment
1-xSr
xCo
1-yFe
yO
3-δIn x, y is respectively 0.3,0.8, then the molecular formula of LSCF consists of La
0.7Sr
0.3Co
0.2Fe
0.8O
3-δ(being called for short LSCF7328), take by weighing raw material, adopt citric acid method, take by weighing analytically pure lanthanum nitrate respectively according to stoichiometric proportion, strontium nitrate, cobalt nitrate, ferric nitrate, each amount of substance sum is 0.03mol, the water that adds 20ml dissolves.Add a certain amount of citric acid; Wherein the mol ratio of citric acid and metal ion is 2.5: 1, and heating begins oxygen blast constantly and makes its spontaneous combustion after concentrating 13h one-tenth brown viscous fluid; Obtain LSCF7328 precursor powder, 700 ℃ of following sintering can obtain the LSCF7328 ceramic powder.
(2) preparation LSCF7328 porous ceramic matrices suitable
With the LSCF7328 powder that obtains in 75% step (1), 15% pore creating material graphite and 10% concentration are the PVA aqueous solution of 3.5wt% according to percentage by weight, and the three carries out batch mixing; Be the moulding of 180MPa pressed at pressure then, drying is placed in the sintering furnace, is warming up to 1000 ℃; Wherein between 200～500 ℃ and 600～900 ℃, heating rate is 2 ℃/min, and all the other heating rates with 3 ℃/min heat up; After being warming up to 1000 ℃; Heat preservation sintering 20h cools to room temperature with the rate of temperature fall of 5 ℃/min, promptly gets the LSCF7328 porous ceramic matrices suitable.The LSCF7328 porous ceramics porosity of preparation is 36.5%, and under 700 ℃, 800 ℃ and 900 ℃ of conditions, its electrical conductivity is respectively 375.800S/cm, 320.500S/cm and 275.853S/cm.
(3) pottery/fused salt two-phase composite membrane preparation
With the LSCF7328 porous ceramic matrices suitable that (2) obtain, preheating 30min above Muffle furnace is immersed in then and contains Li earlier
2CO
3/ Na
2CO
3/ K
2CO
3Flood 25min in (mole percent is respectively 40%, 35%, 25%) mixed liquor,, obtain pottery/fused salt two-phase composite membrane after the cooling subsequently with its slow taking-up.
Pottery/fused salt two-phase the composite membrane of preparation is CO under 700 ℃, 800 ℃ and 900 ℃ of conditions
2Permeability is respectively 0.65 * 10
-8Mol/m
2.Pa.s, 1.72 * 10
-8Mol/m
2.Pa.s with 3.89 * 10
-8Mol/m
2.Pa.s.
Embodiment 2
A kind of high temperature CO that can be used for
2The preparation method of pottery/fused salt two-phase composite membrane that gas separates, this method step is following:
(1) synthetic LSCF ceramic powder;
Ceramic powder La in this experiment
1-xSr
xCo
1-yFe
yO
3-δIn x, y is respectively 0.4,0.2, then the molecular formula of LSCF consists of La
0.6Sr
0.4Co
0.8Fe
0.2O
3-δ(being called for short LSCF6482), take by weighing raw material, adopt citric acid method, take by weighing analytically pure lanthanum nitrate, strontium nitrate, cobalt nitrate, ferric nitrate respectively according to stoichiometric proportion, each amount of substance sum is 0.02mol, the water that adds 10ml dissolves.Add a certain amount of citric acid; Wherein the mol ratio of citric acid and metal ion is 2: 1, and heating begins continuous oxygen blast and makes its spontaneous combustion after concentrating 12h one-tenth brown viscous fluid; Obtain LSCF6482 precursor powder, 650 ℃ of following sintering can obtain the LSCF6482 ceramic powder.
