CN107441892A - A kind of application of two-dimentional MXene films in gas separation - Google Patents
A kind of application of two-dimentional MXene films in gas separation Download PDFInfo
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- CN107441892A CN107441892A CN201710614632.0A CN201710614632A CN107441892A CN 107441892 A CN107441892 A CN 107441892A CN 201710614632 A CN201710614632 A CN 201710614632A CN 107441892 A CN107441892 A CN 107441892A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
- B01D53/228—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
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Abstract
The invention discloses a kind of application of two-dimentional MXene films in gas separation.The application comprises the following steps：（1）Two-dimentional MXene films are put into gas fractionation unit, the mixed gas for needing to separate then is passed through in feed side；（2）Purge gass are passed through in purging survey；（3）Purge gass are passed through in gas-chromatography and detected.The MXene films of the present invention have the H of superelevation2The H of penetration, superelevation2/CO2, H2/N2,H2/CH4, H2/C3H6And H2/C3H8Separation selectivity and excellent mechanical performance, the preparation methods of two-dimentional MXene films is simple to operation, low energy consumption, low cost, high duplication, is adapted to large-scale industrial production.
Description
Technical field
The invention belongs to nanometer film and membrane gas separation field, and in particular to a kind of two-dimentional MXene films separate in gas
In application.
Background technology
Since the industrial revolution, separation is always that a considerable ring in industrial production, especially gas separate.Tradition
Gas separating technology include rectifying separation and pressure-variable adsorption etc..However, the high energy consumption of these separating technologies, complex operation,
Occupation area of equipment is big and separative efficiency is low etc..In order to solve these problems, researcher's active development High-efficiency Sustainable
Isolation technics.Wherein, membrane separation technique represents the developing direction of novel solution with its characteristics of energy-efficient.
The species of separation membrane is a lot.Organic polymer films are studied at first, however exist heat endurance difference and
The problems such as penetration is low.Subsequent occurrences of ceramic membrane solves the problems, such as the heat endurance of organic polymer films, but cost is high,
Preparation process is complicated, it is difficult to large-scale application.Therefore, a kind of preferably film should have the easy preparative and pottery of organic film simultaneously
The stability of porcelain film.
In recent years, the two-dimensional nano film using graphene oxide as representative is successfully prepared out and applied to separation neck
Domain.Two-dimensional nano film has heat endurance good, and chemical stability is strong, and mechanical performance is excellent, prepares simple, the spy such as separating property height
Point.Recently, a kind of two-dimension nano materials-MXene is successfully developed, and causes the extensive concern of scientist.Compared to normal
The graphene oxide seen, MXene have preparation process simpler, and hydrophily is more preferable, the excellent characteristics such as electric conductivity is stronger.
There is research to confirm, the MXene films of same thickness are more preferable than the separating effect of graphene oxide membrane.Therefore, two-dimentional MXene films are expected to
Broader practice prospect is shown in separation field.
Here, we develop a kind of MXene films of inexpensive, high penetration and high selectivity, and are separated for gas.
The content of the invention
In order to improve existing technology and realize important breakthrough in gas separation field, it is an object of the invention to provide
A kind of application of two-dimentional MXene films in gas separation.The two-dimentional MXene films can be used for plant hydrogen purification and carbon dioxide is caught
Obtain.
The object of the invention is achieved through the following technical solutions.
A kind of application of two-dimentional MXene films in gas separation, comprises the following steps：
（1）Two-dimentional MXene films are put into gas fractionation unit, the needs point of different dynamic diameter are then passed through in feed side
From mixed gas；
（2）Purge gass are passed through in purging survey；
（3）By step（2）Purge gass be passed through in gas-chromatography and detected, you can obtain penetration and the selection of gas with various
Property.
