CN110373028A - A kind of nano molybdenum disulfide composite membrane and preparation method thereof - Google Patents
A kind of nano molybdenum disulfide composite membrane and preparation method thereof Download PDFInfo
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- CN110373028A CN110373028A CN201910628972.8A CN201910628972A CN110373028A CN 110373028 A CN110373028 A CN 110373028A CN 201910628972 A CN201910628972 A CN 201910628972A CN 110373028 A CN110373028 A CN 110373028A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2381/06—Polysulfones; Polyethersulfones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
Abstract
The present invention relates to technology field of membrane materials, and in particular to a kind of nano molybdenum disulfide composite membrane and preparation method thereof.Nano molybdenum disulfide composite membrane provided by the invention prepares raw material including following mass fraction: 9~26 parts of high molecular polymer；0.1~10 part of molybdenum disulfide nano sheet；0~20 part of pore-foaming agent；60~90 parts of organic solvent.Present invention material of preparing based on high molecular polymer, molybdenum disulfide nano sheet is introduced directly into wherein without carrying out other modifications, molybdenum disulfide nano sheet can construct convenient water transmission channel, permeance property is improved, makes the nano molybdenum disulfide composite membrane being prepared that also there is higher water flux while there is higher rejection.
Description
Technical field
The present invention relates to technology field of membrane materials, and in particular to a kind of nano molybdenum disulfide composite membrane and preparation method thereof.
Background technique
Seperation film is a kind of membranous type material that ability is penetrated with selectivity, can usually be divided by separating mechanism and the scope of application
For microfiltration membranes, ultrafiltration membrane, nanofiltration membrane etc., environmental protection, in terms of have a wide range of applications.Currently,
It include Kynoar (PVDF), polyamide-imides (PAI), polyetherimide (PEI), sea there are commonly mechanism membrane material
The high molecular materials such as mosanom (SA).Water flux, molecular cut off, anti-fouling performance are the main indicators for characterizing film properties.It is logical
Often, when increase using the membrane material water flux of above-mentioned high molecular material preparation, rejection is decline.Therefore, in not shadow
The main target that water flux is current most of industrialized production films is improved in the case where ringing rejection as far as possible.
Summary of the invention
It is provided by the invention to receive the purpose of the present invention is to provide a kind of nano molybdenum disulfide composite membrane and preparation method thereof
Rice molybdenum disulfide composite membrane also has higher water flux while having higher rejection.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of nano molybdenum disulfide composite membranes, prepare raw material including following mass fraction:
Preferably, the high molecular polymer includes polyether sulfone, polysulfones, Kynoar, polypropylene, polyethylene, polychlorostyrene
One of ethylene, cellulose acetate, polyacrylonitrile, polyimides, polyamide-imides, polyetherimide and sodium alginate
Or it is several.
Preferably, thickness≤15nm of the molybdenum disulfide nano sheet, piece diameter size≤2 μm.
Preferably, the pore-foaming agent includes in polyethylene glycol, polyvinylpyrrolidone, glycerine, propylene glycol and acetone
It is one or more of.
Preferably, the organic solvent includes n,N-Dimethylformamide, n,N-dimethylacetamide, N- crassitude
One or more of ketone and dimethyl sulfoxide.
Preferably, the nano molybdenum disulfide composite membrane with a thickness of 0.1~0.3mm.
The present invention provides the preparation methods of any one of above-mentioned technical proposal nano molybdenum disulfide composite membrane, including with
Lower step:
Nano molybdenum disulfide composite membrane is prepared into deaeration after raw material mixes, obtains casting solution；
The casting solution striking is formed into wet film, inversion of phases film forming is carried out after precuring, it is compound to obtain nano molybdenum disulfide
Film.
Preferably, the deaeration carries out under closed, static conditions；The temperature of the deaeration is 50~80 DEG C, the time 2
~for 24 hours.
Preferably, the precuring carries out in air atmosphere；The temperature of the precuring be 0~80 DEG C, the time be 1~
90s。
Preferably, the temperature of the inversion of phases film forming is 15~32 DEG C, and the time is 2s~48h.
