CN110523297A - A kind of graphene oxide composite nano filter membrane and preparation method thereof - Google Patents
A kind of graphene oxide composite nano filter membrane and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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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
- 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
- B01D71/02—Inorganic material
- B01D71/021—Carbon
Abstract
The present invention provides a kind of graphene oxide composite nano filter membranes and preparation method thereof, method is uniformly coated the following steps are included: by the graphene oxide dispersion drop for improveing the preparation of Hummers method in one side of basement membrane with spreading rod, dry, partial reduction obtains graphene oxide composite nano filter membrane.This method avoid traditional nanofiltration membrane preparation processes to the rigors of condition, and overcome the shortcomings that existing graphene oxide composite nano filter membrane preparation method is difficult to continuous large-area production, preparation method is simple, adjustability is strong, production cost is low and pollution-free, therefore is of great significance for the industrial applications of graphene oxide composite nano filter membrane.The graphene oxide composite nano filter membrane of this method preparation is 3.0~5.0bar, Na in operating pressure2SO4Solution concentration is under 1.5g/L, and water flux is 3.7~13.0kg/ (m2Hbar), salt-stopping rate is 39.1~91.8%.
Description
Technical field
The invention belongs to composite nanometer filter technical field of membrane more particularly to a kind of graphene oxide composite nano filter membrane and its preparations
Method.
Background technique
Nanofiltration (NF) be it is a kind of between ultrafiltration and it is reverse osmosis between, the pressure-driven film point that separation accuracy is 1~10nm
From process, have a wide range of applications in the industries such as water process, food, petrochemical industry, biological medicine.The preparation of nanofiltration membrane
Method mainly has L-S phase inversion, blending method, lotus electrochemical process and interfacial polymerization, at this stage, effectively prepares nanofiltration membrane and scale
The method for changing application is interfacial polymerization, is and the compound one layer polymer foil with separating property on perforated substrate
Preparation.In interfacial polymerization process, need extremely strictly to control concentration, reaction time, reaction temperature and the ring of reaction monomers
The conditions such as border humidity, which greatly increases the nanofiltration membranes of the preparation difficulty of nanofiltration membrane, and interfacial polymerization preparation although to have
The advantages that flux is high, rejection is high, but due to film surface hydrophobicity, film surface roughness and basement membrane and functional layer interaction etc.
Reason, make nanofiltration membrane antipollution and in terms of existing defects, chlorine resistance is poor, lead to film properties sharp fall,
The service life of composite nanometer filtering film is shortened, the application and development of composite nanometer filtering film are seriously constrained.
Graphene oxide (GO) is a kind of carbon material haveing excellent performance, its structure is similar to graphene, has graphene
Monolayer honeycomb shape hexaplanar structure, and oxygen-containing functional groups such as hydroxyl rich in, carboxyl, epoxy group, carbonyl have parent
It is aqueous it is good, lamella is thin, hydrone is the features such as its piece interlayer movement velocity is fast, can by adjust GO interlamellar spacing realize to solute
Retention, show excellent nanofiltration performance.Therefore, graphene oxide has become a kind of material for being used to prepare nanofiltration membrane of hot topic
Material.Currently, the preparation method of graphene oxide composite nano filter membrane mainly have vacuum filtration method, dip coating, spin-coating method, spray coating method and
LBL self-assembly method.But above-mentioned preparation method is unable to continuous large-area preparation graphene oxide composite nano filter membrane, and technique is multiple
Miscellaneous, equipment investment cost is high, it is difficult to realize industrial applications.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of graphene oxide composite nano filter membrane and preparation method thereof, it should
Method is simple, can be realized large area production.
The present invention provides a kind of preparation methods of graphene oxide composite nano filter membrane, comprising the following steps:
The graphene oxide dispersion for improveing the preparation of Hummers method is dripped in one side of basement membrane, is uniformly coated with spreading rod,
Dry, partial reduction obtains graphene oxide composite nano filter membrane.
Preferably, the concentration of the graphene oxide dispersion is 1~5.0g/L.