Preferably, the mixed gas is helium（He, 0.26nm）, hydrogen（H2,0.29nm）, carbon dioxide（CO2,
0.33nm）, oxygen（O2, 0.346nm）, nitrogen（N2, 0.364）, methane（CH4, 0.4nm）, ethene（C2H4, 0.39nm）, propane
（C2H6, 0.42nm）, propylene（C3H6, 0.4nm）And propane（C3H8, 0.43nm）One or more of, such as H2/CO2, H2/N2,
H2/CH4, H2/C2H4, H2/C2H6, H2/C3H6, H2/C3H8, C2H4 /C2H6And C3H6 /C3H8In one or more combinations.
Preferably, the flow velocity of the mixed gas is 10 ~ 1000ml/ min.
Preferably, the purge gass are one or more of nitrogen and argon gas.
Preferably, the flow velocity of the purge gass is 10 ~ 1000ml/ min.
Preferably, the gas-chromatography is Agilent 7890A gas-chromatographies.
A kind of preparation method of above-described two-dimentional MXene films, comprises the following steps：
（1）Lithium salts is mixed with acid solution, obtains mixed liquor；Three-layer laminated MAX phase powder is added in mixed liquor again, stirred
Uniformly, centrifuge washing, dry, obtain MXene powder；
（2）MXene powder is mixed with solvent, ultrasound, centrifugation, gained supernatant is containing the molten of two-dimentional MXene nanometer sheets
Liquid；
（3）By step（2）The solution that gained contains two-dimentional MXene nanometer sheets is stacked into polyethersulfone membranes by Assembling of Nanoparticles
（PES）In substrate, dry, produce two-dimentional MXene films.
Preferably, step（1）Described in lithium salts one or more of for lithium chloride, lithium bromide, lithium sulfate and lithium nitrate；
Described acid solution is one or more of phosphoric acid, sulfuric acid and nitric acid；Described MAX phases powder is Ti2AlC、V2AlC、
Ti3SiC2、Ti3AlC2、Ti4AlN3And Nb4AlC3One or more of.
Preferably, step（1）Described in lithium salts and the mass volume ratio of acid solution be 1g：(100~200)mL；The acid
The volumetric concentration of solution is 10% ~ 40%.
Preferably, step（1）Described in the quality of MAX phase powder be 100g ~ 200g
Preferably, step（1）Described in the time to stir be 24 ~ 48 hours.
Preferably, step（1）Described in the rotating speed that stirs be 50 ~ 600rpm；The rotating speed of centrifugation is 1000 ~ 8000 rpm；
The time of centrifugation is 5 ~ 100 min.
Preferably, step（1）Described in washing to be washed with deionized 2 ~ 10 times.
Preferably, step（1）Described in drying condition for air dry oven is dry, freeze-drying, in vacuum drying
It is one or more kinds of；Described drying temperature is 30 DEG C ~ 200 DEG C；The dry time is 4 ~ 48 hours.
Preferably, step（2）Described in solvent for ethanol, dimethyl sulfoxide (DMSO), water, 1-METHYLPYRROLIDONE, poly- carbonic acid
One or more of ester and dimethylformamide；Described MXene powder and the mass volume ratio of solvent are 1g：（500~2000）
ml。
Preferably, step（2）Described in ultrasonic time be 1 ~ 8 hour.
Preferably, step（2）Described in centrifugal rotational speed be 500 ~ 5000rpm；The time of centrifugation is 1 ~ 3 hour.
Preferably, step（3）Described in the concentration of solution containing two-dimentional MXene nanometer sheets be 0.05 ~ 5 mg/ml.
Preferably, step（3）Described in nanoassemble technology for spray-on process, spin coating method, natural seasoning and
One or more of vacuum filtration method.
Preferably, step（3）Described in polyethersulfone membranes（PES）The aperture of substrate be 0.5 μm, a diameter of 10 ~
500mm。
Preferably, step（3）Described in drying condition for air dry oven is dry, freeze-drying, in vacuum drying
It is one or more kinds of；Described drying temperature is 100 DEG C ~ 300 DEG C；The dry time is 10 ~ 48 hours.
A kind of two-dimentional MXene films as made from the process described above, the MXene films can be peeled off easily from substrate to be turned into
Independent unsupported film, while there is excellent flexibility and mechanical performance.
The present invention by the two-dimentional MXene films of preparation by by two-dimensional material MXene nanometer sheet self assemblies, being applied to choosing first
Selecting property gas separates, and prepared two-dimentional MXene films have high H2Penetration, high H2/CO2, H2/N2, H2/CH4, H2/C2H4, H2/
C2H6, H2/C3H6And H2/C3H8Selectivity, the MXene gas separation membranes of prepared high-sequential apply valency with very big
Value.
Compared with prior art, the invention has the advantages that：
（1）The two-dimentional MXene films of the present invention contain H for separation2Mixed gas when, have superelevation H2Penetration and high
Gas-selectively, had a good application prospect in gas separation membrane.
（2）The two-dimentional MXene films of the present invention are self-supported membrane, and without any substrate, preparation process is simple, and energy consumption is low,
Can be greatly cost-effective in practical application.
（3）The two-dimentional MXene films of the present invention, favorable repeatability, it is adapted to large-scale industrial production.
Brief description of the drawings
Fig. 1 is the penetration analysis chart that two-dimentional MXene films prepared by embodiment 1 are applied to gas separation.
Fig. 2 is the selective analysis chart that two-dimentional MXene films prepared by embodiment 1 are applied to gas separation.
Embodiment
It is further described with reference to the specific implementation of example and accompanying drawing to the present invention, but embodiments of the present invention
Not limited to this.
Embodiment 1
A kind of preparation method of two-dimentional MXene films, comprises the following steps：
（1）First by 1g lithium fluoride and 100ml hydrochloric acid solutions（Volumetric concentration 10%）Mixing, then by Ti three-layer laminated 1g3AlC2Powder
End is added in above-mentioned solution, is stirred 2h, the centrifuge washing under 1000rpm, is dried, obtain Ti3C2Powder；
（2）By 1g Ti3C2Powder mixes with 500 ml ethanol, ultrasonic 1h, 1h, gained is then centrifuged under 500rpm rotating speed
To supernatant be the solution containing two-dimentional MXene nanometer sheets, concentration 5mg/ml；
（3）By the solution of above-mentioned two-dimentional MXene nanometer sheets by spray-on process, aperture is stacked into as 0.5 μm, a diameter of 10mm's is poly-
Ether sulfone filter membrane（PES）In substrate, two-dimentional MXene films are can obtain after drying 10h at 100 DEG C in air dry oven.
Application of the two-dimentional MXene films of the present embodiment in gas separation：
Two-dimentional MXene films are put into gas fractionation unit, H is each led into feed side2/CO2、H2/N2、H2/CH4、H2/C3H6、
H2/C3H8Gaseous mixture（Flow velocity is 10ml/ min）, volume ratio is 1:1, purging survey is passed through N2（Flow velocity is 10ml/
min）It is passed through in gas-chromatography and is detected again.Experiment measures the penetrations of various gases： PH2=1201 GPU, PCO2=5
GPU, PN2=9 GPU, PCH4=1.5 GPU, PC3H6=0.95 GPU and PC3H8=0.59 GPU（1GPU= 1×10−6cm3/cm2·
sec·cmHg at STP）.As a result it is as shown in Figure 2.Separation selectivity is respectively H2/CO2：166.6, H2/N2：77.6, H2/
CH4：324, H2/C3H6：781, H2/C3H8：1101, as a result as shown in Figure 2.
Embodiment 2
A kind of preparation method of two-dimentional MXene films, comprises the following steps：
（1）First by 1g lithium bromides and 200ml hydrochloric acid solutions（Volumetric concentration 40%）Mixing, then by Ti three-layer laminated 100g3AlC2
Powder is added in above-mentioned solution, is stirred 48h, the centrifuge washing under 8000rpm, is dried, obtain Ti3C2Powder；
（2）By 1g Ti3C2Powder and 2000 ml H2O is mixed, ultrasonic 8h, and 3h processing is then centrifuged under 5000rpm rotating speed,
Resulting supernatant is the solution containing two-dimentional MXene nanometer sheets, concentration 2.5mg/ml；
（3）By the solution of above-mentioned two-dimentional MXene nanometer sheets by natural seasoning, it is 0.5 μm to be stacked into aperture, a diameter of
500mm polyethersulfone membranes（PES）In substrate, two-dimentional MXene is can obtain after drying 48h at 300 DEG C in vacuum drying chamber
Film.
Application of the two-dimentional MXene films of the present embodiment in gas separation：
Two-dimentional MXene films are put into gas fractionation unit, H is passed through in feed side2/ CH4Gaseous mixture (flow velocity 1000ml/
Min), volume ratio 1:1, purging survey is passed through N2（Flow velocity is 1000ml/ min）It is passed through in gas-chromatography and is detected.Experiment is surveyed
Hydrogen and the penetration of methane be respectively： PH2=1015 GPU、PCH4=1.7 GPU。H2/ CH4Separation selectivity be 777.
Embodiment 3
A kind of preparation method of two-dimentional MXene films, comprises the following steps：
（1）First by 1g lithium bromides and 150ml salpeter solutions（Volumetric concentration 35%）Mixing, then by Ti three-layer laminated 20g3AlC2
Powder is added in above-mentioned solution, is stirred 14h, the centrifuge washing under 2000rpm, is dried, obtain Ti3C2Powder；
（2）By 5g Ti3C2Powder mixes with 500 ml dimethyl sulfoxide (DMSO)s, ultrasonic 2h, is then centrifuged under 5000rpm rotating speed
1h processing, resulting supernatant are the solution containing two-dimentional MXene nanometer sheets, concentration 0.25mg/ml；
（3）By the solution of above-mentioned two-dimentional MXene nanometer sheets by vacuum filtration method, it is 0.5 μm to be stacked into aperture, a diameter of
100mm polyethersulfone membranes（PES）In substrate, two-dimentional MXene is can obtain after drying 12h at 80 DEG C in vacuum drying chamber
Film.
Application of the two-dimentional MXene films of the present embodiment in gas separation：
Two-dimentional MXene films are put into gas fractionation unit, H is passed through in feed side2/ C3H8Gaseous mixture (flow velocity 500ml/
Min), volume ratio 1:1, purging survey is passed through argon gas（Flow velocity is 500ml/ min）It is passed through in gas-chromatography and is detected.Experiment
The hydrogen and the penetration of methane measured is respectively： PH2=1218 GPU、PC3H8=0.89 GPU。H2/C3H8Separation selectivity be
1274.3。
Above-described embodiment is preferrred embodiment of the present invention, but the technical embodiment of the present invention is not by above-mentioned implementation
The limitation of mode, the simplification made under other any principles and Spirit Essence without departing from the present invention, change, replacement, modification,
Combination, should be equivalent substitute mode, is included within protection scope of the present invention.
Claims (6)
1. application of a kind of two-dimentional MXene films in gas separation, it is characterised in that comprise the following steps：
（1）Two-dimentional MXene films are put into gas fractionation unit, the mixed gas for needing to separate then is passed through in feed side；
（2）Purge gass are passed through in purging survey；
（3）By step（2）Purge gass be passed through in gas-chromatography and detected.
2. application according to claim 1, it is characterised in that：The mixed gas is helium, hydrogen, carbon dioxide, oxygen
It is two or more in gas, nitrogen, methane, ethene, ethane, propylene and propane.
3. application according to claim 2, it is characterised in that：The mixed gas is H2/CO2, H2/N2, H2/CH4, H2/
C2H4, H2/C2H6, H2/C3H6, H2/C3H8, C2H4 /C2H6And C3H6 /C3H8In one or more combinations.
4. application according to claim 1, it is characterised in that：The flow velocity of the mixed gas is 10 ~ 1000ml/ min.
5. application according to claim 1, it is characterised in that：The purge gass are one or more of nitrogen and argon gas.
6. application according to claim 1, it is characterised in that：The flow velocity of the purge gass is 10 ~ 1000ml/min.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108183205A (en) * | 2017-12-13 | 2018-06-19 | 中航锂电（江苏）有限公司 | A kind of sodium-ion battery flexible self-supporting electrode material and its application and preparation method |
| CN109397825A (en) * | 2018-12-03 | 2019-03-01 | 武汉市银莱制衣有限公司 | The MXene based composites and preparation method thereof for having mine toxic dust gas alarm and filtering function |
| CN109553103A (en) * | 2018-12-14 | 2019-04-02 | 华南理工大学 | A kind of two dimension self-crosslinking MXene film and preparation method thereof |
| CN109569319A (en) * | 2018-12-14 | 2019-04-05 | 华南理工大学 | A kind of application of the two dimension self-crosslinking MXene film in ion isolation |
| CN112808030A (en) * | 2020-12-23 | 2021-05-18 | 华南理工大学 | Method for electrochemically preparing self-supporting MXene-ZIF-8 composite membrane |
| CN113058446A (en) * | 2021-03-24 | 2021-07-02 | 昆明理工大学 | Preparation of black phosphorus alkene membrane and application of black phosphorus alkene membrane in gas separation |
| CN113083042A (en) * | 2021-04-12 | 2021-07-09 | 大连理工大学 | Mixed matrix membrane based on MXene/ZIF-composite material and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108183205A (en) * | 2017-12-13 | 2018-06-19 | 中航锂电（江苏）有限公司 | A kind of sodium-ion battery flexible self-supporting electrode material and its application and preparation method |
| CN109397825A (en) * | 2018-12-03 | 2019-03-01 | 武汉市银莱制衣有限公司 | The MXene based composites and preparation method thereof for having mine toxic dust gas alarm and filtering function |
| CN109553103A (en) * | 2018-12-14 | 2019-04-02 | 华南理工大学 | A kind of two dimension self-crosslinking MXene film and preparation method thereof |
| CN109569319A (en) * | 2018-12-14 | 2019-04-05 | 华南理工大学 | A kind of application of the two dimension self-crosslinking MXene film in ion isolation |
| CN109553103B (en) * | 2018-12-14 | 2021-12-21 | 华南理工大学 | Two-dimensional self-crosslinking MXene film and preparation method thereof |
| CN109569319B (en) * | 2018-12-14 | 2021-12-21 | 华南理工大学 | Application of two-dimensional self-crosslinking MXene membrane in ion separation |
| CN112808030A (en) * | 2020-12-23 | 2021-05-18 | 华南理工大学 | Method for electrochemically preparing self-supporting MXene-ZIF-8 composite membrane |
| CN112808030B (en) * | 2020-12-23 | 2022-03-29 | 华南理工大学 | Method for electrochemically preparing self-supporting MXene-ZIF-8 composite membrane |
| CN113058446A (en) * | 2021-03-24 | 2021-07-02 | 昆明理工大学 | Preparation of black phosphorus alkene membrane and application of black phosphorus alkene membrane in gas separation |
| CN113083042A (en) * | 2021-04-12 | 2021-07-09 | 大连理工大学 | Mixed matrix membrane based on MXene/ZIF-composite material and preparation method thereof |
| CN113083042B (en) * | 2021-04-12 | 2021-12-21 | 大连理工大学 | Mixed matrix membrane based on MXene/ZIF-8 composite material and preparation method thereof |
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