The present invention provides a kind of nano molybdenum disulfide composite membranes, prepare raw material including following mass fraction: macromolecule
9~26 parts of polymer；0.1~10 part of molybdenum disulfide nano sheet；0~20 part of pore-foaming agent；60~90 parts of organic solvent.The present invention with
Molybdenum disulfide nano sheet is introduced directly into wherein without carrying out at other modifications by material of preparing based on high molecular polymer
Reason, molybdenum disulfide nano sheet can construct convenient water transmission channel, improve permeance property, make two sulphur of nanometer being prepared
Changing molybdenum composite membrane also has higher water flux while having higher rejection.
The present invention provides the preparation methods of the nano molybdenum disulfide composite membrane, comprising the following steps: by two sulphur of nanometer
The deaeration after preparing raw material mixing for changing molybdenum composite membrane, obtains casting solution；The casting solution striking is formed into wet film, precuring is laggard
Row inversion of phases film forming, obtains nano molybdenum disulfide composite membrane.Preparation method provided by the invention is easy to operate, molybdenum disulfide nano
Piece is directly film-made after raw material mixes with other prepare without complicated modification, and raw material is easy to get, high degree of automation,
Suitable for large-scale industrial production.
Detailed description of the invention
Fig. 1 is the surface scan electron microscope of membrane material prepared by embodiment 1；
Fig. 2 is the cross-sectional scans electron microscope of membrane material prepared by embodiment 1；
Fig. 3 is the pure water flux of membrane material prepared by Examples 1 to 3 and comparative example 1 and the rejection to bovine serum albumin
Datagram；
Fig. 4 is the pure water flux datagram of membrane material prepared by embodiment 4 and comparative example 2；
Fig. 5 is the pure water flux of membrane material prepared by embodiment 5 and comparative example 3 and the rejection data to bovine serum albumin
Figure.
Specific embodiment
The present invention provides a kind of nano molybdenum disulfide composite membranes, prepare raw material including following mass fraction:
The raw material for preparing of nano molybdenum disulfide composite membrane provided by the invention includes 9~26 parts of high molecular polymer, preferably
It is 12~23 parts, more preferably 15~20 parts.The present invention does not have the molecular weight of the high molecular polymer and specific type
There is special restriction, using the high molecular polymer well known to those skilled in the art for being suitable for preparing membrane material.At this
In invention, the high molecular polymer preferably include polyether sulfone, polysulfones, Kynoar, polypropylene, polyethylene, polyvinyl chloride,
One of cellulose acetate, polyacrylonitrile, polyimides, polyamide-imides, polyetherimide and sodium alginate are several
Kind, more preferably polyether sulfone, polysulfones, Kynoar, polypropylene, polyethylene, polyvinyl chloride, cellulose acetate, polyacrylonitrile,
Polyimides, polyamide-imides, polyetherimide or sodium alginate, further preferably polyether sulfone, Kynoar or poly-
Vinylpyrrolidone.
On the basis of the mass fraction of the high molecular polymer, the system of nano molybdenum disulfide composite membrane provided by the invention
Standby raw material includes 0.1~10 part of molybdenum disulfide nano sheet, preferably 0.5~7 part, more preferably 1~5 part.In the present invention, institute
State molybdenum disulfide nano sheet thickness preferably≤15nm, more preferably 5~10nm；Piece diameter size preferably≤2 μm, more preferably
0.5~1.5 μm.In the present invention, described diameter size refers specifically to the size of the longest diameter inside by molybdenum disulfide nano sheet.
The present invention by add a small amount of molybdenum disulfide nano sheet can make nano molybdenum disulfide composite membrane rejection with higher and
Water flux, production cost is low, is conducive to industrial applications；The present invention preferably controls the size of molybdenum disulfide nano sheet in above range
It is interior, be conducive to molybdenum disulfide nano sheet and prepare evenly dispersed in raw material other, guarantees it in nano molybdenum disulfide composite membrane
Microeffect is preferably played, nano molybdenum disulfide composite membrane rejection with higher and water flux are further made.