Preferably, the material of the basement membrane be selected from polycaprolactam, Kynoar, polysulfones, polyether sulfone, polyacrylonitrile,
Polypropylene, polyethylene, cellulose acetate class, Polyurethane, polyvinyl chloride or poly- furan alcohol.
Preferably, it is 0.1 μm poly- that the basement membrane, which is selected from polycaprolactam film, average pore size that average pore size is 0.1 μm,
The PS membrane that the polycaprolactam film or average pore size that vinylidene fluoride film, average pore size are 0.2 μm are 0.2 μm.
Preferably, the speed that the spreading rod uniformly coats is 5~13cm/s.
Preferably, the spreading rod is wire wrap spreading rod；The size of wire wrap spreading rod is 0.2~1.2mm.
Preferably, the mode of the drying is selected from naturally dry, heating, drying, vacuum drying or gas flow purging.
Preferably, the mode of the reduction is selected from ultraviolet reduction, high temperature reduction, hydrazine hydrate reduction or soda boiling reduction.
The present invention provides a kind of graphene oxide composite nano filter membranes of the preparation of preparation method described in above-mentioned technical proposal.
The present invention provides a kind of preparation methods of graphene oxide composite nano filter membrane, comprising the following steps: will improve
The graphene oxide dispersion of Hummers method preparation is dripped in one side of basement membrane, is uniformly coated with spreading rod, dry, partial reduction,
Obtain graphene oxide composite nano filter membrane.This method avoid traditional nanofiltration membrane preparation processes to the rigors of condition, and gram
The shortcomings that existing graphene oxide composite nano filter membrane preparation method is difficult to continuous large-area production is taken, preparation method is simply easy
Row, adjustability is strong, production cost is low and pollution-free, therefore has weight for the industrial applications of graphene oxide composite nano filter membrane
Want meaning.The results showed that the graphene oxide composite nano filter membrane of method preparation provided by the invention is 3.0 in operating pressure
~5.0bar, Na2SO4Solution concentration is under 1.5g/L, and water flux is 3.7~13.0kg/ (m2Hbar), salt-stopping rate is
39.1~91.8%.
Detailed description of the invention
Fig. 1 is the surface electron microscope of basement membrane and the graphene oxide composite nano filter membrane of preparation used in the embodiment of the present invention 1；
Fig. 2 is the surface electron microscope of basement membrane and the graphene oxide composite nano filter membrane of preparation used in the embodiment of the present invention 2；
Fig. 3 is the surface electron microscope of basement membrane and the graphene oxide composite nano filter membrane of preparation used in the embodiment of the present invention 3；
Fig. 4 is the surface electron microscope of basement membrane and the graphene oxide composite nano filter membrane of preparation used in the embodiment of the present invention 4；
Fig. 5 is the surface electron microscope of basement membrane and the graphene oxide composite nano filter membrane of preparation used in the embodiment of the present invention 5.
Specific embodiment
The present invention provides a kind of preparation methods of graphene oxide composite nano filter membrane, comprising the following steps:
The graphene oxide dispersion for improveing the preparation of Hummers method is dripped in one side of basement membrane, is uniformly coated with spreading rod,
Dry, partial reduction obtains graphene oxide composite nano filter membrane.
In the present invention, the preparation process of the graphene oxide of the improvement Hummers method preparation preferably includes following step
Rapid: the concentrated sulfuric acid is added beaker, a certain amount of KMnO is slowly added under magnetic agitation by 1. ice bath4, form blackish green solution, In
Certain time is stirred in ice bath；2. being slowly added to graphite, certain time is stirred under room temperature；3. transferring them to certain temperature water-bath
In, it mixes slowly, reacts certain time, form claret liquid；4. a certain amount of ice is poured into wherein after its cooling；⑤
Melt completely to ice, a certain amount of 30% hydrogen peroxide is added, is sufficiently stirred with glass bar, becomes orange-yellow dispersion liquid；6. being added pure
Water washing, flat crystal natural subsidence outwell supernatant after having clear line of demarcation, add water washing repeatedly, until it is neutral, i.e.,
Graphene oxide needed for obtaining.