(2) preparation LSCF6482 porous ceramic matrices suitable
With the LSCF6482 powder that obtains in 79% step (1), the concentration that adds 13% pore creating material graphite and 8% is the PVA aqueous solution of 3.5wt% according to percentage by weight, and the three carries out batch mixing; Be the moulding of 160MPa pressed at pressure then, drying is placed in the sintering furnace, is warming up to 1200 ℃; Wherein between 200～500 ℃ and 600～900 ℃, heating rate is 1 ℃/min, and all the other heating rates with 4 ℃/min heat up; After being warming up to 1200 ℃; Heat preservation sintering 24h cools to room temperature with the rate of temperature fall of 5 ℃/min, promptly gets the LSCF6482 porous ceramic matrices suitable.The LSCF6482 porous ceramics porosity of preparation is 40.8%, and under 700 ℃, 800 ℃ and 900 ℃ of conditions, its total conductivity is respectively 392.990S/cm, 338.499S/cm and 288.743S/cm.
(3) pottery/fused salt two-phase composite membrane preparation
With the LSCF6482 porous ceramic matrices suitable that (2) obtain, preheating 30min above Muffle furnace is immersed in then and contains Li earlier
2CO
3/ Na
2CO
3/ K
2CO
3Flood 25min in (mole percent is respectively 40%, 30%, 30%) mixed liquor,, obtain pottery/fused salt two-phase composite membrane after the cooling subsequently with its slow taking-up.
Pottery/fused salt two-phase the composite membrane of preparation is CO under 700 ℃, 800 ℃ and 900 ℃ of conditions
2Permeability is respectively 0.73 * 10
-8Mol/m
2.Pa.s, 1.84 * 10
-8Mol/m
2.Pa.s with 4.70 * 10
-8Mol/m
2.Pa.s.
Fig. 1 is that the pottery/fused salt two-phase composite membrane air blowing face of embodiment 2 preparations amplifies 3000 times SEM (SEM) picture, has the platelet of a lot of LSCF to exist among the figure.Fig. 2 is that pottery/fused salt two-phase composite membrane scavenging face of embodiment 2 preparations amplifies 3000 times SEM (SEM) picture, can find out that relatively air blowing face has very big difference with scavenging face pattern, and this is owing to CO under the high temperature
2Chemical reaction has taken place with certain component of composite membrane.
Claims (7)
1. the preparation method of pottery/fused salt two-phase composite gas diffusion barrier is characterized in that this method step is following,
(1) synthetic LSCF ceramic powder;
Said LSCF is La
1-xSr
xCo
1-yFe
yO
3-δAbbreviation, wherein x is 0.1～0.9, y is 0.1～0.9, takes by weighing raw material; Adopt citric acid method, take by weighing analytically pure lanthanum nitrate, strontium nitrate, cobalt nitrate, ferric nitrate respectively according to stoichiometric proportion, add deionized water dissolving after; Add citric acid, mix heating and be condensed into the brown viscous fluid, oxygen blast makes its spontaneous combustion then; Obtain LSCF precursor powder, 500～800 ℃ of following sintering obtain the LSCF ceramic powder;
(2) preparation porous ceramic matrices suitable;
1. take by weighing raw material, the raw materials by weight of preparation porous ceramic matrices suitable is the ceramic powder that step (1) is synthetic: 60～80%, pore creating material graphite powder: 5～20%, binding agent PVA solution: 5～25%.
2. raw material is placed in the sintering furnace in 130～250MPa compression molding drying through 1～2h ball mill mixing, is warming up to 1000～1200 ℃; Wherein between 200～500 ℃ and 600～900 ℃, heating rate is 1～2 ℃/min, and all the other heating rates with 3～5 ℃/min heat up; After being warming up to 1000～1200 ℃; Heat preservation sintering 18～24h cools to room temperature with the rate of temperature fall of 3～5 ℃/min, obtains porous ceramic matrices suitable;
(3) pottery/fused salt two-phase composite membrane preparation
The porous ceramic matrices suitable that (2) are obtained; Preheating 20～40min above the Muffle furnace that the fused carbonate crucible is housed; Be impregnated into 10～30min in the mixed carbonate salt bath of fusion subsequently,, obtain pottery/fused salt two-phase composite membrane after the cooling subsequently with its slow taking-up.
2. the preparation method of pottery according to claim 1/fused salt two-phase composite gas diffusion barrier is characterized in that the mol ratio of citric acid and metal ion sum is 1: 1～4: 1.