On the basis of the mass fraction of the high molecular polymer, the system of nano molybdenum disulfide composite membrane provided by the invention
Standby raw material includes 0~20 part of pore-foaming agent, preferably 0.5~15 part, more preferably 1~10 part, further preferably 3~8 parts.?
In the present invention, the pore-foaming agent preferably includes one in polyethylene glycol, polyvinylpyrrolidone, glycerine, propylene glycol and acetone
Kind is several, more preferably polyethylene glycol, polyvinylpyrrolidone, glycerine, propylene glycol or acetone.The present invention passes through pore-foaming agent
Improve other compatibilities for preparing raw material, merge each raw material for preparing sufficiently, advantageously forms logical with higher rejection and water
The nano molybdenum disulfide composite membrane of amount.
On the basis of the mass fraction of the high molecular polymer, the system of nano molybdenum disulfide composite membrane provided by the invention
Standby raw material includes 60~90 parts of organic solvent, preferably 65~85 parts, more preferably 70~80 parts.In the present invention, described to have
Solvent preferably includes in N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone and dimethyl sulfoxide
One or more, more preferably n,N-Dimethylformamide, n,N-dimethylacetamide, N-Methyl pyrrolidone or dimethyl
Sulfoxide.The present invention selects above-mentioned organic solvent that can other raw materials that prepare sufficiently dissolves, disperses, and guarantee nano molybdenum disulfide is answered
Close the smooth preparation of film.
In the present invention, the thickness of the nano molybdenum disulfide composite membrane is preferably 0.1~0.3mm.
The present invention provides the preparation methods of nano molybdenum disulfide composite membrane described in above-mentioned technical proposal, including following step
It is rapid:
Nano molybdenum disulfide composite membrane is prepared into deaeration after raw material mixes, obtains casting solution；
The casting solution striking is formed into wet film, inversion of phases film forming is carried out after precuring, it is compound to obtain nano molybdenum disulfide
Film.
The present invention prepares deaeration after raw material mixes for nano molybdenum disulfide composite membrane, obtains casting solution.In the present invention,
The nano molybdenum disulfide composite membrane prepare raw material mixing preferably molybdenum disulfide nano sheet is mixed with organic solvent it is laggard
Row ultrasonic treatment, to realize the abundant removing and dispersion of molybdenum disulfide nano sheet, then again by gained molybdenum disulfide nano sheet point
Dispersion liquid and residue prepare raw material (i.e. high molecular polymer or high molecular polymer and pore-foaming agent) mixing.In the present invention, institute
The power for stating ultrasonic treatment is preferably 200~700W, more preferably 350~500W；Time is preferably 2~80h, and more preferably 8
~50h, further preferably 15~30h.In the present invention, in order to accelerate the rate of dissolution of high molecular polymer, two sulphur
Change molybdenum nanometer sheet dispersion liquid and with residue prepare raw material and mix and preferably carried out under the conditions of 50~85 DEG C, specifically, being to described two
Residue is added in molybdenum sulfide nanometer sheet dispersion liquid and prepares raw material, is subsequently placed in baking oven, the temperature for controlling baking oven is 50~85 DEG C,
Stirring is completely dissolved to high molecular polymer, and it is abundant respectively to prepare raw material mixing.
In the present invention, the deaeration preferably carries out under closed, static conditions；The present invention is for providing confined condition
Mode does not have special restriction, specifically, each mixture for preparing raw material can be placed in closed container.In the present invention,
The temperature of the deaeration is preferably 50~80 DEG C, more preferably 55~75 DEG C, further preferably 60~70 DEG C；Time is preferably
2~for 24 hours, more preferably 4~20h, further preferably 8~15h.The present invention carries out deaeration under the above conditions, is conducive to make
Micro-bubble sufficiently removes, convenient for gained casting solution to be formed to the wet film of high quality by subsequent striking.
After obtaining casting solution, the casting solution striking is formed wet film by the present invention, and inversion of phases film forming is carried out after precuring, is obtained
To nano molybdenum disulfide composite membrane.The present invention is not special for the concrete operations mode that the casting solution striking is formed wet film
Restriction, using mode of operation well known to those skilled in the art.In an embodiment of the present invention, specifically by 40~60
DEG C casting solution be placed in hopper, using clearance gauge control thickness, using polyester non-woven fabric as supporting layer, with scraper in polyester non-woven fabric
Striking is carried out on supporting layer, to form wet film on polyester non-woven fabric supporting layer.The present invention does not have the thickness of the wet film
There is special restriction, can guarantee that the thickness of final gained nano molybdenum disulfide composite membrane meets necessary requirement.
In the present invention, the precuring carries out preferably in air atmosphere；The temperature of the precuring is preferably 0~80
DEG C, more preferably 10~60 DEG C, further preferably 20~40 DEG C；Time is preferably 1~90s, more preferably 10~60s, into
One step is preferably 20~40s.In the present invention, in the procuring process, organic solvent can volatilize, and gas enters wet in air
In film, the generation of fenestra in auxiliary molybdenum disulfide nano sheet control nano molybdenum disulfide composite membrane；By the temperature for controlling precuring
Degree and time can guarantee that molecular cut off, the water flux etc. of final gained nano molybdenum disulfide composite membrane meet necessary requirement.
In the present invention, the coagulation bath composition that the inversion of phases film forming uses is preferably that water or organic solvent-water mixing are molten
Liquid；Organic solvent preferably includes N,N-dimethylformamide, N, N- dimethylacetamide in the organic solvent-water mixed solution
One or more of amine, N-Methyl pyrrolidone and dimethyl sulfoxide, more preferably n,N-Dimethylformamide, N, N- diformazan
Yl acetamide, N-Methyl pyrrolidone or dimethyl sulfoxide；The type of organic solvent can in the organic solvent-water mixed solution
It, can also be inconsistent with consistent with the type of organic solvent in the compound film preparation raw material of nano molybdenum disulfide；The organic solvent-
In water mixed solution organic solvent volume content preferably≤20%, more preferable 5~15%.It is certain that the present invention preferably passes through addition
The organic solvent of amount is conducive to the generation for assisting fenestra in molybdenum disulfide nano sheet control nano molybdenum disulfide composite membrane, makes film
Hole has suitable pore size and form, and then advantageously forms the nano molybdenum disulfide composite membrane of high quality.
In the present invention, the temperature of the inversion of phases film forming is preferably 15~32 DEG C, and more preferably 20~25 DEG C；Time is excellent
It is selected as 2s~48h, more preferably 10min~for 24 hours, further preferably 1~12h.In an embodiment of the present invention, specifically,
Be be placed on the wet film precuring 15~32 DEG C water or organic reagent-water mixed solution in carry out inversion of phases film forming 2s~
48h obtains nano molybdenum disulfide composite membrane.
Use the nano molybdenum disulfide composite membrane of above method preparation provided by the invention for microfiltration membranes or ultrafiltration membrane, color
Gray, surface is smooth, has no obvious nanoparticle agglomerates, the addition of molybdenum disulfide nano sheet is in not expendable film rejection
The water flux of film is improved under the premise of energy.
Below in conjunction with the embodiment in the present invention, the technical solution in the present invention is clearly and completely described.It is aobvious
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1
0.6g molybdenum disulfide nano sheet (with a thickness of 5~10nm, piece diameter is having a size of 0.5~1.5 μm) is added to 47gN, N-
In dimethyl acetamide, then the ultrasound 15h under 350W power condition is added 19g polyether sulfone, gained mixture is placed in 60 DEG C
Stirring and dissolving in baking oven, then deaeration (temperature is 60 DEG C, time 8h) under closed, static conditions, obtains casting solution；
60 DEG C of the casting solution is placed in hopper, controls thickness using clearance gauge, is supported with scraper in polyester non-woven fabric
Layer on carry out striking, form wet film on polyester non-woven fabric supporting layer, in air atmosphere carry out precuring (temperature be 30 DEG C,
Time is 60s), be then immersed in 25 DEG C of water carry out inversion of phases film forming for 24 hours, obtain nano molybdenum disulfide composite membrane (with a thickness of
0.2mm, ultrafiltration membrane).
Embodiment 2
Membrane material is prepared according to the method for embodiment 1, the difference is that, the additive amount of molybdenum disulfide nano sheet is
0.34g。
Embodiment 3
Membrane material is prepared according to the method for embodiment 1, the difference is that, the additive amount of molybdenum disulfide nano sheet is
1.0g。
Embodiment 4
0.5g molybdenum disulfide nano sheet (with a thickness of 5~10nm, piece diameter is having a size of 0.5~1.5 μm) is added to 74gN, N-
In dimethyl acetamide, then 13.5g Kynoar and 0.5g polyethylene glycol is added in the ultrasound 10h under 500W power condition,
Gained mixture is placed in stirring and dissolving in 75 DEG C of baking ovens, then (temperature is 70 DEG C, the time for deaeration under closed, static conditions
For 5h), casting solution is obtained；
60 DEG C of the casting solution is placed in hopper, controls thickness using clearance gauge, is supported with scraper in polyester non-woven fabric
Layer on carry out striking, form wet film on polyester non-woven fabric supporting layer, in air atmosphere carry out precuring (temperature be 80 DEG C,
Time is 40s), it is then immersed in 30 DEG C of the n,N-dimethylacetamide aqueous solution (volume ratio of n,N-dimethylacetamide and water
To carry out inversion of phases film forming 10h in 5:95), obtain nano molybdenum disulfide composite membrane (with a thickness of 0.1mm, microfiltration membranes).
Embodiment 5
0.7g molybdenum disulfide nano sheet (with a thickness of 5~10nm, piece diameter is having a size of 0.5~1.5 μm) is added to 75gN- first
In base pyrrolidones, then 17g polysulfones and 2g polyvinylpyrrolidone is added, by gained in the ultrasound 20h under 500W power condition
Mixture is placed in stirring and dissolving in 80 DEG C of baking ovens, then deaeration (temperature is 50 DEG C, time 10h) under closed, static conditions,
Obtain casting solution；
40 DEG C of the casting solution is placed in hopper, controls thickness using clearance gauge, is supported with scraper in polyester non-woven fabric
Layer on carry out striking, form wet film on polyester non-woven fabric supporting layer, in air atmosphere carry out precuring (temperature be 80 DEG C,
Time is 90s), be then immersed in 20 DEG C of water carry out inversion of phases film forming 18h, obtain nano molybdenum disulfide composite membrane (with a thickness of
0.2mm, ultrafiltration membrane).
Comparative example 1
Membrane material is prepared according to the method for embodiment 1, the difference is that, dispense molybdenum disulfide nano sheet.
Comparative example 2
Membrane material is prepared according to the method for embodiment 4, the difference is that, dispense molybdenum disulfide nano sheet.
Comparative example 3
Membrane material is prepared according to the method for embodiment 5, the difference is that, dispense molybdenum disulfide nano sheet.
It is characterized using the membrane material that scanning electron microscope prepares Examples 1 to 5, wherein Fig. 1 is embodiment 1
The surface scan electron microscope of the membrane material of preparation, Fig. 2 are the cross-sectional scans electron microscope of membrane material prepared by embodiment 1.It can by Fig. 1
Know, the surface of membrane material prepared by embodiment 1 is smooth, has no that obvious nanoparticle is reunited.As shown in Figure 2, embodiment 1 is made
Typical ultrafiltration membrane unsymmetric structure is presented in the section of standby membrane material, that is, includes fine and close cortex, sponge hole supporting layer and finger-like
Macropore sub-layer, fine and close cortex and sponge hole supporting layer determine molecular cut off size, and sponge hole supporting layer and finger-like macropore are sub-
The porosity of layer determines the size of water flux；The formula of membrane material and preparation process to fine and close cortex, sponge hole supporting layer and
The respective thickness of finger-like macropore sub-layer, hole form etc. have a major impact, and the microstructure of membrane material for water flux and
Rejection has a major impact.The characterization result of membrane material prepared by embodiment 2~5 and Fig. 1~2 are almost the same.
The membrane material prepared to Examples 1 to 5 and comparative example 1~3 is tested for the property, and the results are shown in Table 1.
The performance test results of membrane material prepared by 1 Examples 1 to 5 of table and comparative example 1~3
Fig. 3 is the pure water flux of membrane material prepared by Examples 1 to 3 and comparative example 1 and the rejection to bovine serum albumin
Datagram, wherein the ordinate on the left side indicates pure water flux, corresponding histogram；The ordinate on the right indicates bovine serum albumin
(BSA) rejection, corresponding line chart；" M0 " corresponds to comparative example 1, " M1 " corresponding embodiment 2, " M2 " corresponding embodiment in abscissa
1, " M3 " corresponding embodiment 3.
Fig. 4 is the pure water flux datagram of membrane material prepared by embodiment 4 and comparative example 2, wherein " M0 " is right in abscissa
Comparative example 2 is answered, " M1 " corresponding embodiment 4.
Fig. 5 is the pure water flux of membrane material prepared by embodiment 5 and comparative example 3 and the rejection data to bovine serum albumin
Figure, wherein the ordinate on the right indicates pure water flux, corresponding histogram；The ordinate on the left side indicates that bovine serum albumin (BSA) is cut
Stay rate, corresponding line chart；" M0 " corresponds to comparative example 3, " M1 " corresponding embodiment 5 in abscissa.
By table 1 and Fig. 3~5 it is found that not influencing all occurs in preparation gained membrane material after addition molybdenum disulfide nano sheet
In the case where rejection, the phenomenon that water flux is risen, illustrate that nano molybdenum disulfide composite membrane provided by the invention has
Also there is higher water flux while higher rejection.
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 (10)
1. a kind of nano molybdenum disulfide composite membrane prepares raw material including following mass fraction:
2. nano molybdenum disulfide composite membrane according to claim 1, which is characterized in that the high molecular polymer includes poly-
Ether sulfone, polysulfones, Kynoar, polypropylene, polyethylene, polyvinyl chloride, cellulose acetate, polyacrylonitrile, polyimides, polyamides
One or more of amine-acid imide, polyetherimide and sodium alginate.
3. nano molybdenum disulfide composite membrane according to claim 1, which is characterized in that the thickness of the molybdenum disulfide nano sheet
Degree≤15nm, piece diameter size≤2 μm.
4. nano molybdenum disulfide composite membrane according to claim 1, which is characterized in that the pore-foaming agent includes poly- second two
One or more of alcohol, polyvinylpyrrolidone, glycerine, propylene glycol and acetone.
5. nano molybdenum disulfide composite membrane according to claim 1, which is characterized in that the organic solvent includes N, N- bis-
One or more of methylformamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone and dimethyl sulfoxide.
6. described in any item nano molybdenum disulfide composite membranes according to claim 1~5, which is characterized in that two sulphur of nanometer
Change molybdenum composite membrane with a thickness of 0.1~0.3mm.
7. the preparation method of any one of the claim 1~6 nano molybdenum disulfide composite membrane, comprising the following steps:
Nano molybdenum disulfide composite membrane is prepared into deaeration after raw material mixes, obtains casting solution；
The casting solution striking is formed into wet film, inversion of phases film forming is carried out after precuring, obtains nano molybdenum disulfide composite membrane.
8. preparation method according to claim 7, which is characterized in that the deaeration carries out under closed, static conditions；Institute
State deaeration temperature be 50~80 DEG C, the time be 2~for 24 hours.
9. preparation method according to claim 7, which is characterized in that the precuring carries out in air atmosphere；It is described
The temperature of precuring is 0~80 DEG C, and the time is 1~90s.
10. the preparation method according to claim 7 or 9, which is characterized in that the temperature of the inversion of phases film forming is 15~32
DEG C, the time is 2s~48h.
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| CN113041847A (en) * | 2021-02-05 | 2021-06-29 | 中国科学院城市环境研究所 | Molybdenum disulfide oxide composite film and preparation method thereof |
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| CN104138716A (en) * | 2014-08-06 | 2014-11-12 | 哈尔滨工业大学 | Modified PVDF ultra-filtration membrane preparation method with namometer MoS2 |
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| CN113041847A (en) * | 2021-02-05 | 2021-06-29 | 中国科学院城市环境研究所 | Molybdenum disulfide oxide composite film and preparation method thereof |
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