In the present invention, step 1. in the concentrated sulfuric acid volume and KMnO4Mass ratio be preferably (50~200) mL:(2~
18)g；In a particular embodiment, the additive amount of the concentrated sulfuric acid is 50~200mL, KMnO4Additive amount be 2~18g.Ice bath
Middle mixing time is 0.5~2h.
In the present invention, step 2. in graphite mesh number be 50~325 mesh；The graphite and KMnO4Mass ratio it is preferred
For 1~4:2~18；In specific embodiment, the additive amount of the graphite is 1~4g.2. middle mixing time is 0~2h to step.
In the present invention, 3. middle bath temperature is 0~60 DEG C to step, the reaction time 1~for 24 hours.
In the present invention, 4. the mass ratio of middle ice and hydrogen peroxide is preferably 100~500:5~50 to step；Specific embodiment
In, step 4. in ice quality be 100~500g；Step 5. in hydrogen peroxide amount be 5~50g.
In the present invention, the concentration of the graphene oxide dispersion is preferably 1.0~5.0g/L.The present invention realizes benefit
Coating preparation nanofiltration membrane is carried out with the graphene oxide dispersion of low concentration.In a particular embodiment, the graphene oxide point
The concentration of dispersion liquid is 5.0g/L, 1.5g/L or 1.0g/L.
In the present invention, the material of the basement membrane is preferably selected from polycaprolactam, Kynoar, polysulfones, polyether sulfone, gathers
Acrylonitrile, polypropylene, polyethylene, cellulose acetate class, Polyurethane, polyvinyl chloride or poly- furan alcohol, are more preferably selected from average hole
Polycaprolactam film that diameter is 0.1 μm, the polyvinylidene fluoride film that average pore size is 0.1 μm, average pore size are 0.2 μm and gather in oneself
The PS membrane that amide film or average pore size are 0.2 μm.
In the present invention, the basement membrane preferably tiles and is fixed on film applicator；The fixed mode of tiling preferably uses transparent adhesive tape
Basement membrane is sticked on film applicator by band close to one end of spreading rod.
In the present invention, the speed that the spreading rod uniformly coats is 5~13cm/s；In a particular embodiment, the painting
The speed covered is 6cm/s, 8cm/s, 10cm/s or 12cm/s.The spreading rod is preferably wire wrap spreading rod；Wire wrap coating
The size of stick is 0.2~1.2mm；In a particular embodiment, the size of the wire wrap spreading rod be 0.2mm, 0.3mm,
0.5mm, 0.8mm or 1.0mm.
The present invention can adjust graphite oxide ene coatings according to the concentration of graphene oxide dispersion and the size of spreading rod
Thickness, adjustability is strong.
In the present invention, the mode of the drying is selected from naturally dry, heating, drying, vacuum drying or gas flow purging.Add
The temperature of heat drying is preferably 60 DEG C~80 DEG C, more preferably 70 DEG C.
In the present invention, the mode of the reduction is selected from ultraviolet reduction, high temperature reduction, hydrazine hydrate reduction or soda boiling reduction.
The present invention provides a kind of graphene oxide composite nano filter membrane of the preparation of preparation method described in above-mentioned technical proposal.It is described
Graphene oxide composite nano filter membrane is 3.0~5.0bar, Na in operating pressure2SO4Solution concentration is under 1.5g/L, and water flux is
3.7~13.0kg/ (m2Hbar), salt-stopping rate is 39.1~91.8%.
The graphene oxide composite nano filter membrane includes substrate and compound graphene oxide layer on the substrate；It is described
The thickness of substrate is preferably 100~300 μm；The thickness of the graphene oxide layer is preferably 50~200 μm.
In order to further illustrate the present invention, it is received below with reference to embodiment is compound to a kind of graphene oxide provided by the invention
Filter membrane and preparation method thereof is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
The graphene oxide of the improvement Hummers method preparation by adopting the above technical scheme, is configured to the oxidation of 5.0g/L
Graphene dispersing solution, by average pore size be 0.1 μm polyvinylidene fluoride film tiling be fixed on film applicator, by GO dispersant liquid drop in
On one side of basement membrane, GO homogeneous dispersion is coated in by plate membrane surface with the speed of 8cm/s with the spreading rod of 0.3mm,
Naturally dry, the film after drying carry out high temperature reduction, can obtain required graphene oxide composite nano filter membrane, referring to Fig. 1, figure
1 is the surface electron microscope of basement membrane and the graphene oxide composite nano filter membrane of preparation used in the embodiment of the present invention 1.
Using pressure filter commenting to prepared graphene oxide composite nano filter membrane progress water flux and salt-stopping rate
Valence.It is 4.0bar, Na in operating pressure2SO4Under conditions of solution concentration is 1.5g/L, the water flux of film is 5.9kg/ (m2·
Hbar), salt-stopping rate 74.6%.
Embodiment 2:
The graphene oxide prepared using the Hummers method of improvement, is configured to the graphene oxide dispersion of 1.5g/L, will
The polycaprolactam film tiling that average pore size is 0.1 μm is fixed on film applicator, by GO dispersant liquid drop on a side of basement membrane,
GO homogeneous dispersion is coated in by plate membrane surface with the speed of 10cm/s with the spreading rod of 0.2mm, 70 DEG C of drying will dry
Film afterwards carries out ultraviolet reduction, can obtain required graphene oxide composite nano filter membrane, referring to fig. 2, Fig. 2 is the embodiment of the present invention
The surface electron microscope of basement membrane used in 2 and the graphene oxide composite nano filter membrane of preparation.
Using pressure filter commenting to prepared graphene oxide composite nano filter membrane progress water flux and salt-stopping rate
Valence.It is 4.0bar, Na in operating pressure2SO4Under conditions of solution concentration is 1.5g/L, the water flux of film is 3.7kg/ (m2·
Hbar), salt-stopping rate is up to 91.8%.
Embodiment 3:
The graphene oxide prepared using the Hummers method of improvement, is configured to the graphene oxide dispersion of 5.0g/L, will
The polycaprolactam film tiling that average pore size is 0.2 μm is fixed on film applicator, by GO dispersant liquid drop on a side of basement membrane,
GO homogeneous dispersion is coated in by plate membrane surface with the speed of 6cm/s with the spreading rod of 0.5mm, vacuum drying will be dried
Film afterwards carries out ultraviolet reduction, can obtain required graphene oxide composite nano filter membrane, be the embodiment of the present invention referring to Fig. 3, Fig. 3
The surface electron microscope of basement membrane used in 3 and the graphene oxide composite nano filter membrane of preparation.
Using pressure filter commenting to prepared graphene oxide composite nano filter membrane progress water flux and salt-stopping rate
Valence.It is 3.0bar, Na in operating pressure2SO4Under conditions of solution concentration is 1.5g/L, the water flux of film is 4.4kg/ (m2·
Hbar), salt-stopping rate is up to 86.5%.
Embodiment 4:
The graphene oxide prepared using the Hummers method of improvement, is configured to the graphene oxide dispersion of 1.5g/L, will
The PS membrane tiling that average pore size is 0.2 μm is fixed on film applicator, by GO dispersant liquid drop on a side of basement membrane, is used
GO homogeneous dispersion is coated in plate membrane surface, naturally dry, after drying with the speed of 10cm/s by the spreading rod of 1.0mm
Film carry out high temperature reduction, required graphene oxide composite nano filter membrane can be obtained, referring to fig. 4, Fig. 4 be the embodiment of the present invention 4
The surface electron microscope of the graphene oxide composite nano filter membrane of basement membrane and preparation used.
Using pressure filter commenting to prepared graphene oxide composite nano filter membrane progress water flux and salt-stopping rate
Valence.It is 5.0bar, Na in operating pressure2SO4Under conditions of solution concentration is 1.5g/L, the water flux of film is 5.8kg/ (m2·
Hbar), salt-stopping rate 80.3%.
Embodiment 5:
The graphene oxide prepared using the Hummers method of improvement, is configured to the graphene oxide dispersion of 1.0g/L, will
The PS membrane tiling that average pore size is 0.2 μm is fixed on film applicator, by GO dispersant liquid drop on a side of basement membrane, is used
GO homogeneous dispersion is coated in plate membrane surface, gas flow purging, after drying with the speed of 12cm/s by the spreading rod of 0.8mm
Film carry out high temperature reduction, required graphene oxide composite nano filter membrane can be obtained, referring to Fig. 5, Fig. 5 is the embodiment of the present invention 5
The surface electron microscope of the graphene oxide composite nano filter membrane of basement membrane and preparation used.
Using pressure filter commenting to prepared graphene oxide composite nano filter membrane progress water flux and salt-stopping rate
Valence.It is 3.0bar, Na in operating pressure2SO4Under conditions of solution concentration is 1.5g/L, the water flux of film is 13.0kg/ (m2·
Hbar), salt-stopping rate 39.1%.
As seen from the above embodiment, the present invention provides a kind of preparation methods of graphene oxide composite nano filter membrane, including
Following steps: the graphene oxide dispersion for improveing the preparation of Hummers method is dripped in one side of basement membrane, is uniformly applied with spreading rod
It covers, dry, partial reduction obtains graphene oxide composite nano filter membrane.This method avoid traditional nanofiltration membrane preparation processes to item
The rigors of part, and overcome existing graphene oxide composite nano filter membrane preparation method and be difficult to lacking for continuous large-area production
Point, preparation method is simple, adjustability is strong, production cost is low and pollution-free, therefore for graphene oxide composite nano filter membrane
Industrial applications be of great significance.It is received the results showed that the graphene oxide of method preparation provided by the invention is compound
Filter membrane is 3.0~5.0bar, Na in operating pressure2SO4Solution concentration is under 1.5g/L, and water flux is 3.7~13.0kg/ (m2·
Hbar), salt-stopping rate is 39.1~91.8%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of graphene oxide composite nano filter membrane, comprising the following steps:
The graphene oxide dispersion for improveing the preparation of Hummers method is dripped in one side of basement membrane, is uniformly coated with spreading rod, is done
Dry, partial reduction obtains graphene oxide composite nano filter membrane.
2. preparation method according to claim 1, which is characterized in that the concentration of the graphene oxide dispersion be 1~
5.0g/L。
3. preparation method according to claim 1, which is characterized in that the material of the basement membrane is selected from polycaprolactam, gathers
Vinylidene, polysulfones, polyether sulfone, polyacrylonitrile, polypropylene, polyethylene, cellulose acetate class, Polyurethane, polyvinyl chloride or poly-
Furan alcohol.
4. according to right ask 1 described in preparation method, which is characterized in that the basement membrane, which is selected from average pore size and is 0.1 μm, gathers oneself
Polyvinylidene fluoride film, the polycaprolactam film that average pore size is 0.2 μm or the average hole that lactams film, average pore size are 0.1 μm
The PS membrane that diameter is 0.2 μm.
5. preparation method according to claim 1, which is characterized in that the speed that the spreading rod uniformly coats be 5~
13cm/s。
6. preparation method according to claim 1, which is characterized in that the spreading rod is wire wrap spreading rod；Wire wrap
The size of spreading rod is 0.2~1.2mm.
7. preparation method according to claim 1, which is characterized in that the mode of the drying is selected from naturally dry, heating
Drying, vacuum drying or gas flow purging.
8. preparation method according to claim 1, which is characterized in that the mode of the reduction is selected from ultraviolet reduction, high temperature
Reduction, hydrazine hydrate reduction or soda boiling reduction.
9. a kind of graphene oxide composite nano filter membrane of any one of claim 1~8 preparation method preparation.
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Cited By (2)
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| CN112619419A (en) * | 2020-10-23 | 2021-04-09 | 深圳前海石墨烯产业有限公司 | Composite carbon material film, composite carbon material nanofiltration membrane and preparation method |
| CN114259891A (en) * | 2022-01-14 | 2022-04-01 | 广东溢达纺织有限公司 | Graphene oxide nanofiltration membrane as well as preparation method and application thereof |
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