3. the preparation method of pottery according to claim 1/fused salt two-phase composite gas diffusion barrier is characterized in that said pore creating material graphite particle diameter is 0.05～0.08 μ m.
4. the preparation method of pottery according to claim 1/fused salt two-phase composite gas diffusion barrier is characterized in that the concentration of said binding agent PVA solution is 2～4wt%, and the PVA degree of polymerization is 1000～2000.
5. the preparation method of pottery according to claim 1/fused salt two-phase composite gas diffusion barrier is characterized in that said fused salt is Li
2CO
3, Na
2CO
3, K
2CO
3In at least two kinds.
6. the preparation method of pottery according to claim 1/fused salt two-phase composite gas diffusion barrier is characterized in that Li
2CO
3, Na
2CO
3, K
2CO
3Mole percent be respectively 0～45%, 20～40%, 20～80%.
7. the preparation method of pottery according to claim 1/fused salt two-phase composite gas diffusion barrier is characterized in that, the said Muffle furnace top that the fused carbonate crucible is housed has the circular hole of diameter 60～80mm, and temperature remains on 400～500 ℃ always in the stove.
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Cited By (6)
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|---|---|---|---|---|
| CN105016714A (en) * | 2015-07-09 | 2015-11-04 | 上海大学 | CO2-resistant perovskite type oxygen-permeable membrane material and preparation method therefor |
| CN105349112A (en) * | 2014-08-18 | 2016-02-24 | 武汉理工大学 | Molten salt/ceramic composite heat accumulator used at high temperature, and preparation method thereof |
| CN106669437A (en) * | 2017-01-16 | 2017-05-17 | 中国矿业大学(北京) | Preparation method of novel high-efficiency biphase CO2 electrochemical separation membrane |
| CN111842853A (en) * | 2020-07-30 | 2020-10-30 | 南昌工程学院 | Porous metal ceramic matrix composite material for preparing self-lubricating bearing and preparation method thereof |
| CN112546878A (en) * | 2021-01-21 | 2021-03-26 | 内蒙古工业大学 | Ceramic-carbonate compact two-phase inorganic membrane with ceramic material as support |
| CN116199513A (en) * | 2023-04-28 | 2023-06-02 | 内蒙古工业大学 | Three-layer ceramic carbonate biphase film with sandwich structure, and preparation method and application thereof |
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|---|---|---|---|---|
| CN105349112A (en) * | 2014-08-18 | 2016-02-24 | 武汉理工大学 | Molten salt/ceramic composite heat accumulator used at high temperature, and preparation method thereof |
| CN105349112B (en) * | 2014-08-18 | 2019-03-15 | 武汉理工大学 | A kind of high temperature fused salt/Ceramic Composite heat storage and preparation method thereof |
| CN105016714A (en) * | 2015-07-09 | 2015-11-04 | 上海大学 | CO2-resistant perovskite type oxygen-permeable membrane material and preparation method therefor |
| CN106669437A (en) * | 2017-01-16 | 2017-05-17 | 中国矿业大学(北京) | Preparation method of novel high-efficiency biphase CO2 electrochemical separation membrane |
| CN106669437B (en) * | 2017-01-16 | 2019-04-05 | 中国矿业大学(北京) | A kind of efficient two-phase CO2Electrochemical separation membrane preparation method |
| CN111842853A (en) * | 2020-07-30 | 2020-10-30 | 南昌工程学院 | Porous metal ceramic matrix composite material for preparing self-lubricating bearing and preparation method thereof |
| CN111842853B (en) * | 2020-07-30 | 2022-02-01 | 南昌工程学院 | Porous metal ceramic matrix composite material for preparing self-lubricating bearing and preparation method thereof |
| CN112546878A (en) * | 2021-01-21 | 2021-03-26 | 内蒙古工业大学 | Ceramic-carbonate compact two-phase inorganic membrane with ceramic material as support |
| CN116199513A (en) * | 2023-04-28 | 2023-06-02 | 内蒙古工业大学 | Three-layer ceramic carbonate biphase film with sandwich structure, and preparation method and application thereof |
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Application publication date: 20120613 |