CN107281941A - A kind of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve and preparation method thereof - Google Patents
A kind of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve and preparation method thereof Download PDFInfo
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- CN107281941A CN107281941A CN201710487144.8A CN201710487144A CN107281941A CN 107281941 A CN107281941 A CN 107281941A CN 201710487144 A CN201710487144 A CN 201710487144A CN 107281941 A CN107281941 A CN 107281941A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
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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
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
- B01D69/06—Flat membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/44—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds, not provided for in a single one of groups B01D71/26-B01D71/42
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention belongs to technical field of membrane separation, specifically related to a kind of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve and preparation method thereof.It is characterized mainly in that：The magnetic graphene of preparation is evenly spread in chloroform, then micropore organic polymer powder is added to be stirred until homogeneous, film is scratched on polyfluortetraethylene plate, solvent evaporation method prepares a kind of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve, for separating oxygen, nitrogen.Compared to other magnetic films, magnetic graphene in the magnetic film has the magnetic property of the special two-dimensional slice structure of graphene and ferroso-ferric oxide concurrently, and be difficult to reunite in magnetic film, it is dispersed preferable, the characteristics of being all improved to gas permeability and selectivity, has important application prospect in magnetic UF membrane oxygen, nitrogen field.
Description
Technical field
The invention belongs to new and high technology and gas separation membrane preparation field, more particularly to a kind of magnetic graphene mixed-matrix
Film and preparation method thereof.
Background technology
Oxygen-enriched air is air of the oxysome fraction more than 21%, except possessing the combustion-supporting of normal air, breathing and industrial oxygen
Outside the important function such as change, also it is widely used in fields such as energy-conserving and environment-protective, medical treatment and biological products.The tradition of oxygen-enriched air is produced
Method is based on separation by deep refrigeration and pressure swing adsorption method, and both of which has the shortcomings of high energy consumption, equipment are complicated.With above method phase
There is compact conformation than, membrane technology, it is simple to operate, energy-efficient and be widely used in gas Separation Research.At present, commodity
The oxygen permeable membrane of change has very strong competitiveness in low concentration oxygen-enriched air (oxysome fraction 28~40%) preparation field, but in system
It is often uneconomic when taking highly concentrated oxygen-enriched air of the oxygen concentration more than 40%.Therefore, how the design of film physicochemical structure is passed through
With the optimization of film production process, the study hotspot that high selectivity oxygen permeable membrane is gas separation membrane preparation field all the time is obtained.
Magnetic oxygen permeable membrane is that the difference acted on by externally-applied magnetic field oxygen nitrogen molecular magnetizing force strengthens oxygen nitrogen separation process
A kind of new gas seperation film.Magnetic oxygen permeable membrane is based on mixed substrate membrane containing nano-grade molecular sieve, by Non-magnetic polymer and its scattered internal magnetic
Property particle constitute.Currently used Non-magnetic polymer is to cause with ethyl cellulose, poly- (2,6- dimethyl -1,4- phenylates)
Close polymer, magnetic particle is then with neodymium, Fe3O4、γ-Fe2O3Based on.The problem of existing magnetic oxygen permeable membrane is present mainly is magnetic
Particle is easily reunited in film, oxygen nitrogen separation selectivity is low, constrains application of the magnetic mixed substrate membrane containing nano-grade molecular sieve in oxygen nitrogen separation field.
Graphene is typical two-dimensional sheet carbon material, with synthesis is simple, specific surface area is high, mechanical performance and excellent heat stability,
Surface can functionalization the advantages of, be widely used in the fields such as gas separation, ion isolation and desalinization.Study at present
Person is loaded to metal-organic framework material ZIF-8 after graphene film layer surface, by being deposited on using graphene as carrier
Al2O3Supporter is added in polymer, prepares the relevant report of gas separation membrane.
The content of the invention
It is an object of the invention to provide a kind of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve and preparation method thereof, to overcome existing skill
The defect of art.
A kind of preparation method based on magnetic graphene mixed substrate membrane containing nano-grade molecular sieve proposed by the present invention, it is characterised in that including as follows
Step：
1~5 part of micropore organic polymer powder is dissolved in 40~50 parts of solvents by A, and magnetic agitation 3-6h forms uniform molten
Liquid；
Above-mentioned solution with after 0.2~0.8 μm of syringe filter filtering, is added 0.0005~0.02 part of magnetic graphene by B
After powder, 6~12h of ultrasonic agitation, film is scratched on tetrafluoroethene plate, film thickness is 80 μm；
Film is dried 24h and removes partial solvent by C at room temperature, is dried in vacuum drying chamber to constant weight, is obtained magnetic
Property graphene mixed substrate membrane containing nano-grade molecular sieve product.
It is preferred that, the micropore organic polymer is one in poly- schiff bases, polybenzothiozole, polybenzoxazoles or polypyrrole
Kind.
It is preferred that, the molecular weight of the micropore organic polymer is 5~60,000.
It is preferred that, the solvent is any one or a few in DMF, chloroform, tetrahydrofuran
Mixture.
It is preferred that, the magnetic graphene is graphene sheet layer area load ferriferrous oxide nano-particle, four oxidations three
Abrasive grit footpath is 30-50nm, and load capacity is 85wt%-90wt%.
The present invention also provides a kind of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve, it is characterised in that formula includes following component：Micropore
1~5 part of organic polymer, 0.005~0.02 part of magnetic graphene, 40~50 parts of solvent.
It is preferred that, the micropore organic polymer is one in poly- schiff bases, polybenzothiozole, polybenzoxazoles or polypyrrole
Kind.
It is preferred that, the molecular weight of the micropore organic polymer is 5~60,000.
It is preferred that, the solvent is any one or a few in DMF, chloroform, tetrahydrofuran
Mixture.
It is preferred that, the magnetic graphene is graphene sheet layer area load ferriferrous oxide nano-particle, four oxidations three
Abrasive grit footpath is 30-50nm, and load capacity is 85wt%-90wt%.
The magnetic graphene mixed substrate membrane containing nano-grade molecular sieve that the present invention is provided, polymeric matrix is micropore organic polymer, by covalent bond
Connect and using micropore as key structural feature, with higher gas permeation flux；The magnetic graphene of inner dispersion has stone concurrently
The magnetic property of the special two-dimensional slice structure of black alkene and ferroso-ferric oxide.Four oxidations three of graphene film layer surface in separation process
Iron produces induced magnetic field under additional magnetic fields, attracts oxygen molecule and repels nitrogen molecule, so as to significantly improve magnetic stone
Selectivity of the black alkene mixed substrate membrane containing nano-grade molecular sieve to oxygen；The semicolumn duct of the random pleated structure formation of magnetic graphene simultaneously,
Graphene oxide thin slice hole between layers and the nanometer micropore as caused by graphene oxide fault of construction are to gas point
From transmission provide extra passage, so as to significantly improve gas molecule permeance property in film；In addition magnetic graphene
Addition can also expand polymer film strand spacing, and diffusional resistance of the reduction gas molecule in magnetic mixed substrate membrane containing nano-grade molecular sieve is carried
High gas permeability.
In summary, the preparation method for a kind of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve that the present invention is provided, with advantages below：
1st, the present invention prepares magnetic graphene mixed substrate membrane containing nano-grade molecular sieve using direct blending, and filming technology is simple, easy to operate,
Production is reproducible；
2nd, the magnetic graphene conduct that the present invention is formed using graphene sheet layer area load ferriferrous oxide nano-particle
Magnetic primitive, with ferroso-ferric oxide particle diameter is small, good dispersion, the characteristics of be difficult to reunite, can effectively reduce magnetic mixed-matrix
The defect of film, improves the selectivity of gas；
3rd, the magnetic graphene mixed substrate membrane containing nano-grade molecular sieve prepared using the inventive method, due to the microcellular structure of membrane polymer matrix
With the synergy of magnetic primitive, the permeance property to oxygen is good, high to the separation selectivity of oxygen/nitrogen.
Embodiment
The following is the embodiment of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve and preparation method thereof, but the embodiment is not constituted to this
The limitation of invention.
Embodiment 1
A kind of preparation method of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve, comprises the following steps：
(1) 1 part of molecular weight is dissolved in 40 parts of DMFs for 50,000 poly- schiff bases, magnetic agitation 3h shapes
Into homogeneous solution；(2) above-mentioned solution is added into 0.005 part of magnetic graphene powder with after 0.2 μm of syringe filter filtering, its
Middle ferroso-ferric oxide particle diameter is 30nm, and after load capacity is 85wt%, ultrasonic agitation 6h, film is scratched on tetrafluoroethene plate,
Film thickness is that 80 μm (3) dry film 24h removal partial solvents at room temperature, is dried in vacuum drying chamber to perseverance
Weight, obtains magnetic graphene mixed substrate membrane containing nano-grade molecular sieve product.
A kind of above-mentioned magnetic graphene mixed substrate membrane containing nano-grade molecular sieve that is based on is separated applied to oxygen-nitrogen, oxygen preferentially passes through magnetic
Property film, measure separation factor for 2.90, oxygen permeation flux is 469Barrer.
Embodiment 2
A kind of preparation method of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve, comprises the following steps, described formula rate is by weight
Part meter：
(1) it is that 60,000 polybenzothiozole powder are dissolved in 40 parts of chloroforms by 1 part of molecular weight, magnetic agitation 5h is formed
Even solution；(2) above-mentioned solution is added into 0.01 part of magnetic graphene powder, wherein four with after 0.45 μm of syringe filter filtering
Fe 3 O particle diameter is 40nm, and load capacity is 87wt%, after ultrasonic agitation 12h, film is scratched on tetrafluoroethene plate, it is thin
Film thickness is that 80 μm (3) dry film 24h removal partial solvents at room temperature, is dried in vacuum drying chamber to constant weight,
Obtain magnetic graphene mixed substrate membrane containing nano-grade molecular sieve product.
A kind of above-mentioned magnetic graphene mixed substrate membrane containing nano-grade molecular sieve that is based on is separated applied to oxygen-nitrogen, oxygen preferentially passes through magnetic
Property film, measure separation factor for 2.73, oxygen permeation flux is 617Barrer.
Embodiment 3
A kind of preparation method of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve, comprises the following steps, described formula rate is by weight
Part meter：
(1) by 3 parts of molecular weight in the molten 50 parts of tetrahydrofurans of 5.5 ten thousand polybenzoxazoles powder, magnetic agitation 6h is formed
Even solution；(2) above-mentioned solution is added into 0.015 part of magnetic graphene powder, wherein four with after 0.8 μm of syringe filter filtering
Fe 3 O particle diameter is 50nm, and after load capacity is 89wt%, ultrasonic agitation 6h, film, film are scratched on tetrafluoroethene plate
Thickness is that 80 μm (3) dry film 24h removal partial solvents at room temperature, dries to constant weight, obtains in vacuum drying chamber
To magnetic graphene mixed substrate membrane containing nano-grade molecular sieve product.
A kind of above-mentioned magnetic graphene mixed substrate membrane containing nano-grade molecular sieve that is based on is separated applied to oxygen-nitrogen, oxygen preferentially passes through magnetic
Property film, measure separation factor for 7.07, oxygen permeation flux is 89Barrer.
Embodiment 4
A kind of preparation method of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve, comprises the following steps, described formula rate is by weight
Part meter：
(1) it is that 50,000 polypyrrole powder are dissolved in 50 parts of chloroforms and tetrahydrofuran in the mixed solvent, magnetic by 3 parts of molecular weight
Power stirring 4h formation homogeneous solutions；(2) above-mentioned solution is added into 0.02 part of magnetic graphite with after 0.4 μm of syringe filter filtering
Alkene powder, wherein ferroso-ferric oxide particle diameter are 40nm, after load capacity is 90wt%, ultrasonic agitation 12h, are scraped on tetrafluoroethene plate
Film is painted, film thickness is that 80 μm (3) dry film 24h removal partial solvents at room temperature, in vacuum drying chamber
Dry to constant weight, obtain magnetic graphene mixed substrate membrane containing nano-grade molecular sieve product.
Above-mentioned magnetic graphene mixed substrate membrane containing nano-grade molecular sieve is separated applied to oxygen-nitrogen, oxygen preferentially passes through magnetic film, infiltration
Flux is 361Barrer, and the separation factor of oxygen/nitrogen is 3.35.
Comparative example 1
A kind of preparation method of microporous polymer membranes, comprises the following steps, described formula rate is by weight：
(1) it is that 5.5 ten thousand polybenzoxazoles powder are dissolved in 40 parts of chloroforms by 5 parts of molecular weight, magnetic agitation 6h is formed
Homogeneous solution；(2) above-mentioned solution is scratched into film, film is thick with after 0.6 μm of syringe filter filtering on tetrafluoroethene plate
Spend and film is dried to 24h removal partial solvents at room temperature for 80 μm (3), dry to constant weight, obtain in vacuum drying chamber
Magnetic graphene mixed substrate membrane containing nano-grade molecular sieve product.
A kind of above-mentioned microporous polymer membranes that are based on are separated applied to oxygen-nitrogen, oxygen preferentially passes through magnetic film, measures
Separation factor is 3.39, and oxygen permeation flux is 342Barrer.
The description of above-described embodiment should be considered as explanation, it is easy to understanding, can not depart from such as in claims
Using many changes and combination of the feature being described above in the case of the present invention of middle elaboration, this kind of change is not viewed as taking off
From the spirit and scope of the present invention, and all such changes are included in the range of claims below.
Claims (10)
1. a kind of preparation method of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve, it is characterised in that comprise the following steps：
1~5 part of micropore organic polymer powder is dissolved in 40~50 parts of solvents by A, magnetic agitation 3-6h formation homogeneous solutions；
Above-mentioned solution with after 0.2~0.8 μm of syringe filter filtering, is added 0.005~0.02 part of magnetic graphene powder by B,
After 6~12h of ultrasonic agitation, film is scratched on tetrafluoroethene plate, film thickness is 80 μm；
Film is dried 24h and removes partial solvent by C at room temperature, is dried in vacuum drying chamber to constant weight, is obtained magnetic stone
Black alkene mixed substrate membrane containing nano-grade molecular sieve product.
2. a kind of preparation method of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve according to claim 1, it is characterised in that the micropore
Organic polymer is one kind in poly- schiff bases, polybenzothiozole, polybenzoxazoles or polypyrrole.
3. a kind of preparation method of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve according to claim 1-2, it is characterised in that described micro-
The molecular weight of hole organic polymer is 5~60,000.
4. a kind of preparation method of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve according to claim 1-3, it is characterised in that described molten
Agent is any one or a few mixture in N,N-dimethylformamide, chloroform, tetrahydrofuran.
5. a kind of preparation method of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve according to claim 1-4, it is characterised in that the magnetic
Property graphene be graphene sheet layer area load ferriferrous oxide nano-particle, ferroso-ferric oxide particle diameter be 30-50nm, load capacity
For 85wt%-90wt%.
6. a kind of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve, it is characterised in that formula includes following component：Micropore organic polymer 1~5
Part, 0.005~0.02 part of magnetic graphene, 40~50 parts of solvent.
7. a kind of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve according to claim 6, it is characterised in that the micropore organic polymer
For one kind in poly- schiff bases, polybenzothiozole, polybenzoxazoles or polypyrrole.
8. a kind of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve according to claim 6-7, it is characterised in that the micropore organic polymer
The molecular weight of thing is 5~60,000.
9. a kind of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve according to claim 6-8, it is characterised in that the solvent is N, N- bis-
Any one or a few mixture in NMF, chloroform, tetrahydrofuran.
10. a kind of magnetic graphene mixed substrate membrane containing nano-grade molecular sieve according to claim 6-9, it is characterised in that the magnetic graphene
For graphene sheet layer area load ferriferrous oxide nano-particle, ferroso-ferric oxide particle diameter is 30-50nm, and load capacity is
85wt%-90wt%.
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Cited By (3)
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| CN112316754A (en) * | 2020-09-24 | 2021-02-05 | 宁波方太厨具有限公司 | Anti-pollution hollow fiber ultrafiltration membrane and preparation method thereof |
| CN113289506A (en) * | 2021-06-15 | 2021-08-24 | 江南大学 | Asymmetric magnetic oxygen-nitrogen separation membrane and preparation method thereof |
| CN115463556A (en) * | 2022-08-30 | 2022-12-13 | 石河子大学 | Mixed matrix membrane based on dual-functional modified GO nanosheets and preparation method and application thereof |
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| CN115463556A (en) * | 2022-08-30 | 2022-12-13 | 石河子大学 | Mixed matrix membrane based on dual-functional modified GO nanosheets and preparation method and application thereof